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1.7.3 Detailed Testing Two series of detailed test programs were conducted using the pilot-scale test unit. The first series of tests were performed to investigate the effects of the key design variables on separator performance and to simultaneously define the overall grade and recovery curve. The subsequent series of testing was used to investigate the effects of key operating parameters. Tests were conducted primarily as a function of teeter bed pressure and fluidization water rate. The coal/rock interface, or teeter bed, was adjusted to different levels (i.e. different bed pressure) for each steady-state test. Fluidization water was adjusted to fine tune the separation. For each test, samples were taken from the feed, overflow, and underflow streams after conditions were stabilized. Five test runs were completed during the on-site test work. 1.7.4 Process Evaluation Due to the low percent solids, the fine size distribution, and the low specific gravity of the material, bed development in the CrossFlow separator was very difficult for this particular application. Initial plans to feed the unit at 1 tph/ft2 could not be obtained due to the turbulence occurring in the bed formation area. Feed rates were slowly reduced over time until a 0.10 tph/ft2 feed rate with a water addition rate of 1.5 gpm produced a stable bed in the unit. Even at this low feed rate, an appreciable amount of plus 100 mesh material was still reporting to the overflow. Five sets of samples were collected of the feed, overflow, and underflow streams. However, laboratory analyses were not conducted on these samples because visual observations of the product streams indicated poor performance at attempting to classify the feed stream. The coal slurry evaluated in this series of experiments possessed a mean particle size of 0.075 mm. Table 1.14 is a summary of the array of operating parameters that were investigated 54
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1.8 Conclusions 1. A comprehensive study of the CrossFlow separator was conducted at four coal preparation plants on the east coast. In-plant testing of a 9 x 16 inch unit resulted in separation efficiencies at or above existing classification equipment in the size class of 0.2 to 1.0 mm. 2. The data demonstrate that for any given product ash content or sulfur content, the CrossFlow separator can produce a higher clean coal yield and higher combustible recoveries at higher feed rates when compared to the existing coal spirals. The CrossFlow also demonstrated its ability to handle the entire flow of multiple spirals in a single-stage circuit. 3. In the instance where the ultimate goal was to compare results against the existing clean coal effluent cyclones (28 mesh by zero material at 100 mesh), it was determined that the material was too fine to develop the necessary teeter-bed, and the project was therefore abandoned. 4. The test work conducted in this series of tests supports the replacement of spirals with the CrossFlow technology for several applications. As a result, several full scale installations of the unit are being planned in the near future. Based on the successful installation of these full scale units, further implementation of additional units can be utilized in a broad spectrum of companies and industries. 56
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Chapter 2 In-Plant Testing of HydroFloat Separator in Phosphate Industry 2.1 Introduction 2.1.1 General Teeter bed technologies can only be applied for gravity concentration when the particles in the feed stream have a relatively narrowly size distribution and moderately large difference in component densities. These units inherently accumulate low density coarse particles at the top of the teeter bed which are too light to penetrate the bed, but at the same time, too heavy to be carried by the rising water into the overflow. As a result, misplacement of low-density, coarse particles to the high-density underflow can occur. This inefficiency can be partially corrected by increasing the elutriation water, to try to carry the low density coarse particles into the overflow. However, this action often causes the fine, high-density particles to also report to the overflow, thereby impacting the quality of the products. As a result, the widespread application of traditional hydraulic separators is greatly limited by these physical constraints. The limitations of traditional hydraulic separators were recently recognized and overcome through the design of the HydroFloat separator. This technology effectively combines the flexibility of a flotation process with the high capacity of a density separator to overcome barriers that commonly limit conventional teeter bed separators. The HydroFloat can theoretically be applied to any mineral classification system where differences in apparent density can be created by the selective attachment of air bubbles. Figure 2.1 provides a schematic drawing of the HydroFloat separator. 58
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through the teeter bed and are eventually discharged through the control valve at the bottom of the separator. 2.1.2 Advantages of a Hydraulic Separator Compared to traditional froth flotation, the use of a fluidized bed within the HydroFloat significantly improves the recovery of particles by (i) reducing turbulence, (ii) enhancing buoyancy, (iii) increasing particle retention time, and (iv) improving bubble-particle contact. The presence of the high-solids teeter bed reduces the turbulence commonly associated in traditional flotation units and therefore enhances the buoyancy of the particles. The teetering effect of the hindered-bed relinquishes the need for bubble-particle aggregates to have sufficient buoyancy to rise to the top of the cell. The low density agglomerates can easily overflow into the product launder, where as the hydrophilic particles move through the teeter bed and eventually discharge through the control valve at the bottom of the separator. Other benefits of the HydroFloat separator versus traditional froth flotation cells include increases in particle retention time by producing a counter-current flow of particles settling in a hindered state against an upward rising current of water, and the increased probability of bubble- particle contacting in the teeter-bed due to the high-solids content. A higher production rate is possible with the HydroFloat separator than in traditional froth flotation cells due to the high percent solids in the compact teeter bed. The HydroFloat separator is ideally suited to recover coarse particles that traditional froth flotation cells cannot efficiently recover for several reasons. One reason for the improved recovery of coarse particles is the upward flow of elutriation water in the HydroFloat separator helps lift the larger particles into the product launder. The teeter bed also produces ideal 60
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conditions for bubble-particle interactions by maintaining high solids content and quiescent flow conditions. In addition, the high solids content within the teeter-bed separator makes it possible to treat large tonnages in a very compact volume as compared to conventional flotation separations which are conducted at very low solids contents using large volume cells. 2.1.3 Project Justification One of the driving forces behind the HydroFloat separator is the phosphate industry’s need to recover coarse particle phosphate (28 x 35 M size fraction) from the feed matrix. It is estimated that 10% of feed material to a Florida phosphate plant is in the plus 35 mesh fraction, which is virtually impossible to recover with present classification equipment. An improvement in coarse particle recovery with the HydroFloat alone corresponds to an additional $7.5-15 million of revenues. As in the coal industry, the energy benefits of the HydroFloat over conventional equipment are related to the reduction in pumping requirements and water usage which is a direct result of the higher feed ton rate. The lower operating and maintenance cost per ton of product is significantly reduced with the HydroFloat versus conventional equipment. Overall, the implementation of the HydroFloat separator will allow operations to become more profitable and more competitive by utilizing reserves more effectively, reducing waste and increasing productivity. 61
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2.2 Literature Review 2.2.1 General The recovery of minerals by flotation is one of the most versatile mineral-processing techniques used in industry today. Flotation methods are utilized throughout the mining industry to treat sulfide ores such as copper, lead and zinc, oxide ores such as hematite and cassiterite and non-metallic ores such as phosphate and coal (Wills, 1992). Since its inception in the early 1900’s, improvements in the flotation process have long been a goal within the industry and numerous studies have been financed to overcome the inefficiencies inherent in the process. Industry and government sponsored research programs have focused on all areas of the flotation process to improve recoveries including advancements in chemical reagents, adaptations to existing equipment and introduction of novel equipment. 2.2.2 History of Flotation Although a subject of considerable debate, flotation was believed to be first utilized in the mining industry by T.J. Goover, who in 1909 patented (British Patent No. 27-02-1909) the first multi-cell impeller-type apparatus for froth flotation (Rubinstein, 1995). However, research into the relationship between particle size and floatability did not begin until 1931, when Gaudin, et al. (1931) showed that coarse and extremely fine particles are more difficult to recover as compared to intermediate size particles. Twenty years after this original work, Morris (1952) arrived at the same conclusion, that particle size is one of the most important factors in the recovery of ores by flotation. Intermediate size particles will achieve the highest recovery, where as very fine particles (d <20Β΅m) will have the lowest recovery. In addition, as the particle p diameter begins to increase, the recovery will start to decline. This reduction in recovery on the 62
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fine and coarse size fractions is indicative of a reduction in the flotation rate of the particles (Jameson, 1977). It can be seen that the efficiency of the froth flotation process deteriorates rapidly when operating in the extremely fine or coarse particle size ranges, which is considered between 10 Β΅m and 200 Β΅m. This is evidence that conventional flotation practices are optimal for the recovery of particles between 65 to 100 mesh. According to Soto and Barbery (1991), conventional flotation cells operate with two contradictory goals. First, a conventional cell has to provide enough agitation to maintain particles in suspension, shear and disperse air bubbles, and promote bubble-particle collision. However, for optimal recovery, a quiescent system is required to reduce detachment and minimize entrainment. As a result, coarse particle flotation is more difficult since increased agitation is required to maintain particles in suspension. Furthermore, coarse particles are more likely to detach under turbulent conditions. To compensate for the lack of recovery, some installations are using relatively small flotation devices operated at low feed rates (Lawver, 1984). As particle size is reduced, two dominating characteristics begin to emerge, i.e., the specific surface becomes large and the mass of the particle becomes very small (Abdel-Khalek, et al., 1990). These are the dominating factors affecting fine particle recovery in flotation systems. Virtually all ores are associated with a clay mineral, which is ultimately transferred to the preparation plant with the mineral of interest. The clay minerals associated with the fine fractions will reduce mineral recovery by inhibiting bubble-particle attachment, and consuming flotation reagents. The variety of flotation machines available on the market today can be classified into two distinct groups: pneumatic and mechanical machines (Wills, 1992). Pneumatic machines 63
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commonly utilize air that is blown in or induced, where it must be dissipated through a series of baffles or some form of permeable base within the cell. Since air is used not only to produce the froth and create aeration but also to maintain the suspension and to circulate it, an excessive amount is usually introduced (Wills, 1992). Complications directly related to the excessive amount of air limited the use of pneumatic machines until the development of the flotation column. Mechanical flotation machines are the most common and widely used flotation machine on the market today. The units are characterized by a mechanically driven impeller which agitates the slurry and disperses the incoming air into small bubbles (Wills, 1992). Air addition into the cell can either be forced through an external blower, or self-aerating. Typically most mechanical flotation cells are set up in a series of β€œbanks”, where several cells will allow free flow from one cell to the next down the bank. Performance is generally based on three factors including: (i) metallurgical performance, i.e., product recovery and grade, (ii) capacity, and (iii) operating and maintenance costs (Wills, 1992). An analysis of the effectiveness of the various types of flotation machines was made by Young (1982), who discusses performance with regard to the basic objectives of flotation, which are the recovery of the hydrophobic species into the froth product, while still achieving a high selectivity by retaining as much as the hydrophilic species as possible in the slurry. Recovery is directly related to particle-bubble attachment and requires quiescent conditions, which is not found in conventional mechanical flotation devices. The mechanical impellers found in typical flotation cells are not ideal for particle-bubble contact, which has led the industry to utilize column cells for a variety of mineral applications that, up until the past decade or two, was unheard of. 64
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Column cells are considered to be ideal displacement machines, where as mechanical cells are ideal mixers (Wills, 1992). A column cells improves flotation performance by minimizing turbulence within the cell and reducing entrainment using froth washing. In 1914, G.M. Callow patented the first apparatus with air sparging through a porous false bottom, (Rubinstein, 1995), which would become the basis for future column cell designs. By 1919, M. Town and S. Flynn had developed the first design involving a countercurrent of slurry and air within a column. While pneumatic Callow apparatuses were very popular in the early 1920’s and 30’s, the lack of technological progress in the area of reliable pneumatic air spargers and lack of process control systems forced the introduction of impeller-type apparatuses. It wasn’t until the mid 1960’s that column cells began to be intensively developed and extensively introduced into the industry, when practically all the work on updating other types of flotation cells ceased (Rubinstein, 1995). The advantages of column cell technology over conventional mechanical cells are directly related to the direction of flow of the slurry and air. The counter-current regime provides for more ideal bubble-particle attachment and enhanced aggregate stability. The likelihood of bubble-particle detachment is minimized due to low turbulence of slurry flows within the column. These benefits have prompted the phosphate industry to implement column flotation cells into the industry for fine and coarse particle flotation. 2.2.3 Phosphate Flotation Phosphate beneficiation plants are designed to process run-of-mine ore, typically called the ore matrix, into a sellable product for use in either the fertilizer market or as an integral part or the production of phosphoric acid. The ore matrix is upgraded by separating the phosphate 65
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grains from other impurities such as clay and silica. Beneficiation plants in the southeastern United States (Florida and North Carolina) generally use sizing and classification processes to concentrate the phosphate rock and separate it from impurities. Florida beneficiation plants typically wash and deslime the ore matrix at 150 mesh. The material finer than 150 mesh is considered tailings and is pumped to settling ponds. Approximately 30% of the phosphate contained in the original ore matrix is lost to the tailings ponds. The remaining rock is separated into three size classes, a pebble size fraction, coarse and fine size fractions. The pebble is a high phosphate content rock (-3 ΒΌ x 14 mesh) that requires no further processing. The coarse size fraction (14 x 35 mesh) and fine size fraction (35 x 150 mesh) are treated separately in different flotation circuits. Historically, fine phosphate flotation is an efficient process with recoveries from conventional froth flotation in excess of 90% for most ores. Recoveries will vary depending on the ore type, with recoveries dropping slightly for some high manganese or dolomitic ores. In contrast, froth flotation recoveries for coarse phosphate are generally much lower than those of fine phosphate ores. Typical recoveries for coarse flotation are less than 50%. Historically, hammer mills were used for size reduction, but due to high maintenance costs and loss of fines, this practice has been discontinued (Soto, 1992). The industry, however, has taken other approaches to circumvent the problem of low floatability of coarse particles. For instance, such approaches are exemplified by the use of gravitational devices such as spirals, tables, launders, sluices and belt conveyors modified to perform a "skin flotation" of the reagentized pulp. Although a variable degree of success is obtained with these methods, they have to be normally supplemented by scavenger flotation. In addition, some of them require excessive maintenance, have low capacity, or involve high 66
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2.3 In-Plant Testing at Phosphate Plant A The Phase I field-testing of the HydroFloat separator involved equipment setup, shakedown and detailed testing at the Phosphate Plant A. The goal of this effort was to compare the unit to existing conventional cells in several different areas of the plant by analyzing the anticipated product grade and recovery, insol content, reagent consumption, and feed capacity at, and above, design feed rates of the unit. The three areas of the plant where the HydroFloat separator was tested included the fine feed, amine flotation and coarse feed circuits. The main objective of the fine and coarse phosphate testing was to demonstrate the potential of the unit as a candidate for the process equipment in a proposed plant design with both fine and coarse circuits. The main objective of the amine flotation testing was to demonstrate the feasibility of using the unit for silica flotation and to develop data to determine its potential application for use in the amine flotation circuit at Phosphate Plant A. Approximately 6 months was allocated to this task. Individuals from Eriez Magnetics and Virginia Tech participated in the testing at Phosphate Plant A with cooperation from key personnel at the processing plant. Additional tests were conducted by Phosphate Plant A representatives to expand the data base for evaluating the potential of incorporating the HydroFloat separator into proposed circuit upgrades. 2.3.1 Equipment Setup 2.3.1.1 Fine Circuit The installation of the pilot-scale unit in the fine feed circuit at Phosphate Plant A was the main objective of this task. The separator was transported from the Eriez Magnetics Central Research Lab in Erie, Pennsylvania to the processing plant. With cooperation from the operators 68
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and mechanics at the plant, the 18-inch diameter pilot-scale HydroFloat separator was installed at the fine circuit at Phosphate Plant A as shown in Figure 2.2. Reagentized feed was supplied to the HydroFloat separator through a 2 inch line connected to the existing plant conditioning tanks. Concentrate and tailings streams were discharged into floor sumps. The unit was operated as a column flotation cell, utilizing the HydroFloat separator air sparging system. The test unit included 3 compartments that allowed more water and air to be added (up to 60 gpm water and 10 cfm air). There was no teeter-bed required in this system. Plant compressed air and 115 volt electrical power were connected to the separator for the automated control system. The separator was automatically controlled through the use of a simple PID control loop which includes a pressure sensor mounted on the side of the separator to measure the relative pressure (level), a single loop PID controller, and a pneumatic pinch valve to control the underflow discharge to maintain a constant bed pressure (level). 69
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added (up to 60 gpm water and 10 cfm air). There was no teeter-bed required in this system. Plant compressed air and 115 volt electrical power were connected to the separator for the automated control system. The separator was automatically controlled through the use of a simple PID control loop which includes a pressure sensor mounted on the side of the separator to measure the relative pressure (level), a single loop PID controller, and a pneumatic pinch valve to control the underflow discharge to maintain a constant pressure (level). 2.3.1.3 Coarse Circuit The same separator used in the fine and amine flotation circuits was also used in the coarse circuit, with one modification. The center compartment was removed from the unit, so as to allow the unit to operate with a typical teeter-bed (a total of 2 compartments). With cooperation from the operators and mechanics at the plant, the 18-inch diameter pilot-scale HydroFloat separator was installed in the coarse circuit at Phosphate Plant A. Reagentized feed was supplied to the HydroFloat through a 2-inch line connected to existing plant conditioning tanks. Concentrate and tailings streams were discharged into floor sumps. Electrical power at 115 volt and plant compressed air were connected to the separator for the automated control system. The separator was automatically controlled through the use of a simple PID control loop which includes a single loop PID controller, a pressure sensor mounted on the side of the separator to measure the relative pressure, and a pneumatic pinch valve to control the underflow discharge to maintain a constant bed pressure. 71
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2.3.2 Shakedown Testing Preliminary shakedown testing was conducted after completing the installation of the test HydroFloat unit to resolve any unexpected operational problems that could arise. These tests are normally necessary to resolve any problems that may have been overlooked in the initial engineering and to confirm that feed capabilities, pipe sizes, electrical supplies, control systems, etc., are adequate. An average of six shakedown tests per circuit was conducted with the unit. 2.3.3 Detailed Testing Two series of detailed test programs were conducted using the pilot-scale test unit. The first series of test were performed to investigate the effects of the key design variables on separator performance and to simultaneously define the overall grade and recovery curve. The HydroFloat separator is designed for feed rates of 2 tph/ft2 and 1 tph/ft2 rougher concentrate, which allows the test unit to operate at 4 tph feed and 2 tph concentrate, respectively. The initial testing in the fine and coarse circuit evaluated the unit at loading rates much higher than design to establish the recovery fall-off. The design rates for the amine flotation circuit were not precisely known going into the testing, but were thought to be similar to those for rougher flotation. Part of the amine testing program was devoted to determining the design rates and evaluating the HydroFloat separator performance across the board, both at the design rate and above. With the recovery fall-off determined for each circuit and unit configuration, the subsequent series of testing was used to investigate the effects of key operating parameters. Tests were conducted to establish reagent consumption (fatty acid, surfactant, amine and diesel oil), to investigate the bed levels and sparger water required for the best unit operation and to 72
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investigate the variability associated with the overall system. For each test, samples were taken from the feed, concentrate and tailings streams after conditions were stabilized. The samples were analyzed for BPL, MgO and insol contents. 2.3.4 Process Evaluation All as-received results were analyzed and adjusted using mass balance software to ensure the test data was reliable and self-consistent. Any experimental values that were deemed by the mass balance routines to be unreliable were removed from the data set. The participating mining company used the compiled data to establish the metallurgical improvement, operating savings and economic payback that may be realized by implementing the proposed high-efficiency technologies. The process evaluation has been divided into three sections including (i) fine feed circuit, (ii) amine flotation circuit, and (iii) the coarse feed circuit. 2.3.4.1 Fine Feed Circuit Fifty-three tests were conducted during the fine circuit testing at Phosphate Plant A. Testing in the fine circuit produced an average of 10% higher BPL recoveries with a 0.8% lower BPL rougher tail in the HydroFloat separator than in the plant Wemco cells. Figure 2.3 displays the HydroFloat separator and plant tails percent BPL for each test. The plant Wemco cells averaged only about 0.7% BPL higher-grade rougher concentrates than the HydroFloat as shown in Figure 2.4. An average HydroFloat separator rougher concentrate grade of 54.9% BPL is satisfactory considering the test feed grade only average 8% BPL through most of the testing. 73
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During testing, several attempts were made to obtain final grade concentrates (7% insol) with one stage of flotation. The results show that insol concentrates between 9-10% produced only 74-76% recoveries, and dropping the insol to 7-8% reduced the recoveries to 70% or less. Further testing in this area needs to be conducted utilizing more selective reagents or higher feed grades to achieve the desired 7% insol concentrates in a one step flotation process with the HydroFloat separator. One of the most important operating parameter to consider for fine flotation is the ability of the process equipment to recover coarser material into an acceptable concentrate: i.e., recover coarse phosphate without recovering fine silica. Comparison testing of the HydroFloat separator with the Wemco Cell produced promising results. As shown in Figure 2.5, the HydroFloat separator recovered 80%, 83%, and 88% of the plus 20 mesh, 20 x 28 mesh, and 28 x 35 mesh phosphate, respectively. The performance values were well above those established for the plant; the plant recovered only 24% of the plus 35 mesh and 67% of the plus 48 mesh phosphate. Percent solids in the tailings averaged between 20-30% at optimum testing conditions. During less than optimum conditions, the solids were as high as 53%. Optimum conditions occurred at 70-75 bed levels, with between 50-60 gpm of sparger water, and 4 tph feed. While higher bed levels and less sparger water could produce a slightly higher percent solids in the tailings, this adversely affected the recovery and concentrate grades. Using the unit with 3 compartments and with bed levels of 70-75, the optimum froth depths were 15-20 inches. Reagent dosages were affected by the poor water quality and excessive slimes in the feed during the testing program. The fatty acid dosage in the plant ranged from 0.80 to 1.20 lb per ton of fine feed during testing, whereas the fuel oil dosage in the plant ranged from 0.35 to 0.55 lb 75
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optimum operating conditions. The optimum conditions for the HydroFloat separator for use in fine flotation as defined by this testing program are: 3 compartment unit, with bed level between 70-75, a froth depth of 15-20 inches, sparger water between 55-60 gpm, air flow of 10 cfm, and a surfactant dosage of at least 0.2 lb per ton of feed. The measured recovery values and concentrate grade at these design rates were acceptable. Based on this data, the HydroFloat separator can successfully be implemented into the Phosphate Plant A fine flotation circuit. 2.3.4.2 Amine Circuit Twenty-four tests were conducted during the amine flotation circuit testing at Phosphate Plant A. HydroFloat separator testing in the amine flotation circuit produced an average of 1.3% higher insol concentrate and recovered about 8% less insol to the amine tailings than in the Plant Wemco Cell. Figure 2.6 displays the concentrate grade for the HydroFloat separator and the plant for each test. The plant Wemco cells averaged only about 0.5% higher BPL recovery than the HydroFloat separator as shown in Figure 2.7. The HydroFloat separator performed virtually the same as the plant Wemco cell for amine flotation over the range 3 to 18% concentrate insol and 95 to 99% BPL concentrate recovery. The unit demonstrated it could effectively recover coarse silica. The HydroFloat separator insol recovery values were about 3% lower on average than those in the plant at above design feed rates. The differences ranged from 6% to 11% in the 35 mesh and 48 mesh fractions to 2% in the finer fractions. The HydroFloat separator insol recovery values were about 2% higher on average than those in the plant at the lower feed rates. 77
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100 95 90 85 80 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 Test No. 79 )%( yrevoceR LPB Plant HydroFloat Figure 2.7. BPL Recovery Comparisons HydroFloat Separator vs. Existing Plant Cells. One of the most important operating parameters to consider for amine flotation is the ability of the process equipment to recover coarse silica without recovering phosphate. Comparison testing of the HydroFloat separator with the Wemco Cell produced promising results. As shown in Figure 2.8, the HydroFloat separator had just slightly less recoveries than the plant for all of the size fractions except the 35 mesh, where it had a nearly 6% increase in BPL recovery than the plant. Reagent dosages were affected by the poor water quality and excessive slimes in the feed during the testing program. The surfactant dosage for the HydroFloat separator ranged from 0.13 to 0.40 lb per ton of feed. The recommended dosage was 0.14 lb per ton at design rates.
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100.00 90.00 80.00 70.00 60.00 50.00 40.00 30.00 20.00 10.00 0.00 35 48 65 100 150 -150 Size Class (Mesh) 80 )%( yrevoceR LPB HydroFloat Plant Cells Figure 2.8. Comparison of Test Results for Amine Phosphate (Plant Circuit #2). The interactions of varying diesel fuel dosage rates were studied during the amine circuit testing. Amine flotation circuits use diesel oil or polymer occasionally to modify the froth when slimy water is present. Froth stability was investigated, but was difficult to determine due to the lack of air flow measurement available at the time of testing. Exact diesel fuel dosage rates are unknown at this time. While the operation of the HydroFloat separator for amine flotation was difficult to optimize due to various outside variables affecting the system, a significant number of tests were conducted at differing operating variables under varying operating conditions to achieve optimum operating conditions. The optimum conditions for the HydroFloat separator for use in amine flotation as defined by this testing program are: 3 compartment sections, with bed level between 70-75, a froth depth of 15-20 inches, sparger water at 25 gpm, air flow of 10 cfm, and a
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surfactant dosage of at least 0.2 lb per ton of feed. Additional testing will be needed in the future to validate these recommendations. The measured silica recovery values and concentrate grades at these design rates were acceptable. Based on this data, the HydroFloat separator can successfully be implemented into the Phosphate Plant A amine flotation circuit. 2.3.4.3 Coarse Circuit Twenty-four tests were conducted during the coarse circuit testing at Phosphate Plant A. Testing in the coarse circuit produced an average 12% higher BPL recovery with a 3.5% lower BPL rougher tail in the HydroFloat separator than in the Plant Wemco Cell. Figure 2.9 displays the HydroFloat separator and plant tails percent BPL for each test. Figure 2.10 displays the concentrate recovery for the HydroFloat separator and Plant Wemco Cell. The plant average about 6% BPL higher-grade rougher concentrates than the HydroFloat separator as shown in Figure 2.11. However, the average concentrate grade of 62.6% BPL was still considered satisfactory for the testing. As with the fine and amine flotation circuits testing, poor water quality played an important role in the overall performance of the reagents during testing. Fatty acid dosage in the plant ranged from 2.04 to 3.61 lb per ton of coarse feed during testing, while fuel oil dosage ranged from 1.06 to 1.68 lb per ton of feed. Both of these values are considered high for Phosphate Plant A, and hindered recoveries as a result. Surfactant dosage for the HydroFloat ranged from 0.23 to 0.77 lb per ton of feed, which was also considered to be a high dosage, mostly attributable to the high fatty acid-fuel oil dosage in the plant. Other contributing factors were the poor water quality and the need to set the 81
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2.4 In-Plant Testing at Phosphate Plant B Equipment setup, shakedown testing, and detailed testing comprised the phase I field- testing of the HydroFloat separator at Phosphate Plant B. The goal of this effort was to compare the unit to existing hydroclassifiers and conventional cells by analyzing the anticipated product grade and recovery, insol content, reagent consumption and feed capacity at, and above, design feed rates of the unit. The main objective of testing was to determine if the HydroFloat separator could achieve higher recoveries of the ultra-coarse particles than the existing second-stage hydroclassifer at the plant. Further investigations of the coarse and fine matrices were conducted, comparing results against the existing conventional cells currently in operation at the plant. Approximately 12 months was allocated to this task. Individuals from Eriez Magnetics and Virginia Tech participated in the testing at Phosphate Plant B with cooperation from key personnel at the processing plant. 2.4.1 Equipment Setup The separator was transported from the Eriez Magnetics Central Research Lab in Erie, PA to the processing plant. With cooperation from the operators and mechanics at the plant, the 1-foot diameter pilot-scale HydroFloat separator was installed at each circuit (ultra-coarse, coarse and fine) for a period of several weeks for each circuit at Phosphate Plant B as shown in Figure 2.13. Reagentized feed was supplied to the HydroFloat separator through a 2-inch line connected to the existing plant conditioning tanks. Concentrate and tailings streams were discharged into floor sumps. Plant compressed air and 115 volt electrical power were connected to the separator for the automated control system. The separator was automatically controlled through the use of a 86
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2.4.2 Shakedown Testing After completing the installation of the test HydroFloat unit in each circuit, preliminary shakedown testing was conducted to resolve any unexpected operational problems that could arise. Shakedown test are commonly utilized to resolve any problems that may have been overlooked in the initial engineering and to confirm that feed capabilities, pipe sizes, electrical supplies, control systems, etc., are adequate. 2.4.3 Detailed Testing Two series of detailed test programs were conducted for each circuit using the pilot-scale test unit. The first series of test were performed to investigate the effects of the key design variables on separator performance and to simultaneously define the overall grade and recovery curve. The HydroFloat separator is designed for feed rates of 2 tph/sqft and 1 tph/sqft rougher concentrate, which allows the test unit to operate at 4 tph feed and 2 tph concentrate, respectively. The initial testing in the coarse circuit evaluated the unit at loading rates much higher than design, to establish the recovery fall-off. With the recovery fall-off determined for each circuit and unit configuration, the subsequent series of testing was used to investigate the effects of key operating parameters. Tests were conducted to establish reagent consumption (fatty acid, surfactant, and diesel oil), to investigate the bed levels and sparger water required for the best HydroFloat separator operation, and to investigate the variability associated with the overall system. For each test, samples were taken from the feed, concentrate and tailings streams after conditions were stabilized. The samples were analyzed for BPL, MgO, and insol contents. 88
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2.4.4 Process Evaluation To ensure the test data was reliable and self-consistent, all as-received results were analyzed and adjusted using mass balance software. Experimental values that were deemed by the mass balance routines to be unreliable were removed from the data set. The participating mining company used the compiled data to establish the metallurgical improvement, operating savings and economic payback that may be realized by implementing the proposed high- efficiency technologies. The process evaluation has been divided into three sections including the (i) ultra-coarse rock feed, (ii) the coarse rock feed, and (iii) the fine feed circuits. 2.4.4.1 Ultra Coarse Feed Grade versus recovery data for the in-plant evaluation of the HydroFloat had BPL recoveries of 87% to 99% with product grades ranging between 5% and 14% insols. The resulting products contained, on average, 67% BPL. Figure 2.14 is a graph of the grade versus recovery data for the in-plant testing and earlier laboratory-scale testing. Size-by-size analysis of the HydroFloat was conducted and results are presented in Figure 2.15. The HydroFloat is capable of high BPL recoveries for even the coarsest size fractions, where 96.7% of the available BPL in the +16 mesh size class was recovered. 89
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2.4.4.2 Coarse Feed Figure 2.16 summarizes the grade and recovery data for the coarse feed test work. BPL recoveries ranged from 90% to 98% while product grades averaged 24.7% insols. The resulting products contained, on average, 55% BPL by weight. Figure 2.16 also illustrates that the results for the laboratory evaluations were superior to those produced for the in-plant trials. This occurrence is a direct result of the mean particle size difference found between the samples used for the laboratory and in-plant testing. It was calculated that the sample used for the coarse matrix laboratory testing was as coarse (mean size: 0.706 mm) as the sample provided for the ultra-coarse testing (mean size: 0.721 mm). During the in-plant trials, it was observed that the coarse matrix was significantly finer, amplifying any occurrence of hydraulic carry-over or activation of fine floatable insols. 100 95 90 85 80 75 70 0 10 20 30 40 50 60 Product Insols (%) 91 )%( yrevoceR LPB Plant Testing Laboratory Testing Figure 2.16. BPL Recovery vs. Product Insol Grade for Coarse Matrix.
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2.4.4.3 Fine Feed The results from the in-plant testing on the fine matrix are shown in Figure 2.17. BPL recovery ranged from 88% to 97% using the HydroFloat. When operated as an open column, BPL recoveries ranged from 85% to 92%, though at a significantly lower product insol (37% vs. 22%, respectively). Results from samples collected around the existing plant rougher-scavenger swing circuit are also presented in Figure 2.17 for comparison. The findings indicate that the open column cell (w/ HydroFloat sparging system) is able to achieve incrementally higher BPL recoveries at lower product insol grades compared to either the HydroFloat or the existing column technology. The corresponding product grade (%BPL) averaged 55% for the open column system as seen in Figure 2.18. As with the ultra-coarse and coarse circuits, the HydroFloat achieved an acceptable product grade and recovery in the fine circuit. 100 95 90 85 80 75 70 0 10 20 30 40 50 60 Product Insols (%) 92 )%( yrevoceR LPB HydroFloat Plant Testing HydroFloat Laboratory Testing Existing Swing Cells Open Column w/HF Sparging System Figure 2.17. BPL Recovery vs. Product Insol Grade for Fine Matrix.
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2.5 Conclusions 1. The in-plant evaluation of the HydroFloat separator demonstrated that this novel separation device can successfully treat the three different size fraction in a typical phosphate processing plant. For the ultra-coarse rock, the separator produced a high grade phosphate product (+66% BPL) at BPL recoveries exceeding 95%. For the coarse sized feed fraction, the separator produced a 99% BPL recovery at an 8% insol grade. Significant improvements were also achieved in the fine feed fractions where a BPL recovery greater than 90% was achieved with product insoles ranging between 22-25%. 2. Several advantages can be realized through implementation of the HydroFloat system. The system can provide a higher product mass recovery, superior metallurgical results, lower reagent costs and lower power requirements, with the greatest advantage being the higher separation efficiency. A higher product mass recovery with a better product quality is a significant achievement for this application. The HydroFloat has a substantially lower operating cost due to reduced reagent consumption and power requirements compared to conventional equipment. 3. One of the goals of this project is to successfully prove the technology in a sufficient period of time to minimize the financial risk that will be taken by industry. The previous years test work has eliminated the uncertainties associated with the HydroFloat separator by proving plant scale units do in fact work. This can be seen by the fact that industry leaders have submitted purchase requests for full scale units in their preparation plants. 95
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Chapter 3 Beneficiation of Ultra-Fine Phosphate Streams 3.1 Introduction Phosphate beneficiation plants are engineered to recover phosphate occurring in the 0.1 mm size fraction. In many cases, phosphate ore coarser than 1mm (i.e., ultra-coarse) is stockpiled and either ground and routed through the beneficiation plant or blended directly with the final product. Unfortunately, the phosphate that occurs in the finer fractions (i.e., finer than 0.1 mm) is generally rejected as waste in the clay slimes. Approximately 100,000 tons of these phosphatic clay slimes in dilute (3-5%) slurry are pumped to tailings impoundments in Florida each day. In addition to the expense of disposing of the waste clay, mining companies are throwing away millions of dollars in phosphate to the refuse stream. It is estimated that 27% of the current annual production of phosphate is lost to this refuse stream. Economic recovery of phosphate from the phosphatic clays could extend Florida’s phosphate resource life by decades. Slimes are a natural component of phosphate ore. The slimes (phosphatic clays) consist of both phosphate and clay particles. According to Zhang (2001), there are three major characteristics of refuse slimes cause extreme difficulty in recovering the phosphate economically: the ultra-fine particle size (35-50% below 1 micron), the even distribution of phosphate particles among the various size fractions and the high clay content (30-50%). As particle size is reduced, two dominating characteristics begin to emerge: the specific surface becomes large and the mass of the particle becomes very small (Abdel-Khalek, et al., 1990). The ultra-fine particles in a slimes stream increase the chance of the fine particles getting carried into the froth as they are either entrained in the liquid or mechanically entrapped with the 98
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particles being floated. Material from a slimes stream will have excess amounts of gangue minerals, which will ultimately reduce the grade of the concentrate if they are carried into the froth. Excessive slimes can significantly reduce flotation performance and simultaneously increase reagent consumption. Because of their high dolomite content, acidulation of such concentrates consumes excessive sulfuric acid and causes problems during phosphoric acid manufacture such as increased acid viscosity, precipitation of insoluble Mg-phosphates and difficulties in filtration and clarification of the final product. As a result, the phosphatic clays are continuously rejected from the beneficiation plant using both vibrating screens and hydrocyclones. The slimes, including the fine phosphate, are ultimately placed in large tailings ponds, which act as large holding cells that are used for both water clarification and refuse storage. Misplaced coarse phosphate values are also present in the refuse stream. The coarse values are predominately a result of inefficient sizing or desliming. For instance, if an excess amount of material is pumped to a hydrocyclone, the cyclone will β€œrope” causing vast misplacement of coarse material. β€œRoping” is a common occurrence in the phosphate industry due to the natural settling characteristics of the coarse ore. A typical Florida phosphate plant discards 100,000 gpm to the tailings ponds, of which a significant portion of is fine phosphate (passing 0.1 mm). Combined with the misplaced coarse particles, the discarded phosphate represents a significant reduction in overall plant efficiency and a resultant increase in the required volume of the refuse tailings ponds. Recovering this material would increase overall plant production, while ultimately reducing operating costs. While previous research has been conducted in this area, there is still not an economical recovery system and as a result, this phosphate is currently considered unrecoverable by industry. 99
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An urgent need exists to develop a low-cost recovery circuit to recover a significant amount of the phosphate values that are currently being thrown away. One circuit configuration that may meet this requirement is shown in Figure 3.1. The circuit, which incorporates simple low-cost unit operations such as hydraulic classifiers, hydrocyclones, and flotation cells, can be tailored to exploit particle characteristics particular to the size range in question. The proposed circuit uses a large free-settling tank to collect the entire flow of phosphatic clays that are currently rejected from the beneficiation plant. Tanks similar to these are already extensively used by industry. The tanks allow the coarse fraction (plus 400 mesh) of the phosphatic clays to settle out in a free-settling regime. The settling tank is equipped with an overflow launder to collect the finest fraction, which is directed to plant tailings. The plus 400 mesh fraction is pumped to a bank of hydrocyclones. The hydrocyclones reject as overflow the remaining slimes that inherently remain with the coarse fraction. At this point in the circuit, the cyclone underflow will be significantly deslimed and will have relatively high percent solids. However, as flotation feed, the cyclone underflow will still contain slimes (due to bypass) that will prove detrimental to flotation performance and reagent consumption. To overcome this problem, the cyclone underflow is further treated using a CrossFlow hydraulic separator. The teeter bed in the CrossFlow separator removes the majority of slimes via countercurrent washing. The underflow from the CrossFlow, which is optimal material for flotation feed, will be discharged through the bottom of the unit at a high percent solids (i.e., up to 75%). The final step of the process involves column flotation to recovery the phosphate ore in the presence of the clay slimes. Unlike coarse phosphate ore, it is expected that the fine nature of 100
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3.2 Literature Review 3.2.1 General Florida has enormous reserves and will continue to produce a third of the world’s phosphate supply simply by making changes in the present system of mining, beneficiation, waste disposal and land reclamation (Lawver et al, 1984). Beneficiation plants continue to optimize separation processes to improve recoveries and minimize gangue minerals in the final product. From improved separation technologies to better flotation reagents, all aspects of the beneficiation process are being analyzed to determine where improvements can be made. As waste disposal becomes a more and more urgent issue, new techniques are being proposed to increase recovery of P O in the clay slimes stream. Current beneficiation plants dispose of one- 2 5 third of the current annual phosphate production through the clay slimes stream. The source of the problematic recovery of phosphate from the slimes stream is the existence of almost 50% clay minerals in the stream. These slimes are removed, not only because they are refractory toward presently known upgrading processes, but they also interfere with the operation of the flotation on the remainder of the material (Hazen, 1969). As a result, researchers have been trying for decades to develop efficient and economical processes to recover the phosphate from the clay slimes stream. Beneficiation has become increasingly more difficult as reserves continue to have more dolomite content, lower ore grades and increased clay content. As production continues into the Hawthorn Formation in Florida, the silicate contamination is compounded with additional magnesium contamination. Beneficiation plants can no longer blend lower MgO ore with higher dolomitic ores (containing the MgO) to alleviate this problem. Both calcite and dolomite consume sulfuric acid and can cause excessive foaming during rock processing. Dolomite is 103
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particularly detrimental to the process because magnesium passes into and degrades both liquid and solid fertilizer products (McCullough et al., 1977). Historically, the separation of dolomite and calcite from phosphate has primarily been conducted through various flotation processes. Three reagents are historically used for rougher flotation of phosphate from most of the siliceous gangue: a fatty acid type collector, an oil-type extender, and a pH regulator (Lawver et al., 1984). Fatty acid collectors consist of crude tall oil, reconstituted tall oil, blends of tall oil with vegetable fatty acids, or tall oil soap skimmings. Oil- type extenders are commonly fuel oils, reclaimed motor oils, or mixtures of these two. The use of fuel oil extenders with fatty acids as an auxiliary collector in flotation is well known and practiced in the industry. Fuel oil does not adsorb onto phosphate and quartz in the absence of fatty acids, and as a result, flotation cannot be achieved with fuel oil alone. Fuel oil will adsorb synergistically with fatty acids on apatite. Ammonia and soda ash are the two most common pH modifiers used in the industry. Sodium silicate is one of the most widely used depressants for floating non-sulphide mineral. Sodium silicate is primarily a strong and selective depressant (Shin and Choi, 1985). The use of selective flocculation has also been studied on the phosphatic clays. While studies have been conducted with all of these reagents, today there is still no industry-wide standard of separating phosphate from dolomite, calcite and other clay constituents. 3.2.2 Advances in Flotation Reagents 3.2.2.1 Use of Sodium Silica Recovery of phosphate from fine clay streams has historically been very problematic due to the high concentration of gangue minerals. Sun and Smit (1963) were able to recover fine 104
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phosphate from Florida washer slime material using various fatty acid collectors and tall oil. Various conditions were tested including effects of pH, fuel oil, pulp density and addition of sodium metasilicate. Flotation results show that phosphate flotation decreases in the order of linolenic, linoleic, oleic and stearic acid, which have 3, 2, 1, and 0 double bonds respectively (Sun and Smit, 1963). Sun and Smit (1963) concluded that unsaturated acids are preferred for most flotation purposes. Duplicate test runs achieved recoveries of 29.8 and 31.0% P O with 2 5 13.0 and 12.7% insolubles, respectively with test conditions including: 8.5 pH, 2.24 lb/ton fatty acid, 6.72 lb/ton fuel oil, 0.10 lb/ton pine oil, and 12 minutes of conditioning at 25% solids (Sun and Smit, 1963). The fatty acid used had between 1.3 and 1.5% rosin acids, with the highest overall fatty acid content of the materials tested (96.5-96.9%) to achieve the best recoveries. Mishra (1982) was one of the first who studied the electrokinetic properties of sodium metasilicate, to be used as the modifying agent for the separation of apatite from calcite by depressing calcite when using sodium oleate as the collector. Mishra determined that the degree of polymerization of sodium silicate is influence by its SiO to Na O ratio, where polymerization 2 2 increases with the increase in SiO to Na O ratio. The optimum rate of polymerization was 2 2 found to be at pH 8.6 (Mishra, 1982). While sodium metasilicate and sodium oleate additions were kept constant at 5 X 10-3 M and 5 X 10-4 M, respectively, flotation test work was carried out at various pH. The addition of sodium metasilicate produced a depression zone between pH 6.0 and 9.0, but flotation recovery increased to 100% between pH 9.0 and 10.0. Recoveries decreased to zero by pH 11.7. Mishra related the differences in recovery to changes in zeta potential, and predicted two causes for its occurrence: (1) the adsorption of cationic species at the apatite surface or (2) the adsorption of colloidal molecular species of sodium silicate. Flotation results suggested that the selective action of sodium metasilicate on calcite, with sodium oleate 105
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as a collector, apatite and calcite could be separated in the alkaline pH environment at about pH 10.0, depressing calcite with sodium metasilicate (Mishra, 1982). Anazia and Hanna (1987) also found that the addition of sodium silicate improved the P O recovery in the phosphate concentrate and increased the rejection of siliceous gangue in the 2 5 tailings in Florida phosphate operations. Their research concentrated first on the removal of dolomite from the feed, followed by silica removal. Testing procedures included 250-g batches of 48 x 400 mesh flotation feed in a D-1 Denver laboratory flotation machine with the impeller speed set at 100 rpm (Anazia and Hanna, 1987). Oleic acid was used as the collector and pine oil as the frother. Dolomite flotation was conducted by adjusting the pH to between 4.5 and 5.0 with various dilute acids. The fatty acid collector (at 3.3 lb/ton collector addition) and frother were injected into the pulp and air was immediately introduced into the pulp to float the carbonate gangue minerals. After separation of dolomite, as froth, the cell product was conditioned for three minutes with 1.1 lb/ton sodium silicate at a pH of 6.0 to 7.0. This was followed by another three minute conditioning with 1.1 lb/ton fatty acid collector and flotation of the phosphate minerals. The silica was depressed by the sodium silicate and the phosphate was floated to give concentrates of 29% P O and 0.8% MgO, with a recovery of 76% (Anazia and Hanna, 1987). 2 5 This process is also referred to as the Mineral Resource Institute (MRI) process. Since there was no phosphate depressant used, the pH had to be strictly controlled, which resulted in large acid consumption. As a result the project was considered unsuccessful. Anazia and Hanna concluded that carbonate minerals (dolomite and calcite) readily react with inorganic acids, resulting in the preferential dissolution or removal of mixed surface contaminants on the carbonate particles and exposure of fresh clean surface sites suitable for 106
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fatty acid adsorption. Carbon dioxide microbubbles are then generated by the carbonate minerals, allowing for enhanced oleic acid adsorption at the solid-liquid-gas interface, and β€˜instant’ flotation of the mineral (Anazia and Hanna, 1987). Oleic acid will still have an affinity for the apatite particles, but it will not be as great as for that of the microbubble-encapsulated dolomite particles. During the same time period, the Bureau of Mines conducted flotation tests on fine phosphate recovered from Florida operation slimes utilizing sodium silicate. The clay was first sized using hydrocyclones and hydroseparators, recovering up to 96% of the plus 400 mesh material, which was then used as a basis for the flotation test work (Zhang, 2001). The study used a fatty acid flotation at pH 9.0 with sodium silicate to depress the quartz in the rougher and cleaner flotation stages. At pH 9.0 the phosphate recovery was above 80% and the rougher concentrate grade was above 26% P O (Jordan et al, 1982). The rougher concentrate grade fell 2 5 quickly as the pH rose above 9.0. At a 3 lb/ton fatty acid and 2 lb/ton sodium silicate addition rates, a concentrate grade of 30% P O and 90% recovery were obtained. Half the sodium 2 5 silicate was added before the fatty acid collector; the rest was added prior to the cleaner flotation stage (Jordan, et al, 1982). While P O concentrates were high, the overall P O recovery from 2 5 2 5 the total clay stream was low. Shin and Choi (1985) continued the investigation of sodium silicate to better understand its selective flotation behavior among calcium minerals. Materials tested were wet-ground and sized to obtain a minus 270 mesh to plus 400 mesh fraction. The maximum amount of adsorption of sodium silicate was found to occur at pH 9.8. The amount of adsorption of sodium silicate increased with the increase in temperature of sodium silicate solutions (Shin and Choi, 1985). 107
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Several years later, another in-depth study of the role of sodium silicate was conducted by Dho and Iwasaki (1990) on Florida phosphate ore. Their research led them to conclude sodium silicate can enhance flotation efficiency through: (1) the removal of impurity minerals and calcium-bearing precipitates from quartz surfaces by dispersion, (2) drier and more persistent froths stabilized by oily droplets containing calcium silicate precipitates, and (3) higher specific flotation rates of phosphate relative to quartz, leading to faster flotation rates and increased selectivity of separation (Dho and Iwasaki, 1990). Their research involved frothability tests and continuous and batch flotation tests to compare flotation results with and without sodium silicate. Testing was conducted with a (1:1) fatty acid-fuel oil mixture, a 3.22 SiO /Na O sodium 2 2 silicate ratio and ammonia as the pH modifier. The material was conditioned for 90 seconds at pH between 9.2 and 9.4 and diluted to 25% solids prior to flotation in a 2-liter Denver laboratory flotation cell. Several observations were noted during the flotation testing, including: β€’ The tests showed more stable froths in the presence of sodium silicates than in the absence of sodium silicates. β€’ The use of sodium silicate improved both the specific flotation rates and the coefficients of mineralization of phosphate, thereby leading to increased relative floatability of the phosphate. β€’ Increasing the amount of sodium silicate prevented the entrainment of quartz particles in the froth, making it more stable (Dho and Iwasaki, 1990). 108
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Factors adversely affecting the efficiency of anionic flotation of phosphate in the absence of sodium silicate can decrease the overall concentrate grade (Dho and Iwasaki, 1990). CaCO is 3 a common precipitate in plant water, caused by the presence of Ca++ ions, which adversely affects flotation. When Ca++ is mixed with sodium silicate, calcium and silicate ions interact, resulting in the formation of calcium silicate precipitates. The main dispersive action of sodium silicate on quartz is produced by electrostatic repulsion due to calcium silicate precipitates formed on the surface of quartz (Dho and Iwasaki, 1990). The calcium silicate eventually detaches as the zeta potential of calcium silicate and quartz decreases, leaving the quartz surfaces virtually free of precipitates and thus is depressed (Dho and Iwasaki, 1990). The aforementioned test work was conducted using the conventional froth flotation technique. Several researchers have successfully floated fine phosphate from clay slimes in a column flotation cell. Fine phosphate particles (<45Β΅m) from an Egyptian phosphate mine were recovered utilizing a laboratory flotation column with a diameter of 5.04 cm by 361 cm high. Testing included the use of oleic acid as the phosphate collector and sodium silicate as the silica depressant. Test results included P O concentrate of 25.3% with a 51.52% recovery (Abdel- 2 5 Khalek et al., 2000). Similar results could not be attained with conventional flotation techniques. 3.2.2.2 Dolomite Recovery More recently, the Florida Institute of Phosphate Research (FIPR) conducted a study to optimize the Chinese dolomite collector, β€œPA-31” for use in the United States phosphate pebble industry. The Chinese Lianyungang Design and Research Institute (CDRI) had previously demonstrated the ability to reduce dolomite content in mainland China phosphate ores and were willing to assist the United States phosphate industry with their findings. The dolomite 109
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collectors USPA-31 and FAS-40A, developed by two Florida local reagent producers, produced concentrates of more than 30% P O and less than 1.0% MgO, with overall P O recoveries 2 5 2 5 averaging approximately 79% (FIPR 02-150-197, 2003). In 2003, another FIPR project (No. 00-02-145, 2003) concluded it was possible to separate dolomite from apatite by coating it with a surfactant and immersing it in a dilute acid solution where the dolomite generates carbon dioxide gas that is trapped by the surfactant and floated to the surface (FIPR 00-02-145, 2003). The preliminary study examined the effects of over a dozen different surfactants and dosages on their amenability to dolomite flotation. El- Shall and Stana found polyvinyl alcohol (PVA) to be the most promising surfactant for coating the mixture of phosphate rock and dolomite to effectively separate the two minerals. The ore is first immersed in a 3% PVA solution and mixed well prior to being added to acidic water (3% sulfuric acid). The sink product of dolomite flotation was further upgraded by either silica or phosphate flotation, achieving concentrates near 64% BPL and 1-2% MgO. While this research looks promising, additional testing will be needed on finer material to determine its feasibility in the industry. 3.2.3 Other Recovery Mechanisms One of the first tests conducted on phosphate slimes material that didn’t incorporate solely flotation testing was in 1992 at PCS Phosphate in North Carolina (TexasGulf). The North Carolina Minerals Research Laboratory (MRL) conducted a preliminary study on the effectiveness of using hydraulic classifiers (Linatex Hydrosizer) to improve the beneficiation process of North Carolina phosphate ores. The main objective of the research was to efficiently deslime feed ore (14 mesh x 0) at a cut size of 200 mesh. Less than 2% of the P O value was 2 5 110
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lost to the overflow, while over 96% of the minus 200 mesh was removed at a throughput of 0.27 stph of feed per ft2 of overflow area (Schlesinger, L.; Hutwelker, J, 1992). Prior to this study, the Linatex Hydrosizer had only been fully tested on 28 x 100 mesh material. The initial test work was deemed a success and additional testing was proposed but never carried out. While flotation is the most typical separation process, there have been several other mechanisms proposed to facilitate the separation of phosphate and gangue minerals. One of the earliest accounts of this is a patent issued by Hazen Research in 1969 (Patent No. 3,425,799) to leach the slimes with sulfuric acid under conditions that allowed crystals of calcium sulfate to form and function as a filter aid. The leach liquor was then treated with an amine solvent and processed through a solvent extraction step using ammonia. The phosphate values were recovered as diammonium phosphate. The Florida Institute of Phosphate Research sponsored a project that utilized an autoclave acidulation technique to recover phosphate from the clay stream (Zhang, 2001). At high temperature and pressure, P O was quickly recovered and minimal clay residue (35-45%) 2 5 remained as a by-product. The project was never brought to full scale due to the high capital investment cost and inconsistent acid availability. 111
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3.3 Testing 3.3.1 Equipment Setup and Sample Acquisition Sample acquisition took place during January 2004 at PCS Phosphate in White Springs, Florida. A 2-inch line from the clay launder located fifty feet above the washer floor fed a 6- inch diameter Krebs hydrocyclone and sump as shown in Figure 3.2. The hydrocyclone was initially set up with a 1.25-inch apex and a 2.5-inch vortex finder. The cyclone/sump configuration was a semi-closed system as a majority of the cyclone overflow was circulated through the system while samples were collected. Eight 5-gallon buckets of fine clay refuse stream were collected over the four day period. Three 55-gallon drums of cyclone underflow were collected and dewatered during the 4-day testing period for the subsequent conditioning and flotation test work. Additional samples of the cyclone underflow were collected, to be used as a composite of the larger bulk sample and for subsequent β€œsettling” tests. These tests were used to determine the size of the required tanks for a full-scale operation. The material was screened at 400 mesh and analyzed for BPL and insol content. After sampling was completed, all samples were shipped to Eriez Magnetics Central Research Lab (CRL) in Erie, Pennsylvania. Here, the samples were thoroughly characterized to determine the size distribution of the phosphate and gangue minerals. The concentrated underflow material was run through a 2 x 6 inch CrossFlow separator to wash the slurry of the minus 400 mesh clay material as shown in Figure 3.3. The plus 400 mesh material obtained from the CrossFlow unit was dried, riffle-split and divided into 250 gram charges to be used as flotation feed. 112
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3.3.2 Plant Hydrocyclone Testing A 6-inch diameter Krebs Hydrocyclone was utilized during the on-site testing and sample acquisition for future evaluations of a full-scale unit. The hydrocyclone was placed in series with the large mixing sump, and the circuit was set up to run continuously in a closed-loop configuration. The cyclone was situated such that the overflow and underflow could return to the feed sump by gravity. The cyclone was optimized to give the optimum size separation by varying feed pressure, vortex finder and apex parameters. The test rig was run at pressures between 20 – 28 psig with three different apexes and two different vortex finders. An analysis of these tests parameters would determine the best suited configuration to maximize the recovery of plus 400 mesh phosphate values to the underflow while simultaneously rejecting the maximum amount of clay slimes to the overflow. Five tests were conducted using the parameters as defined in Table 3.1. Table 3.1: HydroCyclone Testing Parameters at Florida Phosphate Plant. Test Operating Apex Vortex Feed U/F O/F No. Pressure Size Finder Flow (psi) (inch) (inch) (gpm) (gpm) (gpm) 1 27 1.00 2.5 190.7 16.70 174.00 2 20 1.00 2.5 na 27.30 na 3 26 0.75 2.5 na 7.70 na 4 20 0.75 2.0 160.30 10.30 150.00 5 28 0.75 2.0 250.00 10.30 239.70 Underflow and overflow samples were taken for each set of test parameters and assayed for a complete characterization and material balance at plus 150 mesh, 150x270, 270x325, 325x400 and minus 400 mesh. Table 3.2 summarizes the size distribution for each test parameter. 114
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Table 3.2: Size Distribution for Hydrocyclone Tests 1-5. Cyclone Underflow Percent (%) Retained Size Test Number Passing Retained Passing Retained Mean 1 2 3 4 5 Average *** 100 250 150 193.6 1.52 0.53 1.13 0.19 0.13 0.70 100 150 150 106 126.1 3.48 1.00 1.01 0.58 0.26 1.27 150 270 106 53 75.0 82.25 19.70 9.54 7.30 6.41 25.04 270 325 53 45 48.8 2.51 15.30 18.45 4.42 5.51 9.24 325 400 45 37 40.8 1.24 6.88 2.02 1.92 1.15 2.64 400 *** 37 *** 37.0 8.99 56.58 67.85 85.59 86.54 61.11 As described later, the cyclone underflow collected in this step was further processed in a hindered-bed classifier. 3.3.3 Detailed Testing The concentrated bulk cyclone underflow material was next run through a hindered-bed classifier. The objective of this task was to remove any residual slimes that were inherently misplaced to the coarse underflow by the cyclone. Several hindered-bed evaluations were considered to optimize the condition of the underflow material, ideally producing the minimum amount of slimes. The operating parameters were bed level (pressure), fluidization rate, and feed characteristics (i.e., rate and percent solids). The underflow from the hindered-bed classifier was then upgraded through conditioning and flotation evaluations. During conditioning evaluation, the optimum residence time, agitation intensity, and reagent dosage was established. The flotation testing includes determination of the optimum operating parameters, including aeration rate, feed rate and froth level. While ultimately the circuit will include a column cell, the initial test work was conducted with conventional flotation cells. 115
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Table 3.3: Reagents Used in Phosphate Flotation Test Work. Reagent Source Description Fatty acids: Arizona Chemical Sylva FA-1. Contains a low rosin percent PCS Phosphate Standard FA/FO. Current flotation reagent Amine: PCS Phosphate Current reagent Formula β€œD” and β€œN”. Used as a silica Na SiO : PQ Industries depressant 2 3 Alum: Fischer Scientific Used as a dolomite depressant. H O: Erie, PA water system Used in all test work. 2 3.3.4 Process Evaluation A representative sample of the fine clay refuse stream was screened at plus 150, 150x270, 270x325, 325x400 and minus 400 mesh. The size distribution of the feed is summarized in Table 3.4. A screen analysis of the cyclone underflow material was performed and size fractions were assayed for BPL, acid insol, Fe O , Al O and MgO content as shown in Table 3.5. Settling tests 2 3 2 3, were then conducted on this material for future scale up evaluation. The results of the settling tests are summarized in Table 3.6. Table 3.4: Average Size Distribution of Feed Sample. Size Individual Cumulative Mesh Microns Mass Mass Passing Retained Passing Retained (%) (%) *** 100 *** 150 1.0 1.0 100 150 150 106 3.3 4.2 150 270 106 53 3.5 7.8 270 325 53 45 0.8 8.6 325 400 45 37 0.9 9.5 400 *** 37 *** 90.5 100.0 117
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Table 3.5: Cyclone U/F Analysis by Size Fraction (Flotation Feed). Size (Mesh) Size (Microns) BPL Insol Fe O Al O MgO 2 3 2 3 Passing Retained Passing Retained (%) (%) (%) (%) *** 100 *** 150 26.64 51.61 1.16 5.94 2.00 100 150 150 106 15.11 74.28 0.98 2.98 0.58 150 270 106 53 30.25 49.64 1.09 5.86 1.45 270 325 53 45 27.57 48.02 0.89 5.34 2.70 325 400 45 37 25.79 50.18 0.61 4.89 2.97 400 *** 37 *** 18.31 58.86 2.07 8.21 2.14 Table 3.6: Cyclone Underflow Settling Tests. Post Size Pre Post Settling Settling Settling Normalized Percent Mesh Microns Average Average Average Passing Passing Retained Passing Retained Mean (%) (%) (%) (%) *** 100 265 150 199 4.1 2.8 6.0 100.0 100 150 150 106 126 0.9 0.6 1.3 94.0 150 270 106 53 75 3.5 2.4 5.1 92.7 270 325 53 45 49 2.1 1.4 3.0 87.6 325 400 45 37 41 1.0 0.7 1.4 84.6 400 *** 37 *** 37 88.4 38.7 83.1 83.1 Of the initial five tests conducted, an unacceptable 36% BPL was achieved with very high insol and magnesium content. The second series of testing was conducted several weeks later with alternative reagents and flotation techniques that provided more promising results. A total of 21 tests were conducted, with the best test achieving a 58% BPL, 1.75% MgO and 5.5% Al O . A summary of the concentrate and tailings BPL is shown in Figure 3.4, showing none of 2 3 the tests achieved the 65% BPL minimum concentrate grade. As a result, a mineralogical study was undertaken to develop a better understanding of the potential reasons for the poor results (Section 3.3.6). 118
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3.3.6 Mineralogical Investigation 3.3.6.1 SEM/EDX Introduction and Setup The clay tailings sample acquired at PCS Phosphate in White Springs, Florida in January 2004 was analyzed by at the Department of Geological Sciences at Virginia Tech on the SEM/EDX. The Geological Sciences Department at Virginia Tech owns and operates a Cambridge Instruments Camscan II Scanning Electron Microscope (SEM) outfitted with an American Nuclear Systems System 4001 EDX spectroscopy system. The system produces a qualitative, not quantitative image by either back-scattered or secondary electrons. Over a dozen different particles were thoroughly analyzed during the 2 day period, of which this report describes nine of the most common. For each particle, a snapshot was taken along with the corresponding spectrum plot. A software program called Quantum Excalibur was utilized to view the spectrum. The spectrum plot measures the energy of each peak (in keV) versus the intensity of each mineral. 3.3.6.2 Results Some general comments about what was seen on the SEM. First of all, most of the individual particles were covered with fine clay, making it difficult to get the exact components of the particle. The coating caused a significant amount of interference in the analysis. There are few samples that could be easily identified as exactly one mineral; virtually everything was a composition of Al, Si, P, and Ca, with small amounts of Mg, Cl, K, Fe and Ti. Aluminum was associated with virtually all the particles that were analyzed, as most commonly aluminum phosphate and aluminum silicate clay. There were several calcium particles that were obviously dead marine life that were virtually all calcium. Some particles 120
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3.5 Conclusions 1. Based on the SEM/EDX analysis, the clay refuse stream sample appears to be composed of about equal amounts of calcium phosphate, aluminum phosphate and silica. The presence of potassium feldspar and calcium carbonate (seashell material) was visible, but not as prominent as the aforementioned. The presence of aluminum was significant in virtually all of the particles identified, where as very little magnesium was found in comparison. As expected, the presence of β€œpure” particles is minimal as the ultra-fine material has coated all particles of any significant size. 2. The flotation results follow what is shown in the mineralogical analysis. The absence of pure apatite particles and the presence of an assortment of clay particles inhibit the successful concentration of phosphate particles by flotation. A better understanding of the interactions between the clay and apatite particles is necessary before successful completion of this task can occur. 3. After a better understanding of the clay interactions is conceived, it is believed that an acceptable concentrate grade can be achieved with further refinement of the test criteria to minimize the clay/apatite interactions. Additional flotation test work is scheduled for the near future while further research is currently being conducted on the clay interactions. 134
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Development of a Novel Air Sparging Device Andrew Reid Hobert ABSTRACT Column flotation is commonly employed in the processing and recovery of fine mineral particles due to an increase in flotation selectivity unattainable using conventional flotation methods. Such an increase in selectivity is due to the employment of wash water, minimizing hydraulic entrainment of fine gangue particles, and the presence of quiescent operating conditions assisted by the use of various air sparging technologies. High performance air spargers increase the probability of collision and attachment between air bubbles and particles, thereby improving recovery of fine and coarse mineral particles otherwise misplaced to the tailings fraction in conventional flotation cells. Although many high-pressure spargers, including the static mixer and cavitation tube, are currently employed for the aeration of column cells, a low pressure sparger capable of providing equivalent performance while resisting a reduction in aeration efficiency does not exist. In light of escalated energy requirements for operation of air compressors necessary to provide high pressure air to existing external and internal spargers, a low-pressure and porous sparger capable of resisting plugging and scaling was developed. Following the design, construction, and optimization of such a prototype, air holdup and flotation performance testing was completed to verify the viability of the sparger as a replacement to existing aerators. Performance evaluations suggest that the sparger is capable of providing similar functionality to currently employed sparging technologies, but further work is required with regards to manipulation of the porous medium to prevent sparger fouling and sustain high aeration efficiencies.
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1.0 INTRODUCTION 1.1 Background Froth flotation is a method of fine particle separation, physical or chemical, which utilizes differences in surface chemistry of minerals within a mineral/water slurry. Flotation is employed for the recovery of valuable fine grained ores, often less than 100 microns in size and either technically or economically unrecoverable by gravity concentration or other separation techniques such as magnetic separation. Through the introduction of air to a liquid pulp, air bubbles selectively adhere to naturally, or chemically altered, hydrophobic minerals and carry those solids to a surface froth phase for removal. Easily wetted, or hydrophilic, material remains in the pulp phase for removal via a tailings or refuse stream. Froth flotation can be performed using an array of established flotation technologies and methods, but is most commonly executed using mechanical and column flotation cells. Conventional froth flotation, also known as mechanical flotation, utilizes a mechanical agitator to disperse air into a mineral slurry using a rotating impeller. Conventional flotation cells are capable of yielding high mineral recoveries when operated in series, but suffer from limited product grades and non-selectivity due to short circuiting of gangue laden feed water, poor recovery of fine particles less than 20 micron, and entrainment of fine waste particles. The efficiency of fine particle flotation using conventional flotation is also poor due to the low probability of collision between fine particles and bubbles. To solve such issues and improve process efficiencies, column flotation is performed using quiescent countercurrent flows of air and feed slurry in a taller cell to eliminate intense shearing and increase flotation selectivity. The quiescent conditions provided by this flotation method improve the selective flotation of both fine and coarse particles (Luttrell & Yoon, 1993). Downward flowing wash water is also added to the froth phase to minimize the hydraulic 1
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entrainment of fine gangue particles. As a result, column flotation has become widely accepted for its ability to produce higher grade products at increased product yields. To improve mass recoveries and minimize the misplacement of high grade fine particles to the tailings or refuse stream, column flotation employs a more unique aeration method. Conversely to the employment of mechanical agitation in conventional froth flotation for the aeration of a mineral pulp or slurry, column flotation uses an array of air spargers to introduce a fine upward rising air bubble distribution at the base of a column flotation cell. The introduction of a finer air bubble distribution improves flotation kinetics and increases the total bubble surface area flux, or total available bubble surface area for mass transfer (Laskowski, 2001). Efficient and proper air sparging is vital to the success of column flotation as an increase in bubble size promptly decreases the probability of bubble-particle collision. Existing sparging technologies include, but are not limited to, porous spargers, one-phase and two-phase jetting spargers, hydrodynamic cavitation tubes, and static in-line mixers, many of which are operated using high- pressure compressed air. Given the significant horsepower requirements necessary to supply compressed air to currently operated high-pressure spargers, a low-pressure sparger operable by use of an air blower offers potentially substantial economic gains. Additionally, the capital cost of an air blower is considerably lower than that of a high horsepower air compressor. Existing low pressure spargers, such as sintered metal porous spargers, are operable at significantly lower pressures, but often suffer from plugging and diminishing performance when introduced to a mineral pulp, thereby reducing sparging efficiency and increasing air pressure demands over time. As a result, the development of a non-plugging, low-pressure sparger capable of providing equivalent metallurgical performance to both existing jetting and dynamic external spargers 2
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would provide both operational and capital cost savings in many global processing beneficiation applications that employ column flotation. 1.2 Project Objective The objective of this project was to design and develop a low pressure porous sparger capable of resisting a diminishment in performance over extended periods of use in column flotation applications. Such a sparger could be used as an alternative to existing in-line spargers employed in column flotation applications, but would be capable of operation by means of a low- pressure blower. The tasks completed in this research and development project include the design of a low pressure sparger, construction of a sparger with alterable parameters, and completion of an array of test work to verify the viability of the sparger’s performance. The sparger designed in this work effort utilizes magnetism to retain a magnetic media bed through which air is dispersed into a moving slurry. By use of a porous medium, incoming air is distributed and broken into fine air streams before introduction to a recirculated mineral pulp. Similarly to the Microcel design, air bubbles directly contact moving particles to increase the probability of bubble-particle attachment. Magnetism was strictly chosen with a goal of manipulating or rotating the internal magnetic material by movement of external magnets or an alteration in magnetic fields. Although the overall objective of this project was to design a long term non-plugging porous sparger, test work was devoted to proving the viability of the designed sparger as a means of aeration in column flotation processes. This information then makes it possible to test the sparger with several proposed cleaning concepts in both a laboratory and pilot plant setting with knowledge that the sparger is capable of providing sufficient fine and coarse particle flotation performance. 3
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2.0 LITERATURE REVIEW 2.1 Introduction to Flotation Throughout history, numerous forms of technology or processes have been developed for the separation of minerals by density, size, and chemical properties. To concentrate fine particles unrecoverable by existing technology, mineral flotation was tested and established in the mid 1800’s for the separation of minerals using differences in surface chemical properties. Following the initial patenting of a flotation concept used for the separation of sulfides in 1860 by William Haynes, the Bessel brothers designed and constructed the first commercial flotation plant, for the purpose of cleaning graphite minerals, in Germany in 1877 (Fuerstenau, Jameson, & Yoon, 2007). In addition to their innovative use of nonpolar oils to improve the process kinetics of graphite by mineral agglomeration, the Bessel brothers were the first to reportedly use bubbles, resulting from boiling, to increase flotation rates of graphite in water. Flotation continued to develop throughout the late 1800’s as multiple methods of sulfide flotation began to expand. For example, in 1898, Francis Elmore patented and implemented a process utilizing oil to agglomerate pulverized ores and carry them to the surface of water for the concentration of sulfide minerals at the Glasdir Mine in Wales (Fuerstenau, Jameson, & Yoon, 2007). The physical separation or concentration of fine particles by true froth flotation was first utilized in 1905 for the separation of lead and zinc ores from tailings dumps at Broken Hill’s Block 14 mine in Australia (Hines & Vincent, 1962). Shortly after, the Butte and Superior Copper Company built the first froth flotation plant in the United States in 1911 (Hines & Vincent, 1962). Due to the success of sulfide flotation in the early 1900’s, the use of copper in the United States grew by approximately 5.8 percent annually during that time period (Hines & Vincent, 1962). 4
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Although numerous flotation methods and flotation cells have been developed throughout mineral processing history, the conventional mechanical cell and the column cell are most common in present day mineral processing. The mechanical cell was invented in 1912 and is the most widely implemented or accepted form of flotation today. To aerate a slurry, mechanical cells, as shown in Figure 1, utilize an agitator consisting of a stator and impeller. Air is naturally drawn down the stator or delivered using a low-pressure blower, and dispersed by an impeller which agitates, circulates, and mixes the flotation pulp with the introduced air. As a result of high intensity mixing between air and solids, physical contact between particles and air bubbles occurs. Figure 1. Conventional Flotation Cell Schematic (Luttrell G., Industrial Evaluation of the StackCell Flotation Technology, 2011), Used with permission of Dr. Gerald Luttrell, 2014 Mechanical cells are beneficial in that they are capable of treating high material throughputs, but struggle with lower concentrate grades due to short circuiting of feed water to the froth phase and non-selective entrainment of fine particles. To overcome these challenges and improve overall recovery and grade, cells can be operated in series or various flotation circuits can be implemented. For example, in a rougher-cleaner circuit, the concentrate of a 5
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single rougher bank is re-floated to β€œclean” or refine the product, improving concentrate grade. Additionally, a rougher-scavenger circuit can be implemented to re-float the tailings from the rougher bank to improve overall recovery as high solids loading in a rougher bank can lead to inefficiencies in separation and misplacement of coarser material to the tailings due to froth crowding. Vast circuit configurations consisting of multiple cells and recirculation of material, as shown in the rougher-scavenger-cleaner circuit in Figure 2, provide improved recoveries and higher product grades, but equipment and operational expenditures significantly increase and efficiencies in fine and coarse particle flotation remain low. Due to its ability to improve separation efficiencies, minimize hydraulic entrainment, increase fine particle flotation selectivity, and yield higher product grades, while often requiring fewer flotation cells and reagent volumes, column flotation has flourished in the mineral processing industry. Figure 2. Rougher, Cleaner, Scavenger Flotation Circuit 2.2 Column Flotation Column flotation is a form of innovative froth flotation that uses the countercurrent flow of air bubbles and solid particles in a pneumatic cell. Pneumatic flotation, performed in a column 6
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like structure with an air sparging device, was first developed by Callow in 1914 and the concept of countercurrent flow of slurry and air within a flotation column was later introduced in 1919 by Town and Flynn, as described by Rubenstein (Rubenstein, 1995). The column flotation concept, as it is known today, was further investigated and patented in the 1960’s by Boutin and Tremblay and is currently employed in the roughing, scavenging, and cleaning of valuable minerals such as gold, copper, coal, and zinc (Finch & Dobby, 1990). Although various forms of column designs were developed in the 1970’s and 1980’s, including the Hydrochem and Flotaire column cells, the Canadian column was the first to be developed and is the most commonly implemented form of column cell in today’s processing applications, as reviewed by Dobby (Finch & Dobby, 1990). The Canadian column was first tested in the late 1960’s by Wheeler and Boutin and the first commercial column cell was installed for the cleaning of Molybdenum ore in 1981 at Les Mines Gaspe in Quebec, Canada (Wheeler, 1988). Following its successful application in molybdenum cleaning, the column cell became more widely applied for the flotation of sulfide and gold ores, as well as coal, and the cleaning of copper, lead, zinc, and tin in the late 1980’s and early 1990’s (Wheeler, 1988). The rapid employment of the Canadian column, and development of the column flotation method, in many mineral processing applications can be attributed to its ability to yield improved product grades, while increasing the recovery of both fine and coarse particles. Separation of fine particles with high specific surface areas, resulting from crushing and grinding to liberate mineral value, while concentrating a high grade product requires control of hydraulic entrainment of fine gangue particles. In comparison to the flotation performance offered by conventional, mechanically agitated flotation cells, columns yield a higher quality concentrate grade in a single flotation stage due to the removal of entrained fine gangue particles 7
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reporting to the froth through the use of wash water. Wash water showers the froth bed of the column vessel to eliminate entrained gangue minerals that degrade the product grade and replaces pulp that normally reports to the concentrate in conventional flotation methods with fresh water (Kohmuench, 2012). The flow rate of pulp to the froth concentrate must be less than the countercurrent flow of wash water to minimize non-selective recovery of ultrafine gangue (Luttrell & Yoon, 1993). Column cells, as shown in Figure 2, are also built with a smaller cross sectional area to maintain a deeper and more stable froth bed necessary for froth washing. In addition to froth washing and the use of a deep froth, column flotation promotes quiescent operating conditions and utilizes air spargers to improve flotation selectivity and fine particle recovery, respectively. Unlike conventional flotation cells, taller column cells, reaching up to 16 meters in height to permit necessary particle residence times, utilize high-pressure internal or external spargers for very fine air bubble introduction. Air, or an air/water mixture, is injected at the base of the cell, via an arrangement of spargers, as feed is introduced below the froth bed, developing a countercurrent flow of feed particles and air bubbles. Due to lower traveling velocities of both bubbles and particles during column flotation, collision and attachment between the two are more likely. Increased contact time between air bubbles and particles under quiescent operating conditions decreases the probability of hydrophilic particle attachment. Such conditions also greatly improve coarse particle collection efficiency as coarse particles are less likely to detach from air bubbles under less turbulent conditions present within column cells. Due to the use of wash water and a deeper froth bed, a large quiescent pulp or contact zone, and various air sparging technologies, column flotation presents the most ideal separation environment in a single flotation stage. 8
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Essentially, column flotation presents a multi stage flotation circuit within one cell, illustrated by the development of the MicrocelTM by Luttrell et al. (United States of America Patent No. 5761008, 1988). For example, the pulp zone or bubble-particle contacting region represents a rougher stage as hydrophobic particles adhere to air bubbles and are carried to the froth phase in this zone. Additionally, a deep froth and wash water are used to clean the concentrate of hydraulically entrained fine gangue particles to represent the cleaning phase of a multi-state circuit process. Lastly, external air spargers are often utilized to directly introduce air to a circulated tailings stream, scavenging possibly misplaced fine hydrophobic particles. As a result, column flotation is increasingly preferred for the flotation of finer particle size classes to improve recovery and concentrate grade. Figure 3. Flow of Water in a Column Flotation Cell (Luttrell G., Industrial Evaluation of the StackCell Flotation Technology, 2011), Used with permission of Dr. Gerald Luttrell, 2014 Although column flotation produces superior product grades than those yielded by conventional flotation, consideration must be given to carrying capacity for proper cell design. 9
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Carrying capacity, in pounds or tons per hour per square foot, is the mass rate of floatable solids that can be carried by a given superficial gas velocity. As described by Luttrell, a column cell must be scaled according to its carrying capacity due to an inherently smaller ratio between column cross sectional area and volume when compared to conventional flotation cells (Luttrell & Yoon, 1993). The equation for carrying capacity, in mass rate of concentrate solids per unit of cell area, is as shown: C = 4 Q D ρ β / D [1] g p b where β is a packing efficiency factor, ρ is the particle density, D is the particle diameter in the p froth, D is the bubble diameter, and Q is the gas flow rate. To achieve optimal carrying capacity b g conditions, column cell spargers are operated at maximum allowable air velocities, while maintaining the minimum average bubble size. The maximum air flow rate is governed by the bubble size and V , or superficial liquid velocity in the cell. Particle residence times are also L higher in column flotation due to a taller pulp zone and the naturally slower rise of small bubbles. Given increased particle residence times present using column cells given their geometry, work has been completed to develop flotation technology which offers column-like performance with significantly reduced particle residence times. In addition to the column cell, further work has been done in recent years by the Eriez Flotation Division to develop an innovative form of flotation technology labeled the StackCell (Kohmuench, Mankosa, & Yan, 2010). The StackCell, as shown in Figure 4, offers column-like performance with shorter particle residence times, improved bubble-particle contacting, and a reduced unit footprint per processed ton of material (Kiser, Bratton, & Kohmuench, 2012). Unlike typical column cells, the StackCell utilizes an aeration chamber to agitate and mix the feed with air in a high intensity shearing zone. By the act of intense agitation, low pressure air, 10
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introduced to the slurry before entrance to the aeration chamber, is sheared into small bubbles for collection of fine particles. High particle concentration and gas fraction within the chamber greatly reduces particle residence times. Additionally, the use of low pressure air and the turbulent environment within the pre-aeration chamber decreases energy requirements as energy is primarily consumed in bubble-particle contacting instead of particle suspension (Kiser, Bratton, & Kohmuench, 2012). The mixture of slurry and air lastly overflows into a short, column like tank, where froth and pulp are separated. A deep froth bed is maintained and froth wash water is employed with the StackCell design to reduce hydraulic entrainment, similarly to column flotation. Due to their compact size and ability to be stacked in unison, stackcells offer much friendlier orientation in a processing plant than column cells, which are much larger and require more structural steel for support and allowance of de-aeration of the froth before reporting to the dewatering circuit (Kohmuench, Mankosa, & Yan, 2010). Figure 4. Schematic Illustration of a Single Eriez StackCell (Kohmuench, Mankosa, & Yan, Evalutation of the StackCell Technology for Coal Applications, 2010), Used with permission of Dr. Jaisen Kohmuench, 2014 11
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2.3 Column Flotation Performance Flotation performance is influenced by many factors including froth depth and structure, slurry flow characteristics, flotation cell dimensions, wash water utilization, chemical additions, and gas holdup. Air holdup in a gaseous-liquid mixture is primarily controlled by bubble size or frother dosage, superficial gas velocity, slurry density, and superficial or discharge liquid velocity, as detailed in studies completed by Yianatos et al, and Finch and Dobby (Finch & Dobby, 1990; Yianatos, Finch, & Laplante, 1985). Column cells are typically operated with a 12 to 15 percent gas holdup, or percentage of air in a gaseous-liquid volume. Superficial gas velocity and gas holdup maintain a positive linear relationship, in what is known as the homogenous bubbly flow regime, until gas flow rate becomes too significant (Finch & Dobby, 1990). At this point, air begins to coalesce, bubble size uniformity is lost, and water is displaced to the froth phase. To illustrate the reaction of a typical flotation bank as gas flow rate is increased, the effect of superficial gas velocity on the recovery and grade curve of a Mt. Isa copper rougher flotation bank is shown in Figure 5. As superficial gas velocity was increased, copper recovery also increased, but copper grade diminished due to increased recovery of gangue material. Although not evidenced in Figure 5, instigation of air coalescence quickly decreases recovery. As stated by Finch and Dobby, development of very large and quickly rising air bubbles will create a churn-turbulent regime within a flotation column as superficial gas velocity exceeds approximately 3 to 4 cm/s (Finch & Dobby, 1990). Coalescence of air quickens the rise of air in a column and increases mean bubble diameter, decreasing total bubble surface are and diminishing bubble-particle collision efficiency. 12
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Figure 5. Effect of Aeration rate on the Grade and Recovery Curve for a Copper Ore (Finch, Mineral and Coal Flotation Circuits, 1981), Used under fair use, 2014 As gas holdup increases, the probability of bubble-particle collision also increases as the availability of bubble surface area for mass transfer escalates. This is due to a decrease in bubble size or increase in gas flow rate, both of which control the bubble surface area rate, or S . The b bubble surface area rate is the ratio between superficial gas velocity and bubble sauter diameter. The equation for S is as follows: b S = 6V /D [2] b g b where D is the diameter of bubbles and V is the superficial aeration rate (Luttrell & Yoon, b g 1993). Probability of collision between a particle and bubble is predominantly dependent upon particle diameter, bubble diameter, and bubble Reynolds number. Yoon and Luttrell (1989) derived an equation for collision probability that states that as bubble diameter decreases or bubble Reynolds number increases, the probability of collision between a bubble and particle increases. Their derived equation for probability of collision is written as follows: 𝑃 = [3 + 4𝑅𝑒0.72 ](𝐷𝑝)2 [3] 𝑐 2 15 𝐷 𝑏 where D represents the particle diameter, D is the bubble size, and Re is the bubble Reynolds p b number. As particle size decreases, the probability of collision and attachment between a particle 13
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and bubble also decreases (Yoon & Luttrell, 1989). Ralston et al. also derived mathematical equations which suggest that the probability of bubble-particle attachment decreases if particles are too coarse as air bubbles become unable to retain such heavy particle loads (Ralston, Dukhin, & Mischuk, 1999). Although bubble size must be minimized at a maximum allowable superficial air velocity to increase the probability of fine and coarse particle collision and attachment, hydraulic entrainment of gangue laden water must also be managed to maximize product grade. During operation of a column flotation cell, proper bias water rates and froth depths must be utilized to minimize hydraulic entrainment. The effect of wash water utilization on the hindrance of short-circuited feed water to the concentrate is shown in Figure 6. As evidenced by the column flotation tracer study displayed in Figure 6 (Left), employment of wash water cultivates a clean interface free of pulp water contamination. Figure 6. Tracer Study showing the effects of Wash Water Utilization Bias is a measurement of the percentage of wash water which reports to the pulp; the remainder of water reporting to the froth zone. According to Dobby and Finch (1990), an adequate bias rate and froth depth are essential to control concentrate grade as gas flow rates are commonly maximized to improve column carrying capacity. Although wash water is required to optimize the particle cleaning process, a minimum bias rate is recommended, up to 80 percent of 14
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which should flow to the concentrate, to prevent short circuiting of material to the overflow, maximize capacity, and ensure mobility of the froth (Finch & Dobby, 1990). Insufficient wash water will lead to a reduction in product grade and a concentrate flow rate greater than that of the wash water. In laboratory and pilot scale testing, a froth depth of greater than one half meter is suggested for gas rates exceeding 2 cm/s to diminish the feed water concentration in the froth zone (Finch & Dobby, 1990). In addition to the many column cell operational parameters which effect flotation performance, chemical reagents are most intrumental in the flotation of many naturually hydrophilic materials. Although some minerals or rock types, such as coal, are naturally hydrophobic, bubble- particle attachment is strongly dependent upon chemical reagents such as collectors, activators, depressants, and pH modifiers. Collectors (anionic, cationic, or nonionic) are used to generate a thin, nonpolar hydrophobic layer around a particle, rendering it hydrophobic. Selection of collector is dependent upon the charge, positive or negative, or the chemical make-up of the mineral to be floated. Activators and depressants are then used to allow or prevent the collector from physically or chemically adsorbing to a mineral surface, respectively. Lastly, and very importantly, pH modifiers are necessary to control the charge of minerals as a minerals’ charge often becomes more positive as a solution decreases in pH from alkaline to acidic conditions. In addition the importance of collectors and other chemical reagents in promoting the development of bubble-particle aggregates, frother type and dosage dictate both bubble size and rise velocity within a flotation cell. Frother can be either a water soluble or insoluble polymer that stabilizes the dispersion of air bubbles in a flotation pulp by decreasing its surface tension. As surface tension declines, bubble population grows and average bubble diameter decreases. Although many frothers have been developed, the two main classes of frother are alcohols and 15
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polyglycols. Polyglycols help to quickly stabilize a froth, while alcohols are used to expedite the increase of gas holdup (Cappuccitti & Finch, 2009). Much work has been performed to generate relationships between gas velocity and gas holdup using numerous frother types and concentrations (Yianatos, Finch, & Dobby, 1987; Finch & Dobby, 1990; Lee, 2002). Typically, as frother concentration increases, in parts per million, mean bubble diameter reduces and gas holdup rises. In addition to the calculation of gas holdup within a laboratory column using a measurement of pressure differential and pulp density, methods of measuring and mathematically estimating bubble sizes using photography have also been developed to better understand the effects of numerous flotation operating parameters (Yianatos, Finch, & Dobby, 1987). Although operational set-points can be altered to impact flotation recovery and grade, the actual method of bubble generation is integral in obtaining desired flotation performance. 2.4 Flotation Sparging In column flotation processes, internal and external spargers are utilized to introduce and disperse air into a liquid-mineral pulp. Proper sparger design and performance is essential to column flotation as spargers are used control bubble size, air distribution, and air holdup within the flotation column. External spargers are used to aerate a moving slurry which is pumped from a flotation cell bottom and recirculated as a pulp-air mixture to the column; whereas internal spargers inject air or an air-water mixture directly to the flotation cell. External spargers and some internal spargers, such as the Eriez SlamJet, have expedited the development of column flotation as they can be maintained during operation of the column and are easily operated. Since the development of column flotation, numerous spargers have been established and industrialized to improve bubble dispersion, minimize bubble size, decrease operational costs, and reduce maintenance difficulties. 16
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As expressed by Rubenstein (1995), Callow developed the first pneumatic column flotation sparger in 1914 using a perforated metal frame that was wrapped in a woolen cloth. Air was then introduced to a slurry through the covered frame. Many similar spargers were proposed and tested in the early to mid-1900’s, but all suffered from plugging, improper distribution of air, and poor reliability. As sparging technologies have rapidly developed and improved in the last few decades, the popularity of column flotation has grown. Although the overall goal of air sparging remains constant for each type of sparger; the design, sparging method, and features vary substantially between sparger types. Due to differences in operating conditions present in a laboratory in comparison to those found in industrial applications, certain low pressure sparging devices are only feasible in a laboratory setting. Though sparging is applied to industries outside of mineral processing, column flotation sparging for the purpose of valuable mineral recovery will be strictly examined in this report. A detailed explanation of the design and operation of existing spargers in mineral flotation applications is provided to illustrate the advancements and differences in column flotation sparging technologies. 2.5 Internal Spargers 2.5.1 Low Pressure Perforated and Porous Spargers The perforated sparger characterizes the beginning of sparging in a pneumatic flotation cell. Sparging devices developed in the early 1900’s for use in pneumatic columns often consisted of a perforated metal frame or structure through which low pressure air was introduced, sometimes inclusive of a porous filter cover. Filter cloth covers were used to generate finer bubble sizes at low pressures, but suffered from fouling or degradation over extensive periods of use. As a result, various materials, such as glass, ceramic, and fabric, have been used in construction of more rigid porous spargers, but the sintered metal sparger has 17
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become the most widely accepted form of porous sparger. This is due to its rigid construction and ability to produce the most uniform dispersion of fine air bubbles of existing low pressure porous aerators. Sintered metal spargers are comprised of powdered metal which has been fused together due to subjection to heat near the metal’s melting point (Mott Corportation, 2014). The average pore size of sintered metal spargers ranges from 60 to 100 microns; therefore allowing the production of extremely fine bubbles (Mott Corportation, 2014). Mouza and Kazakis (2007) studied the effects of porous sparger aperture size and found that sintered metal spargers with a smaller average pore diameter have a more uniform porosity and therefore maintain a more even air distribution (Kazakis, Mouza, & Paras, 2007). According to a study performed by the University of Florida, the average diameter of a bubble emitted from a sintered aluminum or stainless steel sparger ranges from 0.7 to 0.9 millimeters (El-Shall & Svoronos, 2001). Although sintered metal spargers are capable of producing a more fine bubble distribution when compared to other internal and external sparging methods, sintered metal spargers likewise possess the inability to resist plugging when exposed to a slurry or pulp in an industrial environment. Such sparging inefficiencies have primarily been documented in wastewater treatment applications and the separation of oil and water. As reviewed by Rosso (2005), periodic cleaning of fine pore spargers using water and acid is necessary to prevent a rapid performance decline in wastewater treatment applications due to slime plugging. In a study of porous sparger aearation efficiencies in wastewater treatment applications, diminishing sparger performance was obvious in 21 analyzed wastewater facilities (Rosso & Stenstrom, 2005). Porous spargers require filtered air and water to promote successful continuous flotation and minimize performance deterioration, both of which are not feasible in most industrial beneficiation plants. Single and two-phase porous spargers are sometimes applied 18
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in de-inking flotation, wastewater treatment, and in the separation of oil and water, but are primarily used in a laboratory setting in mineral flotation efforts due to uneconomical maintenance requirements. A single phase sintered metal sparger introduces air only through a porous membrane within a column cell, whereas a two phase sintered metal sparger, as shown in Figure 7, injects air through a porous medium surrounding the circumference of a moving stream of water. The aerated liquid then flows into the column or aerated tank. Figure 7. Two Phase Sintered Metal Porous Sparger (El-Shall & Svoronos, Bubble Generation, Design, Modeling and Optimization of Novel Flotation Columns for Phosphate Beneficiation, 2001), Used under fair use, 2014 2.5.2 Single and Two Phase Jetting Spargers In addition to low pressure porous spargers or bubblers, the US Bureau of Mines (USBM), Cominco, and Canadian Process Technologies (CPT) have developed various forms of high pressure jetting internal spargers. In contrast to the operation porous spargers, the jetting action of these high pressure spargers allows for the emergence of numerous air bubbles from a single or multiple orifices with a reduced risk of plugging. Although sparger fouling is less likely at higher pressures, horsepower requirements for the generation of higher air pressures greatly increase operational costs. Cominco and USBM produced the first two phase, high velocity internal sparger that mixes both water and high pressure air before injecting the air/water mixture into the column cell through a perforated pipe. To improve the distribution of water in air, USBM also formulated a model that uses a bead filled mixing chamber to mix water and high pressure air streams. Water addition is used to shear the incoming air, therefore creating a finer 19
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bubble distribution (Finch, 1994). To improve the concept of on-line maintenance, unattainable by USBM and Cominco spargers, CPT later industrialized a single air phase SparJet sparger. The SparJet is a removable air lance that ejects high velocity air from a single orifice through the column wall. Multiple air lances of varying length can be instrumented around the column perimeter to aerate the full cross sectional area of the column. To adjust the air flow through the sparger orifice or to close the orifice in the event of pressure loss, a t-valve is located at the opposite end of the sparger to increase or decrease the total orifice area. CPT later replaced the needle valve with a high tension spring that controls the orifice area depending upon the provided air pressure. The spring is located at the sparger end opposite the orifice and is used to control the position of an internal rod relative to the sparger tip. If air pressure is lost, the spring closes the orifice of the SlamJet to prevent the backflow of slurry into the air system (Kohmuench, 2012). As detailed by Finch, a long air jet length stretching from the sparger orifice is desired to increase the total population of bubbles. By increasing the density of air by addition of water, the jet length increases and bubbles become finer (Finch, 1994). As a result, EFD enhanced the SlamJet, pictured in Figure 8, with the addition of water as high pressure air and water enter the lance together. Multiple SlamJet spargers consisting of unique orifice sizes exist for any specified flotation duty. The largest SlamJet is operated at pressures in excess of 80 psi for optimal performance in fine coal flotation. The SlamJet sparger is commonly used in flotation of a somewhat coarser feed or deslime circuits which require less collision energy (Kohmuench, 2012). For the flotation of finer particles less than 325 mesh in size, external spargers using direct rapid bubble-particle contacting have been developed. 20
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Figure 8. Eriez SlamJet Sparger (CPT, Canadian Process Technologies, Sparging Systems - SlamJet Series), Used with the permission of Dr. Michael Mankosa, 2014 2.6 External Spargers 2.6.1 Static Mixer/Microcel Many internal spargers suffer from limited control of bubble size, plugging of openings, low collision energies, and poor on-line maintenance capabilities; therefore the development of external spargers such as the static mixer and cavitation tube have greatly expanded the use of column flotation through the use of microbubbles and picobubbles in mineral processing applications. In the mid 1980’s, Luttrell et al. invented and patented the MicrocelTM flotation column using a static in-line mixing sparger for the purpose of bubble particle contacting (United States of America Patent No. 5761008, 1988). A static mixer, as shown in Figure 9, is a tube consisting of a series of geometric shapes used as air-slurry mixing components. Potential tailings slurry is removed from the column bottom using a pump and is delivered to a static mixer in addition to high pressure air supplied before the mixer inlet by an air compressor. Significant air pressure of at least 50 to 60 psi is required for proper operation of industrial scale static mixers to provide 40 to 50 percent air in slurry by volume and to overcome the 20 to 25 psi pressure drop experienced by the air-slurry mixture following its movement through the static mixer. The aerated slurry is then recirculated to the flotation column. Microbubbles generated using a static mixer range from 0.1 to 0.4 mm in size and vastly increase the rate of flotation as bubbles remain small at increased superficial gas velocities (Luttrell, 21
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Yoon, Adel, & Mankosa, 2007). Using a static mixer, high separation efficiencies are realized as a result of a decrease in bubble diameter which increases probabilities of collision and attachment and decreases the probability of bubble-particle detachment. Figure 9. Microcel Static Mixer Sparger (Luttrell, Yoon, Adel, & Mankosa, The Application of Microcel Column Flotation to Fine Coal Cleaning, 2007, pp. 177-188), Used with permission of Dr. Gerald Luttrell, 2014 As reviewed by Luttrell (2007), the use of a static mixer, or other external sparging technologies, in column flotation applications allows for the development of a three stage flotation process within one cell (Luttrell, Yoon, Adel, & Mankosa, 2007). This is illustrated by the successful functionality of the MicrocelTM. As air rises within a flotation column, downward flowing hydrophobic particles collide and attach to air bubbles in the pulp zone in a roughing stage. Risen bubble-particle aggregates are then washed or cleaned in the froth bed to minimize hydraulic entrainment in a cleaning stage. Lastly, the implementation of direct rapid particle contact within a static mixer recycle circuit gives particles a final opportunity for attachment to air bubbles in a scavenger phase. This multi-stage process, as shown in Figure 10, represents a distinct advantage of column floation that is made possible using external in-line spargers such as the static mixer and cavitation tube. To demonstrate the value of a static mixer sparging apparatus in the cleaning of fine coal, Luttrell et al. (2007) completed a flotation test program on multiple minus 28 mesh coal samples 22
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using both column and conventional flotation methods. The separation efficiency, or difference between the combustible recovery of coal and ash recovery, was 6 to 16 percent greater using a single twelve inch diameter column equipped with a static mixer than a bank of four, three cubic foot conventional cells (Luttrell, Yoon, Adel, & Mankosa, 2007). In addition to its application in fine coal flotation, the static mixer has also displayed proven performance in coarse particle flotation. In a coarse phosphate flotation study performed at the University of Kentucky (2006), both a static mixer and porous sparger were individually employed for the flotation of a minus 1.18 mm phosphate ore. The effect of a given sparger type on the concentrate grade and total phosphate recovery was determined at varying gas velocities. At the optimum operating point, or elbow of the P O recovery and grade curve, established for each sparger, the static mixer 2 5 provided twelve percent higher phosphate recovery at a slightly better concentrate grade than the porous bubbler (Tao & Honaker, 2006). Figure 10. MicrocelTM Process Diagram (Luttrell, Yoon, Adel, & Mankosa, The Application of Microcel Column Flotation to Fine Coal Cleaning, 2007, pp. 177-188), Used with permission of Dr. Gerald Luttrell, 2014 23
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2.6.2 Cavitation Sparging In addition to the static mixer, hydrodynamic cavitation based spargers function as in-line aerators utilized in fine particle flotation. Cavitation is the formation of cavities or bubbles within a liquid due to rapid changes in fluid pressure. Bubbles or cavities begin to open up within a liquid at the location of highest fluid velocity where pressure is negative in an attempt to relieve pressure (Zhou, Xu, & Finch, 1993). Such fluctuations in pressure are obtained by the alteration of liquid velocities using a venturi tube configuration. To induce hydrodynamic cavitation in sparging applications, slurry pressure is reduced below its vapor pressure through an area constriction, increasing slurry velocity, and is then returned above its vapor pressure following an increase in slurry flow path cross sectional area. In addition to deviations in fluid pressure, the presence of solid particles and high gas flow rates both help to promote the development of cavities. As discovered by Zhou (1993), high dissolved gas volumes and the addition of frother to decrease the surface tension of a slurry prevent the collapse or implosion of bubbles in the cavitation process, allowing for the successful flotation of fine particles. Using hydrodynamic cavitation, the bubble-particle collision stage is further assisted as bubbles directly form on hydrophobic surfaces immediately during cavitation (Zhou, Xu, & Finch, 1993). Although several spargers are operable using the principles of hydrodynamic cavitation, the cavitation tube, developed by Canadian Process Technologies, is the most cost effective, high performing, and wear resistant cavitation based sparger. Other spargers which rely upon hydrodynamic cavitation include the eductor and two phase ejector, both of which use a parallel throat and diffuser to promote cavitation, but are not operated in-line with recirculated middlings or tailings streams (El-Shall & Svoronos, 2001). The cavitation tube, as shown in Figure 11, is a completely in-line aerator constructed of a wear resistant material in the shape of an hour glass. 24
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Using an hour glass configuration, slurry pressure is rapidly lowered and increased to support cavitation. Wear resistivity of the inner hour glass lining and the lack of internal mechanisms within the cavitation tube are noteworthy as the static mixer relies upon a series of mixing components in the direct line of slurry flow. Unlike the eductor or two phase ejector, the cavitation tube, now produced by the Eriez Flotation Division, does not employ a feed jet nozzle or air-slurry mixing chamber before entrance to a cavitation inducing structure. Figure 11. Eriez Cavitaton Tube Sparger (Canadian Process Technologies, Cavitation Sparging System), Used with the permission of Dr. Michael Mankosa, 2014 Similar to the operation of the static mixer, a pressure drop of approximately 20 to 25 psi occurs across the length of a cavitation tube as a result of rapid modifications in liquid velocity. An operating pressure of 50 to 60 psi is also recommended for industrial applications. As reported by Kohmuench, cavitation tube sparging is common to fine, by-zero, coal circuits that are operated under significant material throughputs as a result of the sparger’s ability to formulate numerous bubbles less than 0.8 mm in size (Kohmuench, 2012). The benefits of cavitation and picobubble sparging in fine particle flotation are also evidenced by improvements in product recovery in the flotation of both zinc sulfides and phosphates (Zhou, Xu, & Finch, 1997; Tao & Honaker, 2006). A cavitation tube was used to pre-aerate the feed to a conventional cell and in unison with a static mixer in each scenario, respectively. 25
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2.7 Sparger Comparisons The air holdup, or percentage of air within an aerated pulp, is directly related to the bubble size generated by a given sparger type and the associated superficial gas velocity. As average bubble size decreases, the air or gas holdup directly increases. Air holdup also increases as a result of an increase in superficial air velocity, until air begins to coalesce. In a study of various sparging technologies conducted at the University of Florida (2001), the performance of multiple sparger types was reviewed under changing operating conditions. Most importantly, the test effort analyzed the effects of increasing superficial air velocity on both the air holdup and bubble size produced by each analyzed sparger. During the sparger performance analysis, a one- phase porous sparger provided the greatest air holdup as gas flow rates were increased, but cavitation based spargers generated the finest bubble sauter diameter, as small as 0.4 mm, at low superficial air velocities (El-Shall & Svoronos, 2001). A complete assessment of the air holdup produced by porous, perforated tube, static mixer, hydrodynamic cavitation based, and jetting spargers as superficial air velocity was increased is shown in Figure 12. As evidenced by this figure, sparging method strongly dictates the relationship between a specified superficial air velocity and resulting air holdup within a flotation column cell. 26
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Figure 12. Comparison of Performance for Various Spargers (El-Shall & Svoronos, Bubble Generation, Design, Modeling and Optimization of Novel Flotation Columns for Phosphate Beneficiation, 2001), Used under fair use, 2014 In an analysis of the sparging performance generated by the selection of aerators, in terms of air holdup, it is apparent that similar sparging methods provide varying results at increasing superficial air velocities. For example, the one and two phase porous spargers are comprised of an identical porous sintered medium, yet the air holdup generated by the single phase sparger was two to three times greater at increased air velocities due to an escalation in bubble population and lower bubble entrance velocities. In comparison to the two phase porous sparger, the static mixer produced a similar minimum bubble size of 0.7 mm, but at slightly greater gas holdup percentages as air rates were increased. Although the air holdup induced by the static mixer and two phase porous sparger were much less than that of a one phase porous sparger, this study did not consider the effect of increased bubble rise velocities resulting from the use of high velocity fluid flows. It is also possible that an insufficient recirculation liquid velocities were delivered to the static mixer as the superficial air velocity was increased. 27
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Although an in-line cavitation tube was not evaluated in this test effort, other hydrodynamic cavitation based aerators were assessed, such as the eductor and two phase ejector spargers. Each of these cavitation sparging technologies supplied an average bubble diameter and air holdup equivalent to those yielded by a single phase porous sparger. Typically, external spargers provide superior air holdup, fine bubble diameters, and increased bubble-particle contacting necessary to optimize flotation performance, but operational costs are great due to the utilization of significant compressed air volumes. To further support the advantages of both static mixer and cavitation tube technologies, the University of Kentucky conducted a phosphate flotation review using multiple sparger types. As reviewed by the University of Kentucky, the use of a static mixer or cavitation tube to decrease particle detachment increases the recovery of a 16 x 35 mesh phosphate ore considerably (Tao & Honaker, 2006). However, using a single phase porous sparger, phosphate recovery remained significantly lower, as apparent in Figure 13. Figure 13. Effect of Implemented Sparger Types on Phosphate Recovery (Tao & Honaker, Development of Picobubble Flotation for Enhanced Recovery of Coarse Phosphate Particles, 2006), Used under fair use, 2014 28
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3.0 EXPERIMENTAL Seeing an opportunity to reduce operational costs associated with column flotation sparging systems, the Eriez Flotation Division designed an innovative low pressure drop sparger capable of resisting plugging and degradation. In design planning of an in-line, non-plugging, and porous sparger, it was determined that magnetic material be employed as a medium through which air be dispersed and introduced to a moving slurry. Such a sparger would maintain an inherently low pressure drop due to the use of a slurry flow path of a uniform cross sectional area and the absence of any in-line mixing components. Alternatively, such a porous sparger would rely upon the dispersion of air through more narrow paths, allowing for the introduction of fine bubble streams from a magnetic media bed. Upon entrance to the flow path, bubble streams would undergo further shearing as a result of high velocity liquid flows. Magnetic material was chosen for the fact it can be manipulated using changes in magnetic fields or movement of host magnets to clean the material during operation. In addition, magnetic material can be structured without need for screens or mesh material to hold the media in place; therefore eliminating the possibility of plugging of apertures through which air must travel. Using the theoretical concept of directing air through a porous magnetic media for the purpose of aerating a recycled slurry stream, a lab-scale magnetic sparger was designed, constructed, and tested at the Plantation Road Facilities in the Mining and Minerals Engineering Department at the Virginia Polytechnic and State University. Although the full scope of the project is to ensure the magnetic material can be cleaned, the first stage of the project was focused on designing of the sparger itself and testing the concept of aerating a slurry through in-line injection of air through a porous magnetic media bed. Before flotation testing progressed, sparger aeration performance was first evaluated under air, water, and frother only conditions. 30
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3.1 Sparger Development A preliminary prototype was first constructed using a ring magnet assembly, as shown in Figure 14. This approach was first taken to stem from previous research completed by the Eriez Flotation Division, which consisted of aerating a moving coal slurry by the injection of air through the crevices of multiple β€œin-line” flexible discs. Each disc was identically milled or grooved to promote undeviating aeration of the coal slurry. Although such a novel sparging device yielded both a fine bubble dispersion and high fine particle recovery, grooved air paths began to plug within hours of being subjected to a 15% solids coal slurry. Aperture plugging resulted in a decrease in recovery and air distribution. Using this aeration concept, it was believed that ceramic magnets, protected or layered by a magnetic medium, could be used to alter the previously tested sparger design to prevent the plugging of crevices and create a filter through which air must travel. Figure 14. Conceptual Diagram of In-Line Magnetic Ring Sparger The constructed prototype, inclusive of an inner perforated pipe to introduce air from behind a surrounding group of ceramic ring magnets, is shown in Figure 15. Both ends of the sparger were tapered to allow moving slurry to more evenly flow past the surface of the sparger for uniform aeration. Rubber gaskets were employed at either end of the ring magnet collection, simulating a spring, to allow for expansion of gaps between magnets to support air flow. For the purpose of this effort, sparger air distribution was observed within a clear water tank. Analogous to the performance of the disc sparger, the ring magnet sparger produced a predominantly fine 31
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bubble flux, but air distribution was uneven and large bubbles were frequently emitted from the sparger surface at confined locations due to inconsistent magnet contruction and magnetic grit. During limited static water testing, ceramic magnets also became worn quickly, further hampering aeration uniformity. Figure 15. In-Line Magnetic Ring Sparger Due to the rapid deterioration of ceramic magnets when introduced to water or high velocity slurries, an improved magnetic sparger was designed to ensure that primary magnetic elements be kept external to slurry or liquid flows in a dry environment. Preservation of magnets external to slurry flow also allows for easier manipulation of magnetic fields or the magnetic medium itself for cleaning purposes. To protect ceramic magnets, improve air distribution, and simplify operation, an external in-line sparging flow box was constructed, as shown in Figure 16. To aerate a recycled slurry or liquid using the designed magnetic sparger, a magnetic medium is held perpendicular to liquid or slurry flows by use of external ceramic magnets as incoming air is dispersed through the medium to dynamically aerate a liquid or solids-liquid mixture. A plexi- glass side housing was used on either side of the sparger to observe the aeration process throughout the testing effort. 32
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Figure 16. MagAir Sparger Prototype Design The external magnetic sparger was designed with completely alterable parameters to better understand their effect on sparging performance due to a lack of research or pre-existing information regarding design of such an aerator. These parameters included cross sectional area of the liquid or slurry flow region, magnetic medium bed depth, and magnetic bed area. The sparger, as presented in Figure 17, was assembled with a two inch by two inch cross sectional area and a length of 28 inches. At the sparger’s inlet, a 1 ΒΌ inch pipe nipple and union were utilized to feed the sparger and easily remove it from the testing set-up, respectively. Additionally, a two inch by two inch square pipe was affixed to the outlet end of the sparger in replacement of a succeeding pipe nipple. This allowed a constant cross sectional area to be maintained following the introduction of air to prevent the coalescence of air prior to departure of the aerated liquid from the sparger. A one inch interchangeable spacer, as shown in Figure 17 (left), was also fabricated in order to decrease the cross sectional area of flow to increase the liquid velocity across the magnetic media bed to overcome pumping limitations. 33
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Figure 17. External Magnetic Flow-Box Sparger Design Within the air inlet chamber perpendicular to the slurry flow region, an adjustable perforated pedestal and slots of fixed height increments were engineered to allow for preparation of a magnetic bed of desired depth. The air chamber was constructed 2 Β½ inches in length and assembled equal in width to the flow region (2”) to ensure complete and even air distribution across the recirculated slurry or liquid. The perimeter of the perforated pedestal was wrapped in an aluminum tape and caulked to promote air distribution and prevent the short-circuiting of air around the media bed along the chamber walls. Magnetic material was contained by the air inlet compartment and held flush with the liquid flow region boundary by use of two large ceramic magnets on either side of the air chamber, external to the sparging device. Due to the generation of a strong magnetic field, the aluminum pedestal was magnetized and therefore created a level foundation for the media bed to compact and rest upon. Opposite the air pedestal, a threaded magnetic feed hole was created to allow magnetic material to be fed onto the perforated pedestal without needing to disassemble the sparging apparatus. This permitted easier transitions between testing of different media types during aeration performance testing. 34
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3.2 Equipment Setup and Test Work 3.2.1 Gas Holdup Testing To verify the magnetic sparger’s aeration capabilities and optimal operating parameters, a test assembly was developed to quantify the air holdup produced by the sparger under various equipment arrangements and functional conditions. In air holdup testing, water and an MIBC frother were strictly utilized. Mineral slurry or pulp was not employed for these exercises to allow for complete visualization of the process within the sparger and the succeeding de-aeration liquid holding cell. Dynamic external spargers are often operated with a combined air and liquid velocity of 17 to 20 ft/s, therefore a variable speed centrifugal pump was instrumented to produce an array of water flows. Optimal arrangement and installation of the sparger was first defined using a simple recycle system consisting of a 20 gallon sump and centrifugal pump. Both horizontal and vertical sparger orientations were implemented to understand the effect of sparger positioning on air pressure requirements and liquid-air mixing, as shown in Figure 18. Horizontal orientation of the sparger was quickly neglected as air naturally rose and coalesced at the ceiling of the sparger upon introduction through the magnetic medium. A bottom fed vertical orientation promoted the mixture of air and water and decreased the coalescence of air, but increased the air pressure required for aerator operation. Such an increase in air pressure was attributed to an increase in water pressure which acted in opposition to the incoming air. To solve this issue, a top fed vertical orientation was chosen. Using this method, air was more naturally drawn into the liquid flow zone due to the downward flow of a high velocity liquid, significantly decreasing the necessary air pressure by a factor of three to four. Following the selection of an optimal sparger orientation necessary for the aeration of a recycled liquid or slurry, a more complex test 35
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A de-aeration tank was applied to the test circuit to increase fluid retention time, increase total fluid capacity, and allow water to de-aerate before recirculation to a feed sump and succeeding variable speed centrifugal pump. In addition, controlled liquid de-aeration in conducted performance evaluations was necessary to properly quantify the air holdup produced by the sparger and to prevent cavitation within the pump head. To determine air holdup, change in liquid elevation within the tank was measured with respect to a fixed measurement port at a known depth of the tank using several elevation rods or measurement tubes. This method of air holdup measurement is illustrated in Figure 20. Using the difference in water elevations determined at transparent measuring ports located just above the sparger outlet inside the tank and below the overflow flume, and the known distance between each port’s centers, the percentage of air holdup within the tank was calculated. To ensure accurate and precise measurements were ascertained, level readings were taken at a collection of time intervals and then averaged. To determine the effect of superficial air velocity and recirculated liquid velocity on air holdup, a multi-facet air manifold and magnetic flow meter were employed, respectively. Figure 20. Holding Cell Air Holdup Measurement Method Compressed air was provided to the experimental system via an air manifold which consisted of a regulator, variable area flow meter, and pressure gauge, as shown in Figure 19 and 37
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Figure 21. Using air pressure and flow rate measurements, the actual air flow rate delivered to the magnetic media bed in standard cubic feet per minute was calculated. Air was supplied to the manifold at approximately 110 psi from a nearby air compressor. In addition to the employment of an air manifold to measure supplied sparger air velocities, a magnetic flow meter was calibrated and utilized to measure water flow rates for each test effort. The maximum water flow produced by the centrifugal pump was approximately 90 gallons per minute. Once steady state air and water flows to the de-aeration tank were obtained, air holdup measurements were taken and recorded using a documented group of sparger operating conditions. Figure 21. Magnetic Sparger Air Holdup Measurement System Before air holdup measurements could be taken, sparging operational parameters were chosen and employed. Operational parameters which were altered during testing included: - Magnetic media type (magnetite, steel shot powder, spherical magnetic media), - Magnetic medium bed depth, - Air fraction (percentage of air in water within sparger), - Cross sectional area of liquid flow region, 38
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- Flow rate of water (gallons per minute), and frother dosage. Due to the substantial quantity of operational parameters, an optimal magnetic media type was chosen using visual observations. During preliminary evaluations it was concluded that dense magnetite and fine steel shot mediums were incapable of providing a uniform air distribution due to significant compaction of particles upon introduction to water, as depicted in Figure 22. As a result, air quickly short circuited to the perimeter of the impenetrable bed when such forms of media were implemented. Coarse magnetite, crushed in two stages to a size fraction of 1000 x 500 micron, promoted air flow and consisted of particles diverse in shape and size, but increased air distribution variability due to a lack of uniform porosity. Additionally, magnetite and steel shot mediums became oxidized, or rusted, within 24 hours of water submersion, further compacting magnetic particles and obstructing air paths. Figure 22. 250 x 150 Micron Wet Magnetite Media Sample To improve air dispersion and maintain a more uniform porous filter medium, a variety of ferritic stainless steel magnetic spheres were employed. A stainless steel coating allows these magnetic spheres to better resist oxidation following extensive subjection to liquid or solids. To perform the testing effort, 1.0 and 1.6 mm magnetic beads, as shown in Figure 23, were utilized. 39
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tailings sump. A variable speed peristaltic pump was used to pump feed material, flotation concentrate, and recycled tailings slurry at a rate of two gallons per minute from the sump to the external porous magnetic sparger. A rate of two gallons per minute permitted the necessary mixing or residence time within the sump and was sustained to maintain a consistent pulp-froth interface level. In addition to this mixture of slurry streams, a high velocity refuse slurry stream, removed from the lowermost zone of the flotation cell by use of variable speed centrifugal pump, was delivered to the recessed sparging unit from above at approximately 14 gallons per minute to simulate a column flotation cell external sparging arrangement. Together, these slurry streams provided the required downward constant traveling fluid velocity to the sparger air interface. The aerated coal slurry was lastly injected at the cell bottom. Due to the scale of this test, a smaller form of the magnetic sparger was fabricated using a hose barb inherent of an inlayed perforated screen and two external ceramic magnets used to retain the magnetic media, as shown in Figure 26. Compressed air was delivered from behind the magnetic bed using a ¾” air-line. Figure 26. Flotation Test Magnetic Sparger Media Housing 42
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Laboratory flotation testing was carried out at an external sparging slurry flow rate of 16.38 gallons per minute. This flow rate was chosen to solicit similar combined air and slurry velocities implemented in previously conducted air holdup evaluations and industrial external sparging applications. To establish a grade and recovery curve for a minus 150 micron coal sample using the magnetic sparger prototype, the provided aeration rate, or air flow rate, was varied from 0 to 2 cubic feet per minute (cfm) using a variable area rotameter affixed to the assembly frame. As air rate was increased, combustible recovery also increased. Air rate was limited to no greater than 2 cubic feet per minute during the test effort to sustain an air fraction, or percentage of air within the aerated recycle stream, of less than 50%. Given a 0.45 in2 cross sectional area of the recirculated tailings and feed line, an air flow rate greater than approximately 2 cfm would have yielded an air fraction in excess of 50 percent and produced excessive burping within the flotation cell. Such burping or air bubble coalescence increases the misplacement of water to the froth launder and decreases bubble particle collision and attachment. To identify the maximum air fraction allowable, gas flow rate was increased until substantial disturbance of the froth was visualized as a result of the coalescence of air or burping. In addition to the variance of aeration rate to control air holdup within the flotation cell, Methylcyclohexanemethanol, or MCHM 8-carbon alcohol frothing agent, was supplied to the feed sump at an addition rate of 10 parts per million (ppm) by volume to decrease the surface tension of the slurry and promote the development of smaller air bubbles. Wash water was not employed in this test program, but an insignificant flow of water was added in the froth launder to provide mobility to the dry froth concentrate to promote drainage and circulation to the feed sump. Minimal water flow was provided to the launder to help maintain the circuit feed percent solids and prevent frother dilution. In an attempt to uphold a constant froth level, a manual gate 43
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valve was located and controlled opposite the high velocity tailings outlet in substitution of a loop controlled pressure transmitter and bladder valve combination. Slurry removed from this valve was deposited in the feed sump below. Following the designation of an aeration rate at a constant tailings recirculation and feed pumping rate, the flotation cell was operated until a steady state process was achieved. Holding a froth level within the cell was proven difficult due to a lack of visibility of the pulp-froth interface given the short height of the cell, turbulence within the cell, and size of the launder, as presented in Figure 27. Once steady state conditions were assumed, samples of the concentrate and tailings were taken for equal time durations using two gallon buckets of documented weights. This process was conducted at five aeration rates to determine the effect of gas flow rate on combustible recovery and concentrate ash content using the magnetic sparger. Additional operating points on the grade and recovery curve were identified without using magnetic material in the sparger air inlet to verify the effect of the employment of a porous medium on flotation performance. Figure 27. Flotation of a Minus 150 Micron Coal using a Magnetic Sparging System 44
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4.0 RESULTS AND DISCUSSION 4.1 Air Holdup Performance Residual gas holdup or aeration performance evaluations were conducted using two MIBC frother concentrations, 12 and 18 ppm by volume. In most industrial flotation applications, the employment of additional reagents, such as collectors and extenders, also alter the surface tension of a liquid or pulp; therefore higher concentrations of MIBC frother were utilized in this test effort in their absence. For each designated frother addition rate and media size, 1.6 mm, 1.0 mm, or 0 mm, the gas holdup within the succeeding de-aeration holding cell was measured as the sparger air rate was increased to determine the effect of aeration rate on air holdup. Air velocity was varied from 3 to 15 ft/s for three recirculated liquid flow rates of 90, 81, and 72 gallons per minute to also define the relationship between recycled liquid velocity and air holdup. A liquid flow rate range of 72 to 90 gpm, or 11.5 to 14.5 ft/s, was chosen to produce similar liquid velocities implemented in industrial external sparging applications. In addition, air velocities were maintained between 3 and 15 ft/s to ensure a sparger air fraction range of 20 to 50%. Liquid and air velocities were calculated using the geometry of the main sparger flow region, 2 in2. The maximum operating air pressure observed throughout all test programs was approximately 6 psi at a combined air and water velocity of 28.6 ft/s. The presence of a magnetic medium negligibly increased air pressure by up to 0.25 at the greatest air velocities. Using air holdup measurements collected at increasing air velocities for each of three liquid velocities, air velocity was plotted versus air holdup for each individual liquid flow rate. Tabulated data and graphs depicting the effect of increases in air and liquid velocities on air holdup during the employment of 1.6 mm magnetic beads, 1.0 mm magnetic beads, and without magnetic media at a frother dosage of 18 ppm are shown in Figures 28, 29, and 30, 46
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respectively. The effect of air velocity on air holdup at increasing liquid velocities when using 12 ppm of frother was also evaluated and is illustrated in Appendices A, B, and C. As evidenced by the air velocity and gas holdup relationships depicted in Figures 28-30, the gas holdup produced by the magnetic sparger increased proportionally to air velocity equally no matter the media type or liquid flow rate. Given a minimal top to bottom ratio of liquid velocities utilized, 1 ΒΌ, the effect of the recycled liquid rate on generated air holdup was difficult to identify. Air Velocity (ft/s) vs. Residual Gas Holdup (%): 1.6 mm Beads -18 PPM 18 16 )% 14 ( p u 12 d lo 10 72 GPM H s a 8 81 GPM G la 6 90 GPM u d 4 is e R 2 0 0 2 4 6 8 10 12 14 16 Air Velocity (ft/s) Figure 28. 1.6 mm Beads: Air Velocity (ft/s) vs. Residual Gas Holdup (%) – 18 ppm Frother Air Velocity (ft/s) vs. Residual Gas Holdup (%): 1.0 mm Beads -18 PPM 20 18 )% 16 ( p u 14 d lo 12 90 GPM H s 10 a 81 GPM G 8 la 72 GPM u 6 d is 4 e R 2 0 0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 Air Velocity (ft/s) Figure 29. 1.0 mm Beads: Air Velocity (ft/s) vs. Residual Gas Holdup (%) – 18 ppm Frother 47
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Air Velocity (ft/s) vs. Residual Gas Holdup (%): No Beads -18 PPM 18 16 )% 14 ( p u 12 d lo H 10 s 72 GPM a G 8 la 81 GPM u 6 d 90 GPM is e 4 R 2 0 0 2 4 6 8 10 12 14 16 Air Velocity (ft/s) Figure 30. No Beads: Air Velocity (ft/s) vs. Residual Gas Holdup (%) – 18 ppm Frother For a given air addition flow rate, gas holdup did not significantly differ as liquid velocity was increased due to the limited range of liquid velocities employed and an increase in bubble rise velocity within the holding cell. As liquid velocity was increased, bubble rise velocity also increased, therefore decreasing the measured gas holdup. If much lower liquid velocities were assessed, it is possible that a difference in the yielded air holdup for a specified aeration rate could be more easily distinguishable. To illustrate the effect of bubble rise velocity on gas holdup, a population balance around the de-aeration tank was formulated to calculate bubble rise velocity as liquid velocity was increased. The derivation for bubble rise velocity is shown in equations 4 through 7 and is as follows: π‘‰π‘œπ‘™π‘’π‘šπ‘’ πΈπ‘›π‘‘π‘’π‘Ÿπ‘–π‘›π‘” π‘‡π‘Žπ‘›π‘˜ = π‘‰π‘œπ‘™π‘’π‘šπ‘’ πΈπ‘ π‘π‘Žπ‘π‘–π‘›π‘” π‘‡π‘Žπ‘›π‘˜ [4] (𝑄 +𝑄 )(πœ€ ) = (𝑄 +𝑄 + 𝑒 𝐴)(πœ€ ) [5] 𝐺 𝐿 𝑖 𝐺 𝐿 𝑏 𝑔 πœ€ = (𝑄𝐺+𝑄𝐿) (πœ€ ) [6] 𝑔 𝑖 (𝑄𝐺+𝑄𝐿+ 𝑒 𝑏𝐴) 𝑒 = (𝑄𝐺+ (πœ€π‘„ 𝑔𝐿 ))(πœ€π‘–) βˆ’(𝑄𝐺+𝑄𝐿) [7] 𝑏 𝐴 48
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where Q is the gas flow rate, Q is the liquid flow rate, πœ€ is the air fraction of the introduced or G L 𝑖 incoming aerated liquid, πœ€ is the air holdup within the holding cell, A is the cross sectional area 𝑔 of the tank, and u is the bubble rise velocity. As shown in equation 6, air holdup is dependent b upon air, liquid, and bubble rise velocities. As air flow rate is increased, air holdup increases, whereas air holdup decreases as liquid and bubble rise velocities increase. This is because retention time of air within a tank or de-aeration cell decreases as the introduced liquid flow rate is increased. Using the derived equation for bubble rise velocity, air rise velocity was calculated for each completed test, as depicted in data summary tables in the attached Appendices. To demonstrate that smaller air bubbles were generated at greater recycled liquid velocities due to an increase in bubble shearing, bubble rise velocities were analyzed for an equivalent introduced air fraction at increasing liquid velocities. Firstly, air fraction was plotted versus air holdup at increasing liquid flow rates, as shown in the Appendix for each testing effort. Although these relationships indicate that air holdup was nearly equal for a given air fraction at increasing liquid flows, bubble rise velocity greatly increased as liquid flow rates increased. For example, at an air fraction of 40%, the air holdup yielded by the magnetic sparger during the employment of a 1.6 mm bead porous medium was nearly 14% at variable liquid velocities. As liquid flow rate was increased from 72 to 90 gpm, bubble rise velocity increased by 1.25 ft/min. In conclusion, lower air bubble rise velocities present at decreased liquid flow rates yielded air holdup values equivalent to those provided at increased liquid flow rates where the average bubble diameter was smaller. At increased liquid velocities, air arose more quickly within the holding cell, but a greater air shear rate at the liquid to air interface generated bubbles much smaller in size. 49
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Although it is difficult to differentiate the aeration performance of the sparger while operated at varying liquid flow rates, the air holdup provided by the magnetic sparger at combined air and liquid velocities employed in industrial external sparging applications is quite distinguishable. A summary of air holdup values produced at increasing combined liquid and gas velocities and frother addition rates for each testing effort is provided in Tables I, II, and III in Appendices A, B, and C. For example, using a 1.6 mm spherical media diameter, the air holdup within the holding cell increased directly proportional to the combined air and water velocity. Using a frother addition rate of 18 ppm, and a combined air and water velocity of approximately 18 feet per second, the air holdup measured within the tank was 12.75 percent. Such an operating point is similar to that employed in an industrial setting. As liquid flow rate was increased using a 1.6 mm magnetic spherical media, the air holdup realized at the burping point also increased to as great as 14.85 percent. Although gas holdup increases as liquid velocities increase, an understanding of pumping economics is necessary to determine an economical operating point of the sparger. In addition to the understanding of sparger performance under varying operating conditions while employing a single porous media type, comparison of performance using differing media yielded a recognizable difference in the sparger generated gas holdup, as represented in Figures 31 through 33. To distinguish the difference in performance of the sparger during the employment of each media type or lack thereof a porous medium, introduced air fraction was plotted versus residual gas holdup for each liquid flow rate utilized. As shown in Figure 31, the use of a 1.6 or 1.0 mm magnetic bead porous medium increased gas holdup by almost two percent at a water rate of 72 gallons per minute. To show the effect of liquid velocity or flow rate on this difference, similar data was plotted for liquid flow rates of 81 and 90 gallons 50
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per minute, as shown in Figures 32 and 33, respectively. As liquid flow rate was increased, the difference in air holdup produced with or without magnetic media was less distinguishable, but still evident. Using 81 gallons per minute of water and a bead size of 1.6 mm, air holdup remained almost two percent greater than without the implementation of magnetic media. In contrast, the difference in air holdup reduced to one percent at combined air and water velocities greater than 25 feet per second as realized when using a liquid flow rate of 90 gallons per minute, as shown in Figure 33. This is most likely due to an increase in the shearing effect at the air and liquid interface. In a comparison of the air holdup performance yielded by each magnetic medium, the 1.6 mm magnetic bead medium continuously produced slightly greater air holdup values than the 1.0 mm bead medium. Because both media types were similar in size, it is difficult to classify the effect of media size on aeration performance. However, preliminary selection of a porous medium did evidence that the use of a uniformly sized porous media is beneficial in the production of a more even air distribution and minimization of short circuited air flows. From optical inspection, the larger media size yielded an improved average air holdup due to an increase in the coalescence of air following its departure from the magnetic bed when using a reduced size of bead. When using a smaller spherical media type, the porosity within the bed remains equal, approximately 26 percent according to a face centered cube lattice, but ejected air streams are located more closely which inherently heightens the risk of coalescence. It is possible that an increase in magnetic bead size could improve air distribution, but bubble size would be expected to increase as well. 51
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Introduced Air Fraction (%) vs. Residual Gas Holdup (%) -90 GPM (18 PPM) 20 18 16 )% 14 ( p u 12 d lo H 10 No Beads s a G 8 1 mm la u 6 1.6 mm d is e 4 R 2 0 20.0 25.0 30.0 35.0 40.0 45.0 50.0 55.0 Introduced Air Fraction (%) Figure 33. Introduced Air Fraction (%) vs. Residual Gas Holdup (%) – 90 GPM (18 PPM) Air holdup evaluations demonstrate that an external porous magnetic sparger using this design concept is a capable and economical sparging device in terms of air dispersion and distribution, and air pressure requirements. According to gathered results, air holdup percentages generated by the magnetic sparger using each media type are quite comparable to those provided by currently employed sparging technologies, but at much lower air pressures. As shown in Figure 34, the air pressure required to operate the sparger during the employment of a 1.6 mm magnetic bead porous medium did not surpass 6 psi at a combined air and water velocity greater than 30 ft/s. At this air pressure, a low horsepower blower can be utilized to supply necessary air flow rates. A similar trend in the relationship between the combined velocity of air and water and air pressure was realized in all testing efforts. Necessary air pressures at increasing combined air and water velocities during the implementation of 1.0 mm magnetic beads and no magnetic beads are further detailed in the Appendices B and C. 53
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1.6 mm Beads -Combined Velocity [Water+Air] (ft/s) vs. Air Pressure (psi) 100 ) is p ( e r u 10 s s e r y = 0.0074x2.1057 P r iA 1 1.000 10.000 100.000 Combined Velocity: Air + Water (ft/s) Figure 34. 1.6 mm Beads: Combined Velocity [Water + Air] (ft/s) vs. Air Pressure (psi) Due to a reliance upon low pressure air, the dimensions of the magnetic bed and the fluid flow region must be properly engineered to minimize required air pressure and promote air distribution. From optical observations of air flow through each tested magnetic medium, the depth and geometrical dimensions of the bed strongly governed the distribution of air at the air inlet. Using a deeper porous bed, air more easily short circuited to a confined location of the bed, thus a minimum bed depth of one inch was utilized. During industrial operation of the sparger, perfect compaction and distribution of material retained at the air inlet will more likely be difficult when a deep bed is maintained. Air pathways increase in size throughout the bed as bead size increases, therefore an increase in bed depth is less detrimental to air distribution. An increase in the width of the bed also increased the short circuiting of air. This was evidenced by the collection of air flow on the low pressure outlet side of the bed at increased fluid pressures. Naturally, air will flow to the path of least resistance where acting pressure is lowest. For the construction of an industrial unit prototype, air inlets should be fabricated with a small cross sectional area of approximately 1.0 square inch or less and a width to depth ratio of 54
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approximately 1.5 to 1.0 to prevent the short circuiting of air. Using multiple air inlets in series as described across the flow region would increase the complete air distribution from the bed and ensure proper aeration of a moving slurry. To prevent the short circuiting of air to the perimeter of the bed, the surfaces of surrounding air inlet walls should be textured roughened to establish similar friction present between individual magnetic beads. The height and hydraulic diameter of the fluid flow region should also be minimized to increase the mixing of air and slurry and to limit the water pressure internal to the sparger to decrease air pressure requirements, respectively. 4.2 Flotation Performance In addition to the completion of air holdup and aeration performance evaluations, flotation scoping tests were conducted to demonstrate the sparger’s ability to yield high mineral recoveries of a finely sized coal sample. Testing was conducted with and without the use of a magnetic porous medium to characterize the benefit of using such material. Steady-state flotation tests were performed at a fixed feed rate as aeration rate was increased from approximately 0.5 to 2.0 scfm to define the relationship between sparger air fraction and mineral recovery. A fixed slurry feed rate of 16.38 gpm, or approximately 12 ft/s, was sustained to reproduce recirculated liquid rates utilized in air holdup evaluations. Once steady-state conditions were established for a given air velocity, samples of the froth concentrate and tailings were procured. An ash analysis was then conducted on each sample to determine their respective ash contents. Ash content values were then employed to calculate the combustible recovery realized for each assumed air flow rate and pressure. The combustible recoveries and concentrate ash contents achieved at variable air addition rates, with and without the employment of a porous magnetic medium, are displayed in Tables I 55
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and II, respectively. Using the mass yield to the concentrate and ash contents of both the tailings and concentrate fractions, a feed ash content was also back calculated for each test. As evidenced by the flotation test data, combustible recovery improved by up to 20% as aeration rate was increased to an air fraction of nearly 50% by volume. As expected, an increase in air flow rate also increased the average concentrate ash content due to an increase in the hydraulic entrainment of high ash slimes or fines. Given the small volume of the employed flotation cell and limited particle residence time, combustible recoveries yielded during the employment of a porous medium can be considered favorable. Table I – Sparger Flotation Results Without use of Magnetic Beads No Beads - Sparger Flotation Results True Slurry Air Pressure Feed Ash Tail Ash Con Ash Combustible Air Flow Fraction (psi) (%) (%) (%) Recovery (%) (scfm) (gpm) (%) 0.51 0.75 16.38 18.97 15.86 21.41 5.66 39.54 1.03 1.00 16.38 32.06 20.02 24.65 9.13 33.92 1.30 1.25 16.38 37.28 18.52 25.77 8.98 48.22 1.57 1.50 16.38 41.83 16.93 25.30 8.04 53.66 2.13 2.00 16.38 49.32 16.71 27.74 9.64 66.12 Table II – Sparger Flotation Results with use of Magnetic Beads 1 mm Beads - Sparger Testing Slurry Air Air Pressure True Air Flow Fraction (scfm) (psi) (scfm) (gpm) (%) Feed Ash Tail Ash Con Ash 0.50 0.75 0.51 16.38 18.97 12.32 21.44 7.62 1.00 1.00 1.03 16.38 32.06 16.38 25.24 9.32 1.50 1.50 1.57 16.38 41.83 16.11 26.29 13.60 2.00 2.00 2.13 16.38 49.32 17.21 34.98 11.86 In addition to the effect of increased aeration rate on recovery, the employment of a 1.0 mm magnetic bead porous medium also greatly improved combustible recovery. Using equivalent air flow rates in both test programs, the utilization of a porous magnetic bed increased combustible recovery by 15 to 25%, as illustrated by the air rate versus combustible recovery 56
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plot illustrated in Figure 35. For example, at an air addition rate of 2.13 scfm, the use of a porous medium increased combustible recovery by 15%. Such an increase in recovery resulted from the production of a finer air bubble distribution, which improved the likelihood of collision and attachment between air bubbles and fine particles. Due to an increase in combustible recovery using a porous medium, yielded concentrates were of a much higher ash content. If a taller column cell had been utilized to increase particle retention time, while also boasting the use of a deep froth and wash water, a more satisfactory concentrate grade and combustible recovery could have been achieved. Air Flow (scfm) vs. Combustible Recovery (%) with and without a Porous Medium 90.00 80.00 )% 70.00 ( y r e 60.00 v o c 50.00 e R e 40.00 No Beads lb it s 30.00 1.0 mm Beads u b 20.00 m o C 10.00 0.00 0.00 0.50 1.00 1.50 2.00 2.50 Air (scfm) Figure 35. Air Flow (scfm) vs. Combustible Recovery (%) with and without a Porous Medium Although an improvement in flotation performance was observed during the employment of a porous medium, inconsistencies in calculated combustible recoveries and measured ash contents are apparent. Most importantly, the calculated feed ash did not remain continuous throughout all test work. This was most likely due to inefficient steady state sampling resulting from difficulties experienced in upholding the froth level within the flotation cell by use of a gate 57
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valve at lower aeration rates. Although material was frequently removed from the system, a proper test should sustain a more fixed feed ash content. Due to the size of the sparging prototype, the maximum allowable air addition rate also hindered the development of a more stable froth at lower sparger air fractions. In column flotation applications, approximately 4 scfm of air per square foot is required to aerate the cell. In this study, a maximum of 2.13 scfm was allowable before burping commenced. To appropriately aerate the flotation cell utilized, a one inch recirculation pipe should have been exercised. Such an increase in sparger size would have increased the permissible air addition rate at both low and high air fractions. Although experimental faults were realized, this study demonstrates the value of a porous medium for its ability to increase recovery as a result of an increase in air holdup. To more fully understand the sparging capabilities of the magnetic porous sparger, a laboratory column cell, incorporating wash water and a loop controlled pressure transmitter to maintain a froth level, must be employed. 58
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5.0 CONCLUSIONS The engineered and performance evaluated low pressure porous sparger demonstrated itself as a viable sparging prototype in terms of bubble generation and distribution, and flotation performance. The air holdup provided by the sparger, ranging from 12 to 16 percent, was similar to that generated by current industrially employed external spargers, such as the static mixer, at comparable combined air and liquid velocities. Due to the presence of a negligible pressure drop at the air-to-liquid interface, the magnetic porous sparger was also capable of yielding such air holdup values at much lower air pressures of 5 to 7 psi. As a result of low operating air pressures, this sparger is operable by means of a low horsepower blower, reducing operational costs significantly. Following the completion of numerous sparging assessments, practical sparger operating parameters, such as a proper porous medium, correct sizing of the chosen media, necessary combined velocities of air and water, orientation of the sparger, and required air pressure were determined. Because air travels to the path of least resistance, a round magnetic media with a bulk uniform porosity is necessary to avoid the short circuiting of air streams to the perimeter of the porous medium or confined locations of the magnetic bed. To provide complete dispersion of air through the magnetic medium, air inlets with a diameter of 1.5 inches or less, and a bed width to depth ratio of 1.5 to 1.0 are also recommended. Subsequently, a top-fed, vertical orientation of the sparger was deemed optimal to more naturally draw air into the sparger at lower air pressures. In addition to the identification of ideal sparger operational parameters, conducted aeration evaluations also confirmed the improvement of the aeration of a recycled liquid or slurry by use of a porous magnetic medium. During the employment of a porous magnetic medium in both air holdup and flotation performance test efforts, an increase in air holdup of up to 2 to 3% 59
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DESIG(cid:6) A(cid:6)D TESTI(cid:6)G OF A HYPERBARIC HORIZO(cid:6)TAL BELT FILTER FOR FI(cid:6)E COAL DEWATERI(cid:6)G by Jeffery Salomon Committee Chairman: Gerald H. Luttrell Department of Mining and Minerals Engineering ABSTRACT This objective of this project was to develop a new dewatering device that could produce a lower moisture content and better fine particle recovery than current technology. To meet this goal, a hyperbaric horizontal belt filter was designed and constructed over the course of 18 months. Once built, the filter was then thoroughly tested to determine operational capabilities. The test data showed that the lowest moisture content that could be achieved with a coarse feed (minus 1 mm screen-bowl centrifuge feed) was 8.8%. This value could be further reduced to 8.2% and capacity increased with the use of dewatering aids. When testing with a fine feed (minus 0.15 mm column product feed), the lowest moisture content was 35% without chemicals and 29% with chemicals. A 50/50 mixture by volume of coarse and fine feeds was artificially created and provided a moisture of 10.8%, which was reduced using reagents to 8.4%. The machine provided a very high recovery rate for all feed materials. Of the coal input, no less than 94% of it reported to the dry product. The pressure used to dewater the coal was the controlling factor for the air consumption of the unit. The data from these tests suggest that a full size production unit is feasible, although the power requirements for gas compression would be high. ii