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ACKNOWLEDGMENTS The author would like to express his sincere appreciation to his advisor, Dr. Roe-Hoan Yoon, for the guidance, inspiration, suggestions and criticisms. Special thanks are also given to his committee members, Dr. Luttrell, Dr. Adel, and Dr. Ismail for their continued interests, useful suggestions, constructive comments and discussion to understand the overall process. The financial support from the National Energy Technology Laboratory and Department of Mining and Minerals Engineering is deeply appreciated. I owe special gratitude to Mr. David Brightbill, Steve Blubaugh and Steven Abbatello for their helpful suggestions and continuous support. I am also grateful to Dr. Jinming Zhang, Mr. Serhat Keles, for their friendship and support. I would like to express my most sincere appreciation to my parents Ziynet and Ali Eraydin for their inspiration, encouragements, moral support and continued suggestions. I would also like to thank my sister Feyza for her continued support. Finally, I would like to express my thanks to Emily A. Sarver for all her encouragements, patience and dedication. iv
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Figure 4.3 Engineering flowsheet for the POC-scale pond reclaim facility……..……… 160 Figure 4.4 Simplified process flow diagram for the pond reclaim facility……………… 163 Figure 4.5 Nearly completed plant incorporating the POC circuitry……………...…….. 164 Figure 4.6 Classifying cyclones used to provide a 100 mesh cutsize…………………… 164 Figure 4.7 Screen-bowl centrifuge used to dewater 100x235 mesh product……..…….. 164 Figure 4.8 Deslime cyclones used to perform a nominal 325 mesh cutsize…………….. 164 Figure 4.9 Three-stage conditions used for conditioning the dewatering aid…………… 165 Figure 4.10 Bank of disc filters used to dewater the fine coal froth product…………….. 165 Figure 4.11 Static thickener used to thicken solids and clarify process water…………… 166 Figure 4.12 Paste thickener used to further thicken wastes for disposal…………………. 166 Figure 4.13 Weight and ash distributions for samples collected from the shakedown tests conducted on the coarse coal treatment circuits………….…………….. 168 Figure 4.14 Weight and ash distributions for samples collected from the shakedown tests conducted on the fine coal treatment circuits……………..……………. 169 Figure 4.15 Moisture content versus dewatering aid dosage (RV)………..…….……….. 174 Figure 4.16 Moisture reduction versus dewatering aid dosage (RV)………..…………… 174 Figure 4.17 Effect of dewatering aid addition on vacuum filter pump power demand…... 175 Figure 5.1 Tergitol NP-7………………………………………………………………… 195 Figure 5.2 PPG-400……………………………………………………………………... 210 xi
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Table 2.14 Coal Clean coal (minus 325 mesh) dewatered using RW, RU, and RA dispersed in Nalco 01DW110………………………………………………. 84 Table 2.15. Coal Clean coal (50% minus 325 mesh and 50% 100x325 mesh) dewatered using RW and RU dispersed in Nalco O1DW110…………………….…….. 85 Table 2.16 Coal Clean coal (75% minus 325 mesh and 25% 100x325 mesh) dewatered using RW, RU and RA dispersed in Nalco 01DW110……………...………. 86 Table 2.17 Effect of disc speed on product rate and moisture content for Coal Clean coal (minus 325 mesh) from the filter module……………………………… 86 Table 2.18 Effect of Reagent 01DW133 on Coal Clean coal (50% minus 325 mesh and 50% 100x325 mesh) from the centrifuge module…………………….…….. 87 Table 2.19 Effect of reagent addition on Concord flotation feed (100 mesh x 0) using RV and RW3…………………………………………………………..…….. 92 Table 2.20 Pilot-scale test results obtained on the Concord flotation feed sample (100 mesh x 0) using various vacuum pressures…………………………..……… 93 Table 2.21 Pilot-scale test results obtained on the Concord flotation feed sample (100 mesh x 0) using various reagent combinations………………………...……. 94 Table 2.22 Pilot-scale test results obtained on the Concord flotation feed sample (100 mesh x 0) using various reagent combinations...…...………..……….......... 95 Table 2.23 Pilot-scale test results obtained on the Concord flotation feed sample (100 mesh x 0) using various reagent combinations……………………………… 95 Table 2.24 Screen analysis of the Buchanan flotation product used for dewatering tests 98 Table 2.25 Screen analysis of the Buchanan filter feed used for dewatering tests…....... 98 Table 2.26. Effect of reagent addition on dewatering of Buchanan’s filter feed………… 99 xiii
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Table 2.27. Effect of reagent addition on dewatering Buchanan’s flotation product……. 99 Table 2.28. Effect of mixing intensity on dewatering of Buchanan’s flotation product… 101 Table 2.29 Effect of pilot-scale filter disc speed on filter cake production rates and moisture content………………………………………....……….………….. 102 Table 2.30. Effect of reagent addition on the pilot-scale dewatering of Buchanan’s flotation product …………………………………………………………...... 102 Table 2.31. Effect of pilot-scale filter vacuum level on filter cake moisture contents….... 104 Table 2.32. Effect of pilot-scale filter vacuum level on filter cake moisture contents (4 lb/t RW)…………………...………………………………………...……….. 104 Table 2.33. Effect of pilot-scale filter vacuum level on filter cake moisture contents (4 lb/t RU)…………….………………………………………………………… 104 Table 2.34 Effect of reagent addition on dewatering of Elkview’s filter feed sample (standard metallurgical coal)………………………………………………… 107 Table 2.35. Effect of using RW, RU and RV on the dewatering of Elkview’s filter feed (STD Met Coal)……………………………………………….........………… 108 Table 2.36 Effect of using RW, RU and RV for Elkview’s filter feed (Mid-Vol Met Coal)…………………………………..………………….…………………. 109 Table 2.37. Effect of using RW, RU and RV on Elkview’s filter feed sample (Mid-Vol Met Coal)…………………………….………………………………………. 109 Table 2.38 Effect of RW addition on the Pinnacle pond sample…………….………….. 119 Table 2.39 Effect of reagent addition on dewatering of Pinnacle thickener underflow sample…………………………………………………………..…………… 120 Table 2.40 Effect of desliming on dewatering of Pinnacle thickener underflow sample. 121 xiv
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Table 2.41 Effect of reagent addition on dewatering of Pinnacle thickener feed sample. 121 Table 2.42 Effect of RW addition on the pilot scale dewatering of the Pinnacle-Smith Branch Impoundment sample using the mobile units……………………….. 122 Table 2.43 Effect of RW addition on the pilot scale dewatering of the Pinnacle thickener feed sample using the mobile test units……………..…………….. 123 Table 2.44 Effect of reagent addition on dewatering of Pinnacle thickener feed sample. 123 Table 2.45 Effect of reagent addition on the dewatering of the froth products obtained using 400 g/t diesel as collector………………………………………..……. 128 Table 2.46 Effect of conditioning time on the dewatering of flotation product using 2 lb/t RV……………………………………………………………………... 129 Table 2.47 Effect of cake thickness on cake moisture in the presence of 3 lb/t RV…….. 129 Table 3.1 Effect of reagent type and dosage on dewatering of mixture sample……….. 139 Table 3.2 Effect of filtration time on dewatering of mixture sample (0.5 in. cake)…... 140 Table 3.3 Effect of vacuum pressure on dewatering of mixture sample (0.5 in cake)… 141 Table 3.4 Effect of cake weight and thickness on dewatering of mixture sample….….. 142 Table 3.5 Sample data collection sheet………………………………………………… 143 Table 3.6 Simulation results on Mingo Logan’s mixture sample………………...……. 150 Table 3.7 Simulation results on Mingo Logan’s flotation sample product……....……. 151 Table 4.1 Effect of RV and RW (dissolved in diesel at 1:2 ratio) at various dosages………………………………………………………………………. 172 Table 4.2 Effect of RV and RW (dissolved in diesel at 1:2 ratio) at various dosages on dewatering of floated sample……………………………………………. 173 xv
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Table 4.3. Effect of RV (dissolved in diesel at 1:2 ratio) at various dosages on dewatering of deslimed samples…………………………..………………… 173 Table 5.1 Effect of amine (DAC) addition as the first step on dewatering of Georgia clay……………………………………………………………..……………. 184 Table 5.2 Effect of RW addition as the second step (10 lb/t DAC & various dosages of RW) on dewatering of Georgia clay………………………….………..… 185 Table 5.3 Effect of using 10 lbs/t amine and RW on the dewatering of PSD Filter Vat kaolin clay sample after dilution to 15% solids at pH 7.0..…..................… 187 Table 5.4 Effect of using 10 lbs/t amine and RW on the dewatering of PSD Filter Vat kaolin clay sample after dilution to 15% solids at pH 7.0…….................... 188 Table 5.5 Effect of using amine only on the dewatering of PSD Filter pre-leached kaolin clay sample (pH 9.5& 30% solids)………..…………………….…… 189 Table 5.6 Effect of using amine only on the dewatering of the coarse pre-leach kaolin clay sample from (pH 7 & 30% solids)………………...………………..….. 189 Table 5.7 Effect of using amine (10lb/t) and RW on the dewatering of PSD Filter pre- leached kaolin clay sample at 30% solids at pH 9.5 and pH 7.0…………... 190 Table 5.8 Effect of foam on dewatering of Georgia clay at pH 7.0 when Tergitol NP-7 and NP-9 is used as foam generating agents……………………....………… 194 Table 5.9 Effect of Tergitol with thick cake (5-6mm) on dewatering of Georgia clay... 194 Table 5.10 Effect of foam on dewatering of Georgia clay at pH 3 when Tergitol NP-7 is used as foam generating agent……………………………………..……… 197 Table 5.11 Effect of alum addition on dewatering of Georgia clay when Tergitol was used as foaming agent…………………………………………….…………. 197 xvi
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Table 5.12 Effect of reagent addition at (1:2) ratio on dewatering of Kentucky coal sample at 17-19 inches Hg vacuum…………………………………..……… 202 Table 5.13 Effect of amine addition at (1:2) ratio on dewatering of Kentucky coal sample at 17-19 inches Hg vacuum…………………………………..……… 203 Table 5.14 Effect of amine (10 lb/t) and RW addition at (1:2) ratio on dewatering of Kentucky coal sample at 17-19 inHg vacuum………………….……..…….. 204 Table 5.15 Effect of amine addition as the first step on dewatering of fly ash sample at 20 in Hg Vacuum pressure……………………………….…....…………….. 205 Table 5.16 Effect RW, RU and RV addition at (1:2) ratio on dewatering of amine pre- treated (3 lb/t of amine) Kentucky fly ash sample at 20 in Hg vacuum......... 205 Table 5.17 Effect of amine addition as the first step on dewatering of fly ash sample at 30psi pressure………………………………………………………………… 206 Table 5.18 Effect of amine (3 lb/t) and RW addition at (1:2) ratio on dewatering of Kentucky coal sample at 30psi pressure……………………………..……… 206 Table 5.19 Effect of amine (1lb/t) and RV addition as the first step on dewatering of fly ash sample at 20 in Hg vacuum pressure………………….……….………... 207 Table 5.20 Effect of using amine (1lb/t) and RV on the dewatering of the fly ash sample at 30% solids………..………………………………………………. 208 Table 5.21 Effect of PPG addition on dewatering of Kentucky fly ash sample at 17-19 in Hg vacuum…………………………….………………………………….. 209 Table 5.22 Effect of Tergitol addition on dewatering of Kentucky coal sample at 17-19 in Hg vacuum………...…………………………...…………………………. 210 xvii
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CHAPTER 1 INTRODUCTION 1.1. INTRODUCTION Fossil fuels, especially coal, oil and gas, are of great importance since they can be burned to produce energy. The Energy Information Administration estimates that in 2005, fossil fuels made up approximately 86% of United States’ energy production and 76% of world consumption. The remaining sources are non-fossil sources such as hydroelectric, nuclear and other (geothermal, solar, wind, wood and waste) at 6.3%, 6.0% and 0.9 % used for energy production, respectively.[1, 2] Fossil fuels are the most important energy sources; however, they are non-renewable. According to Oil & Gas Journal estimates, years of production left in the ground for fossil reserves are 45 years for oil, 72 years for gas and 252 years for coal. Of these fossil fuels coal has the most widely distributed reserves and it is mined in over 100 countries and on all continents except Antarctica. The total recoverable world reserve for coal was estimated by International Energy Annual-2005 to be around 908 million tons. British Petroleum’s statistical review of world energy data from 2007 shows that the United States has enormous coal resources and recoverable reserves. Coal is classified into six types or ranks (peat, lignite, sub- bituminous, bituminous, anthracite and graphite) which depend on the amount and the types of carbon it contains and on the amount of heat energy it can produce. In the United States, the most widely used coal types are lignite, sub-bituminous, bituminous and anthracite. Table 1.1 shows the proved recoverable coal reserves in millions of tons for the United States and the top 10 countries as of the end of 2006.[1-4] 1
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In United States, coal represents approximately 95 percent of the nation’s fossil energy reserves. Coal is mainly found in three large regions: the Appalachian Coal Region, the Interior Coal Region, and the Western Coal Region (includes the Powder River Basin). It is currently produced in 26 states, with most of it mined in Wyoming, followed by West Virginia, Kentucky, Pennsylvania, and Texas. The Energy Information Administration reports that 1,162.8 million short tons of coal were produced in 2006. Currently, approximately 50% of the electricity is produced by using coal and there are approximately 600 power plants. Coal is also one of the nation’s lowest-cost electric power sources (DOE). Thus, today the electric power sector drives the coal demand for electricity production and is almost responsible for 90% of the coal consumption (EIA). Figure 1.1 shows the comparison of electricity produced from the major energy sources in United States.[1-3] 1.2 1 0.8 0.6 0.4 0.2 0 1940 1950 1960 1970 1980 1990 2000 2010 Figure 1.2 Coal consumption by sector (Energy Information Administration) 3 snoT trohS noilliB Electric Power Industrial Residential, Commercial and Transportation Year
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The increase in demand resulted in tremendous expansions on coal mining and capacity. After the 1970s this demand created more mines, especially above-ground. The National Mining Association reports that, of the two main mining methods, surface and underground, approximately two-thirds of today’s coal production is surface mining. The increase in the need of coal also improved mining technologies to produce additional coal. This additional coal is prepared to today’s standard specifications dictated by the users. Thus, coal processing technologies is advanced to produce a cleaner and higher heating content end product.[5] 1.2. LITERATURE REVIEW 1.2.1. Coal Processing Coal preparation includes four major methods, including blending and homogenization, size reduction, grading and handling, and most importantly beneficiation or cleaning for high quality product. Regardless of the intended utilization purposes, there are levels of cleaning to which coal can be economically subjected.[6-10] Coal preparation is a very important practice for processing industries, and market demand determines the selection of preparation methods. Therefore, as shown in Figure 1.4, there are different methods of economically cleaning coal.[6-11] In coal processing, it is typical to employ an operation by starting with the crushing and screening of run-of-mine (ROM) coal into coarse, fine, and occasionally intermediate sizes. Being exclusive of fine sizes, the coarse and intermediate size fractions are then upgraded by gravity concentration e.g. dense-medium baths, jigs, dense-medium cyclones, etc. Because the differences in densities between pure coal particles and liberated mineral impurities are sufficient to achieve an ideal cleaning process, these methods are dominantly used. The fine and ultra-fine 5
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pass through a medium. Solids are retained on the surface of the medium, creating a cake formation, which the liquid media flows through. Sedimentation is a separation method that benefits from the differences in phase densities of solids and liquids by allowing solids to sink in the fluid under controlled conditions.[20, 22-29] In the conventional dewatering processes, thickeners, dewatering screens, vacuum filters (drum, disc, and belt), centrifuges, pressure (hyperbaric) filters are utilized to remove the surface water. Vacuum filtration is one of the dewatering processes widely used in the coal industry, its advantage being a continuous operation that can be utilized under relatively simple mechanical conditions. The removal of free water from the surface of fine particles is difficult and unsatisfactory by mechanical methods. The problems associated with the dewatering of fine particles are complicated. The finer particles have a larger total surface area than the coarse particles, causing very high water retention and smaller capillaries in the filter cake. Eventually, this results in high capillary pressures and slower dewatering rates.[19, 20, 23-26] In general, the costs of cleaning fine particles are approximately 3 times higher than those for coarse particle. This leaves coal producers only a few options as to what to do with the fines in economical terms. The fine products also contain higher levels of impurities, ash and sulfur, that lead to environmental concerns. Therefore, fine particles smaller than 500µm, and ultra-fine particles smaller than 100µm, are abandoned with the discard streams if they constitute only a small fraction (5% to 10%) of the product stream. This has been the case for many U.S. coal producers. As a result, 30 to 40 million tons of fines have been discarded to waste ponds annually, representing a loss of recognized, exploitable natural resources.[8, 17, 18, 21, 31, 36] The key reason for not completely exploiting this energy resource is the cost of the cleaning process as well as dewatering the high levels of moisture associated with the fine 7
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fraction of coal. The dewatering of fines results in a significant expense reporting to overall cleaning expenses because dewatering costs increase severely when the particle size is smaller than 500µm. The cost also includes thermal drying, which is the only practical method of drying fine coal to further decrease the moisture content. An acceptable level of moisture reduction is usually below 10% (by weight). Even though preferred moisture levels can be achieved by thermal drying, it is a capital-intensive and costly technology compared to mechanical dewatering methods.[31, 33, 40, 44-46] There have not been any significant technical innovations in fine particle dewatering in decades because most of the fine fraction was sent to waste ponds. This lack of technological knowledge generated approximately two billion tons of fine coal in waste ponds to date, and 500 to 800 million tons of the fines are still in active ponds. On the other hand, in recent times, the industrial demand for coal has increased, and recovery of this size fraction has become more important. Recent advances in the recovery of fine and ultra-fine particles by flotation have also lead to more fine size coal production, creating an incompatibility between efficient, cleaner coal production and insufficient, fine-particle dewatering techniques.[9, 23, 31, 46, 47] The need for understanding and enhancing fine-coal dewatering will be a considerable contribution to the performance of studies to meet the industry’s needs. Studies on fine-coal dewatering will increase the availability of efficient dewatering processes that can provide lower filter cake moisture, resulting in reduced thermal drying costs, reduced transportation cost, improved product quality, increased calorific value, and minimized freezing during winter storage.[31, 36, 48] This study was carried out to achieve a better understanding to solve the problems associated with fine particle dewatering. For this reason, two new dewatering technologies, 8
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which have been developed at Virginia Polytechnic Institute and State University, were tested. The first technology utilizes novel dewatering aids that have revealed promising options to receive significantly lower moisture. The other technology is the utilization of foam-supported dewatering, which is superior when compared to the current, commonly-used technologies. 1.2.2. Coal Dewatering Because flotation is accomplished in an aqueous solution to produce clean coal, the product contains approximately 80% water. Although, coal fine products may represent only 20% of the weight of a preparation plant feed, this fraction is accountable for almost two-thirds of the final product moisture. From a utility viewpoint, a one-ton decrease in moisture can offset four tons of steam coal. This steam coal can be added to clean coal product, strongly indicating that the success of coal utilization is critically dependent on solid/liquid separation technology.[23, 49, 50] As the first step in dewatering, large settling tanks can be used to remove the free water, where the slurry is thickened from 35% to 75% solid content. The second step involves subjecting the pulp to filtration methods including vacuum, drum, disc, and belt filters, centrifuges, and pressure (hyperbaric) filters to remove the remaining surface water. Despite all of this, the fine coal, filtered by using these mechanical methods, may still include undesirable amounts of water in their compositions. Thermal drying, the only fully-developed method to lower the moisture to single digits, can further decrease cake moisture contents to attain desired levels; however, the associated high energy intensives, operation costs, and special installation permissions limit the employment of thermal driers.[20, 26, 51-53] 9
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Thermal drying is the last operation conducted on dewatered solids when these two mechanical solid-liquid separation methods are not sufficient.[22, 24, 54] At processing plants, dewatering is practiced normally in a combination of the above methods. First, the bulk of the water is removed by sedimentation methods, followed by filtration methods. If needed, thermal driers are used to produce the desired final moisture content. Several common factors influence all solid-liquid separation steps and equipment selection, such as solid concentration, particle shape, specific gravity, surface characteristics, liquid viscosity, and, most importantly, particle size and size distribution. Figure 1.6 describes 100 80 Static Thickeners 60 Cyclones, Sieve Bend, Vor-Sieve 40 . Vac Drum Filter 30 Vacuum Filter Disc Type High Speed Vibrators 20 10 Solid Bowl/Screen Bowl Centrifuge High Speed Vibrators 5 Positive Discharge Type Basket Centrifuge Vibrating Basket Centrifuge Thermal Drying Ranges 2 Vibrating Screens 325M 200M 100M 48M 28M 20M 10M 6M 4M Mesh 0.001 0.005 0.01 0.05 0.1 0.50 1.0 2.0 5.0 Inches Figure 1.6 Commonly used dewatering equipment in coal industry for various size ranges and corresponding approximate moistures 11
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the tools that are generally employed for different size fractions of coal to be dewatered.[8, 9, 20, 26, 51-53] In general, sizes larger than 1.5 inches do not exhibit any particular/serious dewatering problems since very basic types of shaker screens can produce products with low moistures. For intermediate to 0.02inch particle size dewatering, high-speed vibrators may be used. Usually, for dewatering of 3/8 to ¼inch size particles, centrifuges of various types and designs are used, where the centrifugal force can be employed to promote/aid dewatering. For sizes smaller than 0.02 inch, solid bowl and screen bowl centrifuges can be used, even though higher moisture values may result than what is desired. Vacuum filtration becomes increasingly important with finer sizes (-30 mesh) for further dewatering.[8-10, 15, 41, 55, 56] a) Sedimentation Techniques Sedimentation is a collective term describing the gravity separation of the fine solids, usually under quiescent conditions, resulting in the formation of a sedimentary layer of solids and a relatively clear supernatant liquid. It is mainly used at the very early stages of the dewatering process to increase the solid content of the slurry in large capacity thickeners. Depending on the particle size and the solid percent, sedimentation processes involve the settling of solids in slurry by either employing gravitational or centrifugal force. Because the settling velocity of the very fine particles is extremely slow by gravity alone, the centrifugal force will have greater affect on settling time and velocity. Alternatively, the particles may be agglomerated into larger lumps to facilitate the dewatering. The settled solids are then collected, removed, and introduced to filtration to further reduce the moisture content of the cake before thermal drying.[20, 26, 41, 44, 52] 12
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b) Centrifugation Techniques Centrifugal Separation can be considered an extension of gravity separation because the equipment creates high gravity forces to increase the settling rate of particles for the purpose of solid-liquid separation. Compared to thickeners, centrifugal separation does not require a density difference between the solid and the liquid. Even though high maintenance costs exist, centrifugal dewatering is commonly the most effective mechanical method as a result of these high forces’ ability to dewater the particles in a short time and a continuous manner. Centrifugation is primarily utilized for mineral and coal processing industries because it can collectively dewater a wide range of sizes (normally with a 37.5mm upper limit, where fine is 0.5mm x 0).[8, 9, 29, 41, 61] Centrifugal separation can be executed by using cyclones or centrifuges. Cyclones are very simple and cheap, but they suffer from limitations such as low efficiency when dealing with fine particles and their inability to use flocculants due to high shear forces. Therefore, cyclones are considered more like classifiers than thickening tools. Centrifuges are generally classified into two groups. a) perforate-basket type - without transporting device - with positive discharge system - vibrating basket b) bowl type - co-current solid bowl - countercurrent solid bowl - screen bowl 13
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In coarse coal dewatering, perforated basket centrifuges are most commonly used, and bowl type centrifuges are most generally used for fine particles. Bowl type centrifuges are commonly used to dewater coal at sizes from approximately 10mm to 1.0 mm. Two types of bowl centrifuges may be used, solid bowl centrifuges and screen bowl centrifuges.[8, 9, 29] c) Filtration Techniques Filtration is a widely utilized dewatering application in mineral processing industries and generally occurs after thickening. In filtration, there are four types of driving forces employed to obtain flow through the filtering medium: gravity, vacuum, pressure, and centrifugal forces. There are basically two types of filtration used in practice, surface filters, in which the solids are deposited in the form of cake on the upstream side of the relatively thin filter medium, and depth filters, in which particle deposition takes place inside the medium. In coal-preparation applications, most filters are surface filters, employing vacuum and pressure forms of driving force.[26, 29, 51, 52, 62, 63] Vacuum filtration can be categorized into two groups: batch and continuous. In coal dewatering, where continuous filters are widely employed, batch vacuum filters are not practical. There are several types of vacuum filters that are used for fine particle dewatering. Three types of vacuum filters are rotary drum, rotary disc, and horizontal belt (HBF), or disc, filter.[26, 44, 52] Rotary vacuum drum filters are the most widely used continuous filters for fine coal and mineral particles. They utilize a drum partially submerged into a tank of agitated slurry. Once the vacuum is applied, cake is deposited on the drum surface and discarded by various types of mechanisms, such as fixed knife and air blowing. Effluent is drained by different methods, depending on the manufacturer’s design. Adjustable operating parameters, such as drum rotation 14
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speed (rpm), applied vacuum pressure, and submergence, dictate the performance of the drum filter. Changes in these conditions affect the cake formation, drying, throughput, and the degree of dewatering achieved.[26, 44, 52, 64] The key advantages of drum filters are i) effective washing and dewatering properties, ii) low labor and operating costs, iii) wide operation variations, and iv) easy maintenance and clean operation. The main disadvantages are i) high capital cost, ii) large space requirements, iii) incompatible for fast-settling slurries, and low efficiency with ultra-fine particles that blind the filter cloth.[26, 44, 52, 64] Rotary vacuum disc filters have almost the same fundamental design as the drum filters. Disc filters consist of a number of flat filter elements, mounted on a central shaft and connected to a normal rotary vacuum filter valve. As the unit rotates, the discs are submerged in slurry contained in a slurry tank and agitated. Gradually, cake is formed and dewatered as the unit rotates out of submergence. The filter cake is usually removed by a combination of scraper blades and a blowback mechanism. The disc filters have a low capital cost per unit area, and they supply large filter areas in smaller floor areas; however, blowback systems may cause higher moisture, and cake washing cannot be done efficiently.[26, 44, 52, 64] Horizontal belt filters are continuous filters and consist of an endless reinforced perforated rubber belt with drainage channels, where the vacuum is applied. The filter medium/cloth sits on the rubber belt and moves along with it. The suspended slurry is fed from one end of the filter to produce cake, and filtrate is collected in a tank to be pumped out as effluent. The horizontal belt filters occupy large floor areas, and the installation costs per filter area are high; however, being fully automatic, flexible, and having relatively high speeds of operation offset these weak points.[22, 24, 29] 15
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The pressure filters normally perform in a batch-wise manner under positive (air or hydraulic) pressures to remove water and retain solids in the form of a cake. Pressure filters are utilized very often in process industries that deal with fine, slow-settling particles exhibiting low filterability and suspensions that contain higher solid contents. Pressure filters have advantages over vacuum filters due to higher pressures and vertical incompressibility of solids. In these units, high pressure creates an increased dewatering rate and lower filter cake moisture. On the other hand, the discharge of the cake in a continuous manner from the inside of the unit is difficult and therefore pressure filters are usually employed as batch units. The high capital costs and inefficient returns associated with batch units create an additional economic disadvantage. Batch, chamber filter presses and continuous, belt filter presses are two distinct types of pressure filters most frequently utilized in coal dewatering.[25, 26, 52, 65] d) Thermal Drying Thermal drying of minerals and coal is the last and the most expensive unit operation performed on the dewatered materials before transportation. For that reason, the surface area of particles increases proportionally with the fineness of size and the final cake moisture. The coal’s ultimate dewatering cost is strongly related to the amount of the fines. Thermal dryers are utilized to generate low moisture, maintain high coal-pulverized capacity in power plant applications, reduce heat loss, prevent freezing, and ease handling, storage and transportation.[66-68] There are different types of dryers available, but only a small number of them are used in coal preparation. Coal thermal dryers can be categorized into two main groups, direct or indirect heat exchange. The most common dryer in use today for coal preparation industries is the direct- heated, fluid-bed type dryer. This type of dryer is generally used for fine particle drying, where 16
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hot gas passes through the fine particles inside the dryer and removes water from the unit. In the indirect heat exchange method, the fine particles in the chamber of the dryer are externally heated by hot gas to obtain dry product. It is mostly employed when environmental concerns arise. [66-68] 1.2.4. Dewatering Parameters The performance of most of the dewatering tools that are used today depends strongly on several parameters of particle-aqueous systems. Parameters which affect the dewatering process include equipment properties, mineral type, particle size and distribution, physical and chemical properties of the mineral surface, cake structure and thickness, impurity content, surface oxidation, solid/liquid ratio, and the presence of chemical additives.[10, 14, 25] a) Effects of Physical Properties To improve dewatering to a large extent, understanding the characteristics and properties of coal and their effects on dewatering behavior is of utmost importance. Coal is the most abundant resource of fossil fuel available. It is 20 times more abundant than crude oil and over 1.5 times more than other fossil fuels and crude oil combined. Coal is an inherently heterogeneous material, possessing organic matter, mineral matter, and has an extensive pore structure. This is shown below in Figure 1.7.[1, 6, 10] 17
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water that is not readily removable by mechanical methods, chemically bound to the particle, and which is a part of the particle. It is also generally known as intra-particle moisture. This is extensively seen in the structure of low rank coals, such as lignite, and it can only be removed by thermal drying methods (over 100oC). The capillary water is trapped in small channels of the filter cake, which, again, requires more complex and intensive methods for removal. Free water, which is not associated with solids and behaves thermodynamically as pure water occupying the bulk of the slurries, can be removed by any means of mechanical dewatering. Screens, thickeners, cyclones, and centrifuges are widely-used tools to remove this type of water.[23, 24, 26, 38, 41, 56] The existing relationship between water and particles is of interest in the dewatering process, as well. Essentially, particle-water interaction has three main states. Figure 1.9 shows a brief description of these 3 stages. Liquid More Almost Middle Small None Content Saturated State Slurry Capillary Funicular Pendular Dry -First- -Second- -Third- Stage Stage Stage Schematic Diagram Figure 1.9 Schematic of particle-water relationship in cake structure In the saturated, or capillary, state, where all the pores and voids (or capillaries) of the particles are filled with water, the liquid pressure is lower than the air pressure, and the surface 19
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tension, capillary radii, and the contact angle of the system determine the magnitude of capillary forces. Only if the applied forces of vacuum, pressure, centrifugal, and gravity are greater than the capillary forces, can water be removed. This is called the funicular state, where the remaining water starts to create bridges around the contact points of the particles. If the applied force is further increased, it will lead to the formation of lenses of water between the particles. Most of the time, this determines the final cake moisture. Figure 1.10 shows three main stages of the water content of the particles under applied forces.[24, 30, 31, 66, 69, 70] Figure 1.10 Relationship between applied pressure and moisture reduction The deposition of solids on a filter medium is achieved by applying vacuum, pressure, or centrifugal forces to a suspension. Throughout this process, several stages occur starting from cake formation through the end of the drying cycle. The stages of the dewatering process are illustrated in Figure 1.11. Figure 1.11(A) represents an enlarged slice of the filter medium and slurry, where the initial bridging of particles begins. In this stage, the filtration commences, and 20
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the first few layers of the cake start to emerge. Figure 1.11 (B) shows the formation of cake on the filter media, and Figure 1.11 (C) shows the cake after it is formed. The time that passes during these first three stages is called the cake formation time. Once the cake is formed, it gets compacted and air starts to enter the cake structure, displacing the water from the largest pores (shown in Figure 1.11 (D) and Figure 1.11 (E)). Finally, macropore and micropore channels (capillaries) are formed where the air breakthrough is achieved, draining more water from the cake. These three stages represent the dry cycle time.[23, 30, 70] A B C D E F Figure 1.11 Cake formations during dewatering stages During the drying time, applied pressure, ∆P, is not capable of removing water horizontally from the fine capillaries in the cake. Cheremisinoff, et.al, suggested a model with zones between the particles in which water is located (shown in Figure 1.12). 21
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Figure 1.12 Schematic of the moisture zones Once the pressure is applied, the water in Zones 2 and 4 can be removed and displaced with air. On the other hand, the water in Zones 1 and 3 will not be affected by the airflow, which determines the final moisture, and water will still be located between the particles. To displace water with air in these zones, chemicals can be used to increase the hydrophobicity of particles and lower the surface tension of water, which, in turn, increases water removal.[24, 26] b) Effects of Chemical Properties The use of chemical additives as dewatering aids to increase the mechanical filtration efficiency has become more crucial in mineral processing industries. No matter what dewatering equipment is employed, it is almost a standard procedure to pre-treat the slurry with the addition of chemicals. The applications show that using the appropriate chemicals may provide significant improvements in dewatering efficiency as a means of reducing moisture content in the filter cake and increasing the dewatering kinetics. Practically, chemical additives can be fitted into two main categories, flocculants/coagulants and surfactants.[25, 44, 71-73] Flocculants and coagulants are the chemicals that change the packing density and inter- particle separation distances in the particle structure, modifying the compressibility and the 22
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drainage features of the formed cake. Surfactants, on the other hand, are long-chain polymers that are absorbed between two surfaces in order to change the surface properties. [25, 44, 71-73] Coagulants or inorganic salts (electrolytes), such as aluminum, copper, chromic, and ferric and calcium sulfates (or chlorides) affect the composition and the extent of the electrical double layer surrounding the particles. They also change the zeta potential of the particles, as well as the inter-particle electrostatic repulsion, which in turn lead to coagulation.[20, 21, 74, 75] The balance between the repulsive, double-layer force and the attractive Van der Waals force determines whether coagulation will occur. If the particle surfaces are not charged, particles come closer to one another, which in turn help the attractive forces bring them together to create small agglomerates. Conversely, the surfaces of the particles may be charged electrically, creating repulsive forces between the particles and preventing the spontaneous agglomeration brought about by Brownian motion. This phenomenon is shown in Figure 1.13. A B (Stabilized Particles) (Coagulated Particles) Figure 1.13 Potential energy curves 23
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The curve (A) in Figure 1.13 A represents Van der Waals energy. It is an attractive force having an increasingly negative value, which is effective in small distances between particles. Curve (B) represents the repulsive electrical force and curve (C) is the outcome of these two forces, showing the maximum energy barrier for the colloidal system to become steady. At this point, because the resultant force is repulsive, coagulation does not occur. To allow the agglomeration to take place, chemical additives can be used to change the surface charge in favor of Van der Waals forces. Figure 1.13 B shows the changes on the particle surface when coagulant is introduced to the system. It reduces the electrical force and brings the curve (B) to lower values. This causes the resultant curve (C) to fall below zero and allows the particles to coagulate – if they come close enough – and the Van der Waals forces can be effective.[20, 31, 58, 71, 73, 74, 80] The magnitude of the repulsive forces at the interface of the particles and the liquid determines the colloidal stability. This stability can be explained by Stern’s double-layer theory. Particle Surface Surface Potential Shear Plane Zeta Potential Diffuse Layer of Ions Shear Plane in Liquid Bound Layer of Ions Distance into Liquid Figure 1.14 Double layer model 24
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The suspended particles, having a certain type of charge in an electrolyte solution, attract the ions of opposing charges from the liquid, repel the ions that have similar charges, and develop an electrical double layer of ions as shown in Figure 1.14. The ions that are located in the inner stratum of the double layer are more strongly bound, and the ions that are located in the outer stratum are weaker and more diffuse. The electrical potential between these two stratums is called the zeta potential.[21, 50, 58, 71, 72, 80] The ions of a coagulant compress the double layer by bringing the charges within the plane of shear between the bound and the diffuse layers. This compression becomes more effective when multivalent ions are in solution because they have greater charge concentration. As a result, the zeta potential is decreased. The minimum ionic concentration required to produce coagulation and its overall effect is described by the Shulze-Hardy rule. According to the Shulze-Hardy rule, to start coagulation the minimum ionic concentration must be proportional to the sixth power of reciprocal counter ion charge. The Al3+, Fe3+, and Ca2+ ions are the commonly used ions as coagulants. The pH level of the slurry is important for the hydrolysis of these salts. pH values of a slurry that are above or below the effective pH value range for a given specific salt, or coagulant, may not allow hydrolysis, and chemical dosage requirements may be higher than the ideal dosage.[21, 50, 58, 71, 72, 80] Flocculants are long-chain polymers, or electrolytes, that cause the particles to aggregate by forming bridges between particles. Typically, flocculants are categorized into two groups: natural and synthetic. [71, 81] Natural polymers, such as starches, gums, alginates, and polysaccharides, are mostly short-chain, neutral, organic compounds. The effectiveness of these polymers is dependent on the pH of the slurry as well. At alkaline and neutral conditions, polysaccharides are more 25
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effective while, gums, alginates, and starches are more effective at acidic conditions. Because natural polymers that are used as flocculants have short, rigid chain structure and low bonding strength, their shear strength is very low. Thus, for flocculation applications, excessive amounts of these polymers may be needed. In recent times, synthetic polymers, or polyelectrolytes, have displaced these natural materials, as these polymers can be designed to give desired behaviors, such as providing more durable flocs and more economical dosages when applied to a particular problem.[25, 58, 77, 78, 80, 83] The synthetic polymers are based on polyacrylamide or one of its derivatives that may have very large polymer chains. These chains consist of anionic, cationic, or neutral groups, causing the polymer to uncoil and bond to the surface of the coal or clay minerals. This may result in a desired or undesired selectivity. Polymers with long chains have more contact with particles and produce large and open floccules. However, they have low shear strength and contain high residual moistures. In contrast, shorter and lesser-charged polymers generate more compact granular floccules and improve the filtration characteristics. The high shear forces due to dewatering methods might reduce the effectiveness of flocculation on fine particle dewatering. When the flocculants/polymers in solution are introduced to the slurry, they work in two stages: ion, or charge, neutralization and bridging. Although, the exact absorption mechanism is still not fully understood, initial adsorption occurs by strong bonding between the polymer and the solid particles. It involves a molecular bridge, or a series of bridges, between polymer and the solid particles. The polymer chain from the solution adsorbs onto the solid particles and, when the extended part of the chain or particles come close enough, creates bridges and continues to adsorb onto the other particles. These basic floccules grow by bridging with other solid particles until a most favorable floc size is formed. This is a quick and, unlike coagulation, irreversible 26
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reaction, which again, needs low heat rates to avoid breaking the molecular bridges in order to initiate a fast settling of solid. The use of flocculants can increase the filtration rate, as well as the cake thickness, by several multiples. The combined use of anionic and cationic flocculants exhibits further improvements. It is also reported that anionic flocculant is more effective in promoting fine coal dewatering than cationic flocculant in vacuum filtration. On the other hand, cationic flocculant was more effective in high shear centrifugal filtration. The positive increase in kinetics is, however, accompanied by an increase in moisture content resulting from water being trapped in the agglomerate structure. In addition, it was observed that the use of flocculants increased final cake moisture due to increased kinetics, thicker filter cake, and water trapped in the agglomerate structure.[25, 30, 50, 54, 58, 72, 73, 77, 78, 80, 82, 83] Surfactants, also referred to as surface-active agents, are the chemicals that modify and control interfacial interactions by adsorption. This can take place between any two phases or immiscible components, including solid-vapor (S/V), solid-liquid (S/L), solid-solid (S/S), liquid- vapor (L/V) and liquid-liquid (L/L) interfaces in a system. Surfactants consist of two compounds, hydrophobic tail and hydrophilic head, and they are characterized by the chemical structure of their hydrophilic groups as anionic, cationic, non-ionic, and amphoteric (shown in Figure 1.15 below).[31, 80, 84] Anionic Cationic Hydrophilic Hydrophobic Amphoteric Head Tail Non-ionic Figure 1.15 Surface active agents 27
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In the filtration process, these surfactants are used to control the characteristics of the interface between a solid and a liquid by building molecular films, resulting in a reduction of the viscosity and the surface tension of the liquid and an increase in the contact angle. This supplies a better water drainage from the filter cake capillaries by simply lowering capillary retention forces and increasing hydrophobicity, which provides lower final cake moisture. Changes in the surface chemistry of the particles and filtrate by adding surfactants increases the contact angle and makes the surface more hydrophobic. This relationship is shown in Figure 1.16.[31, 80, 84] Figure 1.16 Contact angle and hydrophobicity If the surface potential of a particle in a liquid has the same sign as the surfactants, repulsive force is, in effect, between the particles and the surfactants which stabilizes the additives in solution, preventing any absorption on the surface of the solid. When counter ions are added to the system, these ions populate between particle surfaces and the head of the 28
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surfactant, allowing adsorption. The adsorption occurs in two ways: ion exchange and ion pairing. Ion exchange happens when the surfactant molecules are placed on the charged side of particles which have not been occupied by the counter ions. In ion pairing, the surfactant molecules displace the charge of the same counter ions and stay on the surface. Based on the orientation of the surfactant molecules, the surface chemistry of the particles changes, and becomes hydrophobic or hydrophilic. Depending on the surfactant concentration, the formation of the additives forms either a neutralized monolayer or reversed, secondary bilayer (shown in Figure 1.17).[24, 25, 31, 71, 77, 81, 86] A B C Figure 1.17 Schematic illustration of the layer formations When the surfactant dosage is low, few or no surfaces may be coated, not causing a change in hydrophobicity (Figure 1.17-a), while higher dosages form a close-packed monolayer, representing neutralized surface charges (Figure 1.17-b). If the amount of chemical is further increased or overdosed, there will be a bilayer or reverse orientation (Figure 1.17-c), which, in dewatering, will decrease the hydrophobicity of the particles. [24, 31, 71, 77, 81, 84-86] 29
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Polyelectrolytic polymers are highly charged, short-chain polymers that are used when the solid content is very low. These types of polymers are used when the flocculants cannot be effectively employed.[24, 31, 38] 1.2.5. Dewatering Theory a) Dewatering Kinetics Filtration kinetics is an important characteristic of fine particle dewatering that determines the volumetric flow rate of liquid to be removed through a porous media created by the particles and the filter throughput. Darcy first described the filtration kinetics in 1856 as the rate equation for the dewatering process. Darcy’s basic filtration equation relating the flow rate is [20, 26, 44, 88] : dV A ∆P = K [1] dt η L where V is the volume of fluid, t is the filtration time, ∆P is the pressure drop across the cake, and L is the thickness. A is the cross-sectional area of the cake, η is the absolute viscosity of liquid, and K is the rate constant referred to as the permeability of the cake. The equation reveals a basic relationship; the rate of dewatering is proportional to the pressure gradient and the cross- sectional area and is inversely proportional to the viscosity. Equation [1] is also written in the form: dV A ∆P = [2] dt η R where R is the medium resistance (the medium thickness is divided by the permeability of the cake). If the suspension does not include any solid particles, all the parameters in Equations [1] and [2] will be independent of filtration time, t. This will result in a constant filtration rate for a 30
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constant pressure drop. It also represents a linear increase of the cumulative filtrate volume; however, if the suspension contains particles, resistance of the cake will increase gradually with time and lead to a drop in the flow rate.[20, 22, 26, 39, 44, 88] In batch filtration, resistance has two components, medium resistance, R, which can be assumed constant, and cake resistance, R , which increases with time as a result of increase in c cake thickness (shown in Equation [3]). dV A ∆P = [3] dt η(R+R ) c If the resistance of the cake is assumed to be directly proportional to the amount of cake deposited (w), then R =αw [4] c where α is the specific cake resistance. The mass of cake deposited is a function of time (t) and can be related to the accumulated filtrate volume, V by wA=cV [5] where c is the concentration of solids in the system (mass per unit volume of the filtrate). By integrating and rearranging Equations [3], [4] and [5], the general filtration equation can be reached. The general filtration equation, Equation [6], is shown: dt αηc ηR = V + [6] dV 2A2∆P A∆P The fundamental filtration parameters, such as α and R, can be determined to evaluate the effects of different conditions on filtration kinetics. The filtration kinetics can be altered using chemical additives, which change filter cake properties, such as permeability (K), cake porosity (ε), and the specific surface area of particles (S). [20, 22, 26, 39, 44, 88] 31
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b) Dewatering Thermodynamics To remove the liquid located in these capillaries, it is important that the applied pressure be larger than the capillary pressure, (p), which is defined by Laplace: 2γ cosθ p= 23 [10] r where, γ is the surface tension of liquid, and θ is the water contact angle. The Laplace equation 23 suggests that decreasing surface tension leads to a lower capillary force and improved cake dewatering. Increasing the solid/liquid contact angle, θ, lowers the cosθ, and as a result, it s decreases the capillary force. This controls the water removal from the cake.[25, 31, 39] By using an appropriate surface-active reagent, it is possible to hydrophobize the surface, decrease γ , and increase contact angle by absorption in such a way that its hydrophobic part is 23 oriented away from the surface. The Young’s Equation describes the relationship between the solid/liquid contact angle and the work of adhesion, a measure of how strongly water is bound by the solid surface: [44, 71, 89] γ =γ cosθ+γ [11] 13 23 12 where θ is the solid/liquid contact angle, γ is the surface free energy of the solid/air interface, 13 γ is the surface free energy of water/air interface, and γ is the surface free energy of the 23 12 solid/water interface. The free energy change per unit area, ∆G/dA, is determined by the following equation in a solid/liquid/air system. This is also known as the Dupre equation.[31, 44, 71, 89] 33
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dG W = =γ +γ −γ [12] adh dA 13 23 12 By substituting Equation [11] into [12], the following relationship can be obtained (Young-Dupre Equation): W =γ (1+cosθ) [13] adh 23 The Young-Dupre equation suggests that the work of adhesion between solid and liquid can be calculated from the liquid surface tension and the contact angle. The spontaneous hydrophobization and effect of contact angle is illustrated in Figure 12, where A is the solid, B is the liquid, and C is the air. [31, 44, 71, 90] γ γ lv lv γ θ γ θ γ sv γ sv sl sl A B C Figure 1.18 Schematic representation of solid/liquid/air interfaces For a completely hydrophilic surface, θ =0o, cosθ =1, and W will be at their 12 12 adh maximum values. On the contrary, for a completely hydrophobic surface, θ =180o, cosθ =0, 12 12 and W will be at their minimum values. This, in summary, suggests that for a dewatering adh process, the work done on a hydrophilic solid surface can be minimized by simply decreasing water/air surface tension and increasing the contact angle, as seen in Figure 12.[31, 44, 71, 89] Novel dewatering aids introduced in this study are non-ionic, low hydrophile-lipophile balance (HLB) number surfactants. The surfactant molecules adsorb on a hydrophobic solid surface, such as coal, as a result of hydrophobic attraction and, thus, increase its contact angle. 34
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CHAPTER 2 LABORATORY AND PILOT SCALE EVALUATION OF DEWATERING AIDS 2.1. INTRODUCTION The fine size coal production has increased as a result of several factors. These factors can be broadly explained as follows[1, 2]; i) The mechanized ROM coal production methods have increased the fine coal production ii) The coal produced, for both coking and power industries, has to meet with certain quality constraints, such as calorific value, ash, sulfur and moisture content. To meet these requirements and produce a higher quality product, the raw material should be crushed to a lower top size for improved liberation. iii) The possibility of economical recovery of fine size fraction of coal that reports to plants’ discard streams iv) Recovery of the fine/ultrafine coal from the waste ponds which represents an economically viable resource Froth flotation is the widely used and the most effective separation method for fine coal cleaning. It is a wet process and the separation results in two products in the form of slurry, i.e. the concentrate (coal) and the tailing (ash-forming minerals). Of the products, the tailings are discarded to the waste ponds and the coal is further processed before it reaches to the final consumer.[2-4] In processing plants, clean coal is dewatered by means of filters, such as vacuum disc, horizontal belt and drum filters, and centrifuges. However, the larger surface area of fine/ultra fine particles per mass results in more water adsorption. Additionally, the fine particles create 43
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smaller size capillaries in the filter cake from which water cannot be removed easily during the application of vacuum or air pressure. As a result, these dewatering methods cannot produce the desired moisture levels if there is not a thermal drier. Therefore, fine coal dewatering is the most difficult and costly operation in preparation plants.[5, 6] Previous studies on fine coal dewatering addressed the problem and a number of dewatering aids were developed to lower the final cake moisture to the extent that is not achievable by mechanical means. In this study, laboratory and pilot scale tests were conducted on a variety of fine coal samples to do engineering evaluation of these dewatering aids; and possible industrial applications have been investigated. 2.2. GENERAL EXPERIMENTAL DETAILS 2.2.1. Samples Laboratory- and pilot-scale dewatering tests were conducted on various samples comprised of different mixtures of coarse and fine coal. Following are the samples that were used in these tests: i) Flotation feed (cyclone overflow or underflow) ii) Flotation product iii) Filter feed (blend of flotation and spiral products) These samples were received from different preparation plants located in North America region. Table 2.1 shows the selected coal samples for the dewatering tests. 44
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Table 2.1 Names of the operations and their locations from where the samples received for dewatering aid evaluation tests Operation Location Mingo Logan West Virginia Coal Clean West Virginia Concord Alabama Buchanan Virginia Moatize Mozambique Elkview BC, Canada Pinnacle Reclamation Virginia These samples were tested i) as received, if the sample was directly collected from filter feed stream, ii) after upgraded with flotation, if it was cyclone overflow or cyclone underflow, iii) after blended at different ratios. For laboratory dewatering tests, the samples were collected or received as coal slurry in 5 gallon buckets. To minimize the adverse effects of superficial oxidation of the coal samples, the dewatering tests were conducted within 24-48 hours of receipt. The samples were first subjected to solid content determination (% solid) and particle size distribution determination. When flotation step was carried out, Denver D-12 flotation equipment was used, where kerosene and MIBC were added as collector and frother, respectively. After dewatering aid addition, each sample was conditioned with a stand-alone mixer to ensure a proper dispersion and adsorption of the dewatering aids. 45
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2.2.2. Methods and Procedures ` a) Laboratory Scale Dewatering Test Equipment and Procedure The laboratory-scale dewatering tests were conducted using the following equipments: i) 2.5 inch diameter Buchner funnel ii) 2.5 inch diameter pressure filter Buchner Funnel was used in the bulk of the tests fitted with various sizes of filter cloth depending on the samples treated. It was mounted on a vacuum flask, which in turn was connected to a larger vacuum flask to protect the pump itself and stabilize the vacuum pressure. Before initiating the filtration, first, a known volume of coal slurry was transferred to container, to which a known amount of a dewatering aid (or a mixtures thereof) was added by means of a microliter syringe. The coal slurry was then subjected to mixing with a three-blade propeller type conditioner for a given time to ensure that proper chemical dispersion and adsorption were achieved. After conditioning, the slurry sample was poured into the funnel before opening the vacuum valve. Filtration started when a vacuum was applied to the slurry. After the cake formation, the vacuum pressure was kept on for a desired length of time to remove the remaining water trapped in the capillaries. This period was called the dry cycle time. The amount of volume added to the Buchner funnel determined the cake thickness. After the pump was stopped a representative sample was removed from the cake and dried for a give time. The filter cake was weighed before and after drying; and moisture content was determined from the dry-wet weight differences. In each experiment, the cake thickness, set up and actual vacuum pressure and cake formation time were recorded. Figure 2.1 shows the basic experimental set-up used for the Buchner funnel filtration tests. 46
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(Figure 2.2). The vacuum disc filter consisted of a disc mounted on a horizontal shaft. The disk had interchangeable elements which could be changed for fitting and removing filter cloths. The disc rotated in a sump into which the suspension was fed (the sump also has two agitators to provide even cake formation), and a vacuum was applied through the core of the shaft. The submerged sector of the disc collected the cake and then removed it by blow-back air cake discharge system utilized in conjunction with a scraper just before re-entering to the sump. The specifications of the equipment were as follows: • 2 ft diameter with 10 removable sectors • 0.2 - 2.0 ft2 of adjustable filter area by varying number of filter sectors used • Peterson “Syncro-Blast” air cake discharge system • 0.5 - 12 minutes per revolution • 29 inches Hg vacuum pressure at 2.5 cfm. • Dual filtrate sumps: 25 gal capacity each • Connected HP: 2.25 • Dimensions: 5ft. High x 5ft wide x 4ft deep. • Weight: 1,800 lb. 48
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compressor. Coal slurry was fed to the column from an agitated tank using a variable-speed centrifugal pump. Pulp level in the column was maintained by adjusting the tailings flow rate using a pneumatic control valve. The valve actuated based on readings from a pressure transducer mounted in the side of the column. Wash water was added to the froth to minimize the entrainment of fine mineral matter. Chemical metering (reagent) pumps were used to add the desired dosages of frother and/or collector to the feed slurry. Head Pneumatic Air Froth Tank Sampler Compressor Launder Viewing Reagent Feed Window Pump Power Mixer Supply Column Speed Tank Feed Electronic Controllers Sump Timer Sparger Breaker (In - Line Mixers Box Mixer) Conditioner Feed Sparger Circulation Tanks Pump Pump Pump (a) (b) Figure 2.5 Photographs of (a) the column unit, (b) the conditioner A schematic diagram of the Conditioner Module is shown in Figure 2.5 (b). The module incorporated two 20-liter conditioning tanks that were operated in series to provide up to 10 minutes of conditioning time. The conditioning tanks were equipped with single-impeller mixers that could be varied in speed from 0 to 2500 rpm using electronic controllers. To ensure that 52
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coarser particles did not settle when low feed rates were used, the slurry in the conditioning tanks was continuously circulated through a head tank using a centrifugal pump. The head tank was equipped with an automated sampling system that consisted of an electronic timer and a pneumatic sample cutter. During operation, the sampling system was used to divert a defined portion of circulated slurry to the Filter Module (or any other downstream operations). A chemical metering (reagent) pump was used to add the proper dosage of dewatering aid to the feed slurry as it enters the conditioning tanks. To obtain a consistent feed rate, a small peristaltic pump was installed at the plant to pump feed slurry from the plant’s filter feed box to the conditioning module. 2.3. FIELD TESTING 2.3.1. Test Program Overview A series of laboratory dewatering tests were conducted to identify the best chemicals and optimize the dewatering parameters. After successfully completing the bench-scale, a diverse set of field tests were undertaken using the mobile test modules described previously. The on-site field tests were required in order to provide site specific operational information and scale-up data for the development of the POC plant. The field tests were conducted using samples comprised of different mixtures of coarse and fine coal obtained as flotation feeds (either cyclone overflow or underflow), flotation froth products or filter feeds (blends of flotation and spiral products). As a result, the various samples were tested as-received (if the sample was directly collected from filter feed stream), after upgrading with flotation (if it was cyclone overflow or cyclone underflow), or after blending at different mass ratios. In support of the field testing effort, numerous laboratory tests were also performed. The specific procedures used for conducting these laboratory dewatering tests have been described previously. 53
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2.3.2. Mingo Logan Site a) Site Description The Mingo Logan Coal Preparation Plant is located in the counties of Mingo and Logan, WV. This is in Central Appalachia Region. As Arch’s principal source of metallurgical coal, the plant produces approximately 3.9 million tons (2006) at a quality of 13,000 Btu/lbs. and, 1.1 lbs. SO /MM Btu. The preparation plant consists of two independent 800-ton circuits, each 2 provided with separate surge bins to ensure uniform splitting of the plant feed. Each of the circuits consists of heavy media vessels for the 160 x 7.7 mm (6 x 0.3 inch) material, heavy media cyclones for the 0.3 x 16 mesh material, spirals for the 16 x 65 mesh material, and froth flotation for the 65 mesh x 0 material. Dewatering is accomplished through centrifuging for the various size fractions. However, the dewatering efficiency was not satisfactory due to (i) the fine particle size of flotation product, (ii) the screen bowl centrifuges were not capable of capturing the fines, and (iii) the accumulation of excessively stable foam over the screen bowl centrifuges. Also, the issues resulted in high final cake moistures and loss of considerable amount of valuable material that might be recovered by other means. If recovered and dewatered more efficiently, such losses could be turned into profits. An extensive laboratory and pilot-scale dewatering test program was conducted to study the feasibility of new approaches on more efficient dewatering methods and the recovery of the fine particle size material which reports to the plant’s discard stream as a result of centrifuge’s lack of fine particle capturing capability. To meet the objectives, exploratory laboratory dewatering tests were conducted to evaluate the performance of various types and dosages of newly developed fine particle dewatering aid technology. Data from the laboratory studies were used to provide technical justification for the pilot-scale test program undertaken at a coal 54
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preparation plant using a horizontal belt vacuum filter. Investigations incorporated the study for the possible utilization of these technologies in industrial applications for fine coal beneficiation. b) Reagents The investigation, both laboratory and pilot-scale, was performed with varying amounts of three types of dewatering aids, namely RW, RU, and RV. Since these dewatering aids are insoluble in water, they were dissolved in a solvent. In both laboratory and pilot-scale experiments diesel was used as the solvent. The ratio of reagents-to-solvent was optimized in previous studies by varying the individual dosages (0.5 to 3lb/ton), while maintaining the total blend dosage constant. For this test program, the optimum combination for a given dewatering aid and solvent is one to two (1:2) dewatering aid-diesel ratio. The flocculants, Nalco-9822 and Nalco-9806, were prepared at a 0.09 % solution and used both alone and in conjunction with dewatering aids. After examining various dewatering aid and flocculant combinations and their orders of additions, the best combination was found to be to add dewatering aids first, then to add flocculants. As it is going to be discussed in the following sections, the agitation and mixing intensity play an important role in determining the chemical performance. The dewatering aids require certain amount of mixing intensity; however, it may be excessive shear for a given flocculant. Excessive shear may lead to chain breakage, which reduces the effectiveness of a flocculant for bridging. Therefore, flocculant was added after mixing the dewatering aids; and the new combination was conditioned at a very low intensity for 15-20 seconds. 55
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Table 2.2 Size distribution of Mingo Logan flotation product Size (mesh) Weight (%) 65 10.95 65X100 9.25 100X150 11.91 150X325 22.25 325 45.65 Total 100 c) Coal Samples The dewatering tests were conducted on feeds comprised of three different mixtures of coarse and fine coal feeds. The first series (Series A) was conducted using a fine coal sample from a classifying cyclone overflow that had been cleaned by flotation. The product solid content was 23% by weight. Approximately 45%of the material was finer than 325 mesh size. Table 2.2 shows the sieve analysis results on flotation product sample. In some of the experiments, the cyclone overflow sample was also used to produce clean flotation product for dewatering tests. The second series (Series B) was conducted using a mixture of fine and coarse coal. The flotation product sample was mixed with a portion of the spiral product at a ratio of 3:1 (i.e., 75% fine coal and 25% coarse coal) to prepare the dewatering feed slurry for dewatering tests. The solid content of the combination of Table 2.3 Size distribution of Mingo Logan mixture sample Size (mesh) Weight (%) 35 17.80 35x100 22.25 100x325 23.25 325 36.71 Total 100 56
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spiral/flotation product slurry was approximately 27% by weight. The third and final series (Series C) was performed with a feed comprised of 50% coarse coal from the spiral circuit and 50% fine coal from the conventional flotation circuit. Table 2.3 shows the size distribution of mixed clean spiral and flotation product (at 1:1 ratio) sample. The solid concentration of the slurry was about 25% by weight, while 36% of the solids were minus 325 mesh. d) Laboratory Procedures All the samples including the flotation product, obtained in the lab using cyclone overflow sample or collected directly from the preparation plant, and the mixture sample were conditioned with the dewatering aid before the dewatering tests. As stated earlier, a conditioning system is very important for the chemical dispersion and adsorption. The surfactants adsorb on the surface of the solid leading to an increase in the solid/liquid contact angle and a decrease in liquid surface tension. Each slurry sample subjected to mixing to ensure that proper chemical dispersion and adsorption was achieved. The sample was first agitated in a 300 ml Plexiglas cell equipped with a three-blade propeller-type mixer. The mixer was designed to control the mixing strength by adjusting the input current and voltage of its motor. Once the sample was mixed, it was transferred to a Buchner vacuum filter and subjected to dewatering tests. When flocculants were used, proper mixing was supplied. This ensured that high shear conditions neither degraded nor rendered the flocculant ineffective. Essential test parameters affecting the final cake moisture and filtration performance, such as pressure level, specific cake weights, and filtration time were recorded. Upon receipt, all the samples were subjected to dewatering tests within 24 hours to minimize the effects of aging and artificial oxidation that can change surface properties rapidly and affect the filtration behavior. 57
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e) Pilot-Scale Procedures Pilot-scale dewatering tests were conducted on feeds comprised of mixtures of coarse and fine coal feeds. Feeds specifically used, for example, are fine flotation product or combinations of coarse spiral and fine flotation products. The coal feeds, flotation product/spiral product coal sample, were reasonably consistent for most test work. The blend sample contained approximately 28% of solids by weight and 12% ash on dry basis. Table 2.4 provides the particle size and ash analysis results. The particle size is almost uniformly distributed over the range of 18 mesh x 0, but obviously, the fine particles contain more ash. As shown, 68% ash is included in the fine fraction (325 mesh x 0). Table 2.5 shows the particle size and the ash contents of each size class of the flotation product. Of the sizes, 43% of the particles was passing 325 mesh (-44 µm), and more remarkably, 81% ash was distributed in this fine fraction. Table 2.4 Particle size and ash content analysis of Mingo Logan plant spiral/flotation product mixture (on-site samples) Size Weight Ash Ash (mesh) (%) (%) Distribution (%) 35 19.66 3.74 6.09 35x100 22.54 4.75 8.87 100x325 23.83 8.55 16.87 325 33.98 24.23 68.18 Total 100.00 12.08 100.00 Table 2.5 Particle size and ash content analysis of Mingo Logan plant flotation product (on- site samples) Size Weight Ash Ash (mesh) (%) (%) Distribution (%) 35 1.77 2.53 0.48 35X100 15.06 2.08 3.45 100X325 40.22 3.38 15.00 325 42.96 17.1 81.07 Total 100.00 9.06 100.00 58
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The on-site pilot-scale test work was conducted using a conditioning tank and the pilot- scale horizontal belt filter built by WestTech/Delkor. The spiral/flotation product mixture intercepted from the screen bowl feed pipe was fed to a 35 gallon conditioner. Flotation sample was taken from the distribution box. After conditioning with the dewatering aids under test, a desired amount of coal slurry was then fed to the filter. The total feed rate to the conditioning tank was generally controlled at 13gal/min. This allowed approximately 3 minutes of conditioning time for dewatering aids. The dewatering aids, RU and RV were used. The flocculant, R9822 from Nalco, diluted to 0.09% solution, was directly pumped to the horizontal belt filter’s feed pipe. The belt speed of the filter was adjusted to allow the materials travel over the vacuum zone in the time interval between 65 to 184 seconds, which enables to investigate the effect of different cake thicknesses under certain filter feed rate, and of different dry cycle times. The cake sample was taken for moisture analysis periodically from the ending point of the belt when a steady-state was achieved after the test parameters were changed. f) Laboratory Test Results (Series A – Fine Coal Only) In this series of experiments, Mingo Logan’s clean coal product from the conventional flotation circuit and cyclone overflow samples were used. The first dewatering tests were conducted to determine whether the flotation product coal samples provided by Mingo Logan Preparation Plant would respond well to the addition of the novel dewatering aids. The preliminary results showed that with the addition of dewatering aids, it is possible to reduce the final cake moisture content of fine coal cake by about 20%, while also increasing the rate of dewatering. The surface moisture was reduced down to about 19% using 3 lb/ton RW, where it was approximately 23% for control tests at about 8-11mm cake thickness. As many factors 59
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influence the filtration performance, particle size distribution and corresponding ash contents were the dictating parameters. Considering the amount of material under 325 mesh size in the flotation product sample, a portion of ultra-fine particles was removed from the sample via desliming. The tests results on the deslimed sample showed that moisture was further decreased to 16.7 % at the same RW dosage. This is another significant moisture reduction from a baseline of 21%. This moisture reduction in both baseline and with reagent tests is achieved by desliming of the ultrafine fraction that results in more freely draining filter cake capillaries. This also prevented the fines from forming an impermeable layer which might be positioned on the top of the cake. The screen analysis results also showed that 81% of the ash was in the minus 325 mesh size fraction. This material, which consists of clays and slimes, is hydrophilic in nature and this affects the dewatering performance negatively. The use of flocculants may be another way to compensate the negative effects of the ultrafine particles. The principle of using of flocculants is to bring the fine particles together in the coal slurry and create looser packing in the filter cake. This loose packing results in larger capillaries between the aggregates and a more porous, permeable cake. This allows a rapid drainage of water from these voids, which, in turn, increases the filtration rate. To investigate the effects of flocculants on dewatering kinetics, a series of tests was conducted. To optimize the dosage, various amounts of flocculant were tested, from 5 g/ton to 75g/ton. It was determined that 25 g/ton was the most appropriate flocculant amount when being used alone or in conjunction with other chemicals. The test results showed that in most cases, the addition of flocculant did not improve the final cake moisture, due to the water trapped inside the flocculants. Instead, the dewatering kinetics increased significantly i.e., 30% to 75%. 60
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Another way of lowering the moisture may be to clear out the excessive amount of ash- forming minerals in the fines. To investigate this idea, prior to laboratory dewatering tests, the plant’s clean coal product was subjected to another step of flotation using 1 lb/ton (454g/t) RV (in Diesel (1:2)) as collector and 100g/t MIBC as frother. The particle size analysis results showed that the 37.6% of the re-floated sample was minus 325 mesh. Dewatering test results showed after its addition, RW, at about 3 lb/ton, can reduce the moisture to 15.5%, where the baseline was approximately 20%. In addition, the dewatering kinetics of the coal sample was also increased by 50% as a result of the increased hydrophobicity. As stated earlier, the surfactant adsorption is very important so that it can lead to an increase in solid/liquid contact angle and a decrease in liquid surface tension. For this reason, it is very important to have an effective conditioning system. To investigate and optimize the effectiveness of the dewatering aids and their performances, two series of filtration tests were conducted at various mixing intensities and times. Table 2.6 gives the laboratory test results obtained on the flotation product sample using RW at 3 lb/ton at about 20-24 mm cake thicknesses. As shown, the moisture reduction was substantially improved when mixing intensity was increased. The use of RW at 3 lb/ton reduced the filter cake moisture from baseline value of 30.02% to 25.98% and 25.45% when using low and medium-energy agitation at one minute, respectively. The cake moisture was further reduced to 20.26% moisture when Table 2.6 Effect of mixing intensity and conditioning time on Mingo Logan flotation product (20 inHg vacuum and 3 lb/ton RW) Speed Moisture @ specified conditioning time Level 1 min 2 min 0 30.02 30.02 Low 25.98 25.29 Medium 25.45 23.91 High 20.26 18.66 61
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using high-energy agitation at the same reagent dosage of 3 lb/ton. The moisture reduction showed a similar trend, but improved final cake moistures were obtained when the agitation time was increased to two minutes. The final cake moisture was reduced to 23.91% and 18.66% using medium and high-energy conditioning, respectively, at the same dewatering aid dosage. It was found out that two minutes of conditioning at high intensity mixing was optimum. Beyond two minutes of conditioning, there was no change in the residual moisture of the cake. These results clearly demonstrate that the importance of proper conditioning when using the novel dewatering aids. In the light of the results obtained in the initial laboratory filter tests, using dewatering aids were believed to be a promising method because it could not only remove water but also increased the filtration kinetics. To evaluate the filtration performance in detail as a function of cake formation time, dry cycle time, and specific cake weight in the absence and presence of different types of dewatering aids, a series of vacuum filtration tests was carried out. It is very informative to know the effects of these physical parameters for scale up of using chemicals, optimization of total filtration time, production rate, and, consequently, the final cake moisture. These parameters would also provide general suggestions to meet the desirable filtration efficiencies. The dewatering tests were carried out using a fixed amount of dewatering aids (3lb/ton) and flocculants (25 g/ton) after the optimum dosage was determined. The tests were conducted at a fixed setup vacuum pressure and pre-measured amount of slurry was added to the Buchner funnel for dewatering tests. The dry cycle times were changed randomly, varying from 14 to 120 seconds. The cake weights were changed by increasing the slurry volume from 50 ml to 300 ml. The cake formation time, dry cycle time, cake weights, amount of filtrate, and solid contents for 62
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each test were recorded for production rate calculations. The filter cake production rates were investigated in the absence and presence of dewatering aids and flocculants. Figure 2.6 is a plot of the final cake moisture percent as a function of pounds of dry solids per hour per square foot, or the production rate. The filtration kinetics without the surfactants and flocculant addition were observed to be very slow, and the residual cake moisture of the cake was found to be in the range of 31-36% at about 60-100 lb/hr/ft2 throughput, which corresponds to approximately 5-20 mm cake thickness. The filtration time used for the calculations was the sum of cake formation time and dry cycle time. In the absence of dewatering aids, a production rate greater than 100lb/hr/ft2 was found to be impractical, as achieving a dry cake was no longer possible. There was also segregation of particles in the filter 40 35 30 25 20 15 10 0 50 100 150 200 Figure 2.6 Normalized production rate (lb/hr/ft2) versus cake moisture cake and a considerable amount of solid loss – up to 10% - in the filtrate. As expected, the cake 63 )%( erutsioM none Reagent RU (3lb/t) Reagent RV (3lb/t) Filter Production Rate (lb/hr/ft2)
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moisture increased proportionally with increased production rate; however, the results showed that using dewatering aids lead to very significant reductions in the final cake moistures and increase in the filtration rate by several times. The addition of reagents outperformed baseline to a great extent because it gave the same or lower cake moisture at a higher production rate with almost 97% to 99% solid recovery. Also given in the Figure 2.6, RU and RV produced very similar results. The results obtained with the plants flotation product showed that moisture values as low as 25-30% at improved throughputs – as high as 100-150 lb/hr/ft2 – could be achieved. When the production rate was further increased at the expense of final cake moisture, it became possible to increase the throughput almost 2.5 times (compared to baseline) in the presence of dewatering aids. The test work demonstrated that the use of dewatering aids provided an outstanding dewatering performance on Mingo Logan’s flotation clean coal product and produced significantly lower final cake moisture values, as well as a higher rate of dewatering, and improved the filtration efficiency. If the other operating parameters are kept constant, the effectiveness in productivity of filtration is related to the time required to complete a full solid-liquid separation cycle, consisting of cake formation time and dry cycle time. The correlation between the cake moisture and total filtration time, normalized with cake weight, is shown in Figure 2.7. Test results showed that when the dewatering aids and flocculant were used in a combined manner, the time consumed for filtration of a given amount of material was reduced, which, in turn, increased the production rate by several factors. There was also significant moisture reduction in the presence of dewatering aids; however, it appears that even when the filtration time was increased in the absence of dewatering aids, the reduction in final cake moisture content was very small. The 64
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40 35 30 25 20 15 10 0 0.005 0.01 0.015 0.02 Figure 2.7 Cake moisture versus normalized drying cycle time results suggest that there is an increase of 100% in solids throughput at a fixed moisture value or 5-10% moisture reduction at approximately the same solid throughput. Figure 2.8 shows the effect of chemicals on cake formation time and, eventually, the filtration kinetics. A strong correlation was observed between cake formation time and the throughput of the filter. In the presence of RU and RV, even at higher specific cake weights, the formation times were much shorter than what was seen in the baseline tests. Approximately 100- 140 seconds were required to produce 3.5-4.5 lb/ft2 of coal in baseline tests; however, for the same coal production, using dewatering aids, approximately 30-60 seconds was needed. Above 5 lb/ft2, obtaining a baseline value was impossible because the filter time was impractically prolonged, while 6-7lb/ft2 of coal could be produced when using dewatering aids. The test data indicated that cake formation time was a significant parameter in throughput and residual cake 65 )%( erutsioM none RV 3lb/t + 25 g/t F RU 3lb/t + 25 g/t F Time (hr/lbft2)
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moisture; however, formation time can be altered by using dewatering aids. In addition, in daily practice, decreased cake formation time allows a longer dry cycle time to complete the full filtration operation, increasing the throughput of the filter at lower final cake moisture. 19 17 15 13 11 9 7 5 3 1 0 50 100 150 200 250 Figure 2.8 Cake moisture versus cake formation time After completing the tests using the fine clean coal sample from Mingo Logan, a second set of tests were performed using a fine cyclone overflow sample that had been subjected to froth flotation to minimize the adverse effects of high ash content. The tests were conducted by floating the cyclone overflow sample using diesel (0.66 lb/t) as collector and MIBC (0.33 lb/ton) as frother. Both conventional laboratory-scale flotation and bench-scale column flotation equipment were used to produce ash-free clean coal. Both products were tested in the absence and presence of dewatering aids. 66 2tf/bl thgieW eKaC none RV 3lb/t + 25 g/t F RU 3lb/t + 25 g/t F Cake Formation Time (sec)
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The first series of clean coal samples were produced using lab scale Denver cell. The solid concentration of the product was about 15% by weight, while maintaining approximately 44% of minus 325 mesh particle size. The test results on this sample showed that the control cake moisture was 25.31%, and with RW addition at about 3 lb/ton, the final cake moisture was reduced approximately to 19.5% at 7-10 mm cake thickness. Another set of flotation tests was run on the plant’s flotation product to discard ash-forming minerals, and the product of the flotation tests was subjected to the same type of dewatering tests. The results indicated that the floated cyclone overflow and re-floated samples, using the laboratory-scale Denver flotation machine, gave considerably better results compared to the plant’s as-is flotation product sample. This may be the result of discarding ash-forming minerals and removing ultra-fine particles more efficiently from the coal slurry compared to plant operation. Using a laboratory scale column flotation unit produced another series of clean coal samples. In this set of tests, the flotation feed/cyclone overflow sample was floated using 0.66 lb/ton diesel as collector and 0.22 lb/ton MIBC as frother. The solid concentration of the column flotation product was about 10% by weight, and approximately 39% of particles were minus 325 mesh size. The dewatering tests were conducted using a 2.5inch-diameter Buchner funnel at 20 inch Hg set-up vacuum pressure with 2 minutes drying cycle time and about 11 mm cake thickness. RU and RV were used as dewatering aids with several of dosages ranging from 0.5-3 lb/ton. Vacuum filtration results on both column and Denver unit clean coal products showed that RV alone was capable of both reducing the moisture and cake formation time significantly; therefore, flocculant addition was unnecessary. The cake formation time for control tests was 94 seconds, whereas it was approximately 10 seconds in the presence of the dewatering aid, RV. The presence of dewatering aids also made it possible to reduce the final cake moisture content 67
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of the cake by about 35%. The dewatering test results from the column flotation’s clean coal product are represented in Table 2.7. The final cake moisture for control tests was approximately 22.80%. With RV addition, the moisture was reduced to 14.91%, and with RU addition, the cake moisture was lowered to 14.55%, giving approximately 36% overall moisture reduction. When the dry cycle time was lowered to one minute, the baseline was 26.9%, and with about 1 lb/ton RU and RV addition, the moisture was lowered down to 20.44% and 17.95%, respectively. The influence of cake thickness on final cake moisture was also investigated. To study the effect of dewatering aids on a thicker filter cake, the thickness was increased to approximately 20 mm by increasing the slurry volume that was added to Buchner funnel. As expected, thicker cake resulted in increased baseline moisture and cake formation time. The addition of RU and RV at 3 lb/ton lowered the cake moisture to 17.81% and 15.08%, respectively, from the baseline moisture 24.8% with 2 minutes of dry cycle time. These results correspond to 22% and 33% total moisture reduction. The test results indicated that even with thick cake, dewatering aids showed improvements with final cake moisture. Another set of tests was performed to investigate the effect of flocculant on the dewatering of the laboratory column flotation product (Table 2.8). The same procedure was applied, and the same types of collector, frother, and dosages were used to produce clean coal. Table 2.7 Effect of reagent addition on Mingo Logan flotation feed sample (cleaned using bench-scale column). Reagent Dosage Moisture (%) (lb/ton) RV RU 0 22.80 22.80 0.5 16.51 19.20 1 16.99 17.02 3 14.91 14.55 68
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For this series of dewatering tests, the moisture results for the baseline tests were considerably higher than what was obtained previously. This might be attributed to the excessive amount of fine material associated with this fine fraction. The baseline values for the tests were around 27.30% at approximately 10 mm cake thickness. The addition of flocculant alone at about 25 g/ton was capable of reducing the final cake moisture to 20% and decreasing the cake formation time from 120 seconds to 25 seconds at about 7-9 mm cake thickness and 20 inch Hg vacuum pressure. For lower vacuum pressure, about 15 inch Hg, flocculant additions were capable of reducing the moisture to 23% from 28.1%, and significant improvement in dewatering kinetics was present, as well. The cake formation time was lowered significantly to 26 seconds from 310 seconds. The final cake moisture was also lowered down to 15.52% and 17.02% at addition of 5 lb/ton RU and RV, respectively, in conjunction with flocculant addition. These results show that, in terms of producing a cleaner product, column floatation is superior to the Denver test. The results illustrate how dewatering aids can lower the final cake moisture significantly. g) Laboratory Test Results (Series B – Mixture of 75% Fine and 25% Coarse) A limited number of dewatering tests were conducted using a mixture of 75% fine coal and 25% coarse coal as a function of various dosages of RW, RU and RV. The solid content of the combination of spiral/flotation product slurry was around 27% by weight and it was subjected to dewatering tests using novel dewatering aids at various dosages. The test results showed that the final cake moisture was about 16% to 17% when dewatering aids were added at about 1lb/ton dosage. The moisture content for the control test was approximately 20% at about 8-11 mm cake thickness. Tests were also performed in the presence of flocculant alone and in conjunction with dewatering aids; however, increases in the dewatering kinetics were close to 69
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Table 2.8 Effect of flocculant and dewatering aid addition on Mingo Logan floation feed sample (cleaned using bench-scale column) Reagent Flocculant Moisture (%) (lb/ton) (lb/ton) RV RU 0 0 27.30 27.30 0 25 19.99 19.99 0.5 25 18.78 18.55 1 25 19.66 17.41 3 25 19.99 16.55 5 25 17.02 15.52 those obtained with reagents. Even though the preliminary dewatering test results were promising, due to the Plant’s request dewatering tests were focused more on flotation or flotation/spiral mixture samples. Thus, no further tests were done. h) Laboratory Test Results (Series C – 50% Mixture of Fine and Coarse Coal) The fine and ultra-fine size fraction of a stream to be dewatered is very influential on dewatering, which affects the filtration performance. In the dewatering of such particles, lower moisture percentages are always desirable; however, mechanically, there is a limit to the level of moisture achievable, regardless of operating parameters, such as the length of the filtration time or the applied pressure. In filtration, most of the water is held between and on the surfaces of the particles. Finer particles will create a larger overall surface area and smaller inter-particle openings, which, in turn, keep more water than coarser size distributions do. As the capillary filtration model suggests, a filter cake consists of numerous capillaries with a range of diameters. When the capillary radii are increased, the filtration rate should also increase.[5-8] It can be achieved either by de-sliming or coarse particle addition into the stream or, in this case, into the slurry. As mentioned earlier, when the coal slurry was partially or fully deslimed the drainage of the filter cake was much more efficient, thus lowering the final cake moisture and increasing the 70
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kinetics. Blending coarse particles with fine particles will also increase the capillary radii and improve the filtration performance. In some coal preparation plants, this is already applied to increase the dewatering efficiency as an alternative to other means. In fact, currently, Mingo Logan Coal Preparation Plant has been blending spiral clean coal (18 X 100 mesh) with the finer flotation clean product (smaller than 100 mesh) at about 1:1 ratio before filtration in dewatering centrifuges. The preliminary dewatering test results using RW, RU and RV on one-to-one spiral/flotation blend product showed that significant cake moisture reduction can be obtained using novel dewatering aids by about 20.5-28%, while also increasing the rate of dewatering so much that the formation time could be reduced by as much as 50%. A set of three preliminary tests was conducted to investigate the effectiveness of the dewatering aids (Table 2.9). The dosages used were 1, 3 and 5 lb/ton. The baseline tests produced an average of 19% final cake moisture at about 8mm cake thickness. Even at low dosage, 1lb/ton, when RW, RU and RV was used, the cake moisture was decreased to 15.6%, 14.4%, and 14.8%, respectively, and the filtration kinetics were increased by 30-50 %. Of the reagents and dosages being tested, RU was the most effective for the cake moisture reduction. In this case, the addition of 5 lb/ton RU reduced the cake moisture from 19.00% to 13.7% which corresponds to 20-30 % overall moisture reduction. 71
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Table 2.9 Effect of reagent addition on dewatering of Mingo Logan mixture sample (50% flotation product and 50% spiral product) Reagent Moisture Content (%) Dosage Reagent Reagent Reagent (lb/ton) RW RU RV 0 19.0 19.0 19.0 1 15.6 14.4 14.8 3 15.7 13.8 14.9 5 15.1 13.7 14.3 Similar dewatering tests were conducted to evaluate the filtration performance with different types of dewatering aids as a function of filtration time and specific cake weight. Filtration tests were done at the same vacuum level; however, the dry cycle times were varied from 15 to 100 seconds. RU and RV were prepared at 2:1 active solvent ratio, and the dosage amount was fixed at 3 lb/ton. The coal slurry was conditioned with the dewatering aids for 2 minutes. Then, flocculant was added at a 25g/ton dosage and conditioned at a very low intensity for 15-20 seconds. Tests were conducted on a pre-measured amount of slurry to differentiate the specific cake weight. This, in turn, varied the cake thickness from 5 to 20 mm. The cake formation time, dry cycle time, and cake weights were recorded for each test. The filter production rate was plotted as pounds of dry solids per hour per square foot, and the filtration time used for filtration rate calculations was the sum of cake formation time and dry cycle time. Figure 2.9 shows the relationship between production rate and cake moisture for the spiral/flotation mixture sample. 72
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40 35 30 25 20 15 10 0 100 200 300 400 500 600 700 800 Figure 2.9 Cake moisture versus normalized filter cake production rate The baseline tests were conducted without reagents and produced a cake of 29-34% moisture at about 5-20 mm thickness, yielding a production rate in the range of 60-120lb/hr/ft2. Throughput greater than 120 lb/hr/ft2 was found to be impossible because the cake formation time was being prolonged to impractical limits. The additions of RV and RU, along with 25 g/ton flocculant, surpassed the baseline throughput to a great extent. The usage of RV reduced the final cake moisture to 14-18%, and the usage of RU reduced the final cake moisture to 18- 21%. The production rates were also increased by multiples of 1.5 to 2.5, corresponding to 150- 190 lb/hr/ft2. The results also showed that the throughput could be increased at the expense of cake moisture. When the production rate was increased to the 200-400 lb/hr/ft2 range, the cake moisture increased to 20-25%; however, final cake moistures were still 5-15% lower compared 73 )%( erutsioM none rv 3lb/t +f 25g/t ru 3 lb/t +f 25gr/t FilterProduction Rate (lb/hr/ft2)
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to baseline. Further increases in production rate were also achieved i.e., the 550-650 lb/hr/ft2 range was achieved at a 25-30% moisture range. It was obvious that the addition of reagent outperformed baseline, and it was possible to increase the production rate with significantly lower final cake moisture values. The results also showed that the use of RV represented better performance than RU because it gave higher filtration rates at the same, or lower, final cake moisture values. Further data evaluation was carried out on the effect of filtration time on final cake moisture. Figure 2.10 shows the correlation between the cake moisture and total filtration time (normalized with cake weight) in the absence and presence of dewatering aids. In the baseline tests the total filtration time varied between 130 and 360 seconds. On the other hand, the total filtration times in the presence of RU and RV were 65 to 120 seconds and 50 to 118 seconds, respectively. As seen, the dewatering aids that were tested decreased the filtration time, which, in turn, produced higher production rates. It is also noteworthy that these outstanding times were achieved while maintaining very low moisture levels. The test data also indicated that cake formation time is an important factor in determining dry cycle time and, thus, cake moisture and throughput, as well. Figure 2.11 shows the effects of dewatering aids on cake formation time and, eventually, the filtration kinetics. The formation times were found to be much shorter in the presence of RU and RV. When used with a flocculant, even at higher specific cake weights, the formation times were shorter than those that were recorded during the baseline tests. 74
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As seen in Figure 2.11, only 10-15 seconds were required to produce 4.5 lb/ft2 of coal when dewatering aids were used; however, in baseline tests, approximately 100-120 seconds were needed for the same coal production. When the cake weight was increased to 7 lb/ft2, the cake formation time was 20 seconds using dewatering aids, where it was 340 seconds for baseline test. Cake weights above 5 lb/ft2 were found to be impractical for dewatering in the absence of dewatering aids. Conversely, it was still possible to produce a cake weight of 11 lb/ft2 while maintaining a short cake formation time. The results showed that the use of dewatering aids decreased the cake formation time by several multiples. The usage of dewatering aids also substantially improved the throughput. This is a strong indication that in the presence of dewatering aids, more material can be treated. 40 35 30 25 20 15 10 0 0.005 0.01 0.015 0.02 Figure 2.10 Cake moisture versus normalized filtration time 75 )%( erutsioM none RV 3lb/t + 25 g/t F RU 3lb/t + 25 g/t F Time (hr/lbft2)
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19 17 15 13 11 9 7 5 3 1 0 50 100 150 200 250 300 350 400 Figure 2.11 Cake moisture versus total cake formation time i) Pilot-Scale Test Results (Series A – Fine Coal Only) The pilot-scale dewatering tests were conducted using two feeds intercepted from the plant’s main stream (i.e., flotation concentrate and blended products). The first set of tests focused on dewatering of the flotation product, which is very difficult to dewater because of the amount of fine size particles and high ash content. As mentioned earlier, nearly 43% particles of this product was passing 325 mesh (-44 µm) and contained 81% ash. The tests were conducted over a range of filter feed rate that typically varied at 2, 3, 4 and 7 gal/min of coal slurry. The preliminary analysis showed that of the feed rates, 4-7 gal/min were at optimal ranges for the filtration tests and also adequate to produce 0.33 to 1.0 inch cake thicknesses. The pilot-scale 76 2tf/bl thgieW eKaC none RV 3lb/t + 25 g/t F RU 3lb/t + 25 g/t F Cake Formation Time (sec)
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Table 2.10 Effect of RV on Mingo Logan flotation product sample Cake Moisture (%) Filter Cake 0.5 0.5 1.0 1.0 Time Thickness 25 g/t Control lb/ton lb/ton lb/ton lb/ton (sec) (mm) Floc RV RV* RV RV* 184 25 31.49 34.61 27.11 26.13 - - 120 15 31.59 34.13 25.92 25.95 31.73 23.59 85 10 31.18 - 28.49 - 28.12 24.45 65 8 31.63 36.2 - - 28.9 26.67 *With Roller test procedure was same as the mixture sample tests except that the flotation product was intercepted from the distribution box pipeline. The first set of dewatering tests was conducted with a pilot-scale horizontal belt filter (HBF) at the feed rate of 4gal/min. Baseline tests provided a filter cake with 31~32% moisture. With 25 g/ton flocculant addition to the feed, even though a slight decrease in cake formation time was observed, the cake moisture increased to 34~36%. On the other hand, at 0.5 lb/ton RV addition, the cake moisture was reduced down to approximately 26~28% (see Table 2.10). The results also showed that, in this set of tests, the belt speed had a slight effect on the dewatering when flocculant and reagent were added; however, it did not appear to influence the cake moisture for the control tests (it only caused changes in cake thickness and formation time). During the tests, it was observed that even though the filter feed rate was kept constant; using RV increased the cake thicknesses. This can be attributed to increased porosity, which in turn creates more permeable cake. This phenomenon also caused a cake-cracking problem. As a result, the vacuum pumps also lost pressure. To overcome this problem, a roller was attached on the belt to press down the cake, presumably to prevent the cracking. The test results clearly showed that the cake moisture was further reduced to 23~26% when a roller was applied to the 77
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Table 2.11 Effect of RV on Mingo Logan flotation product sample (with 5 g/t of flocculant) Filter Cake Final Cake Moisture (%) Time Thickness 1 lb/ton 1 lb/ton 3 lb/ton 3 lb/ton (sec) (mm) Control RV RV* RV RV* 184 25 31.49 28.65 26.32 25.69 26.93 120 15 31.59 29.05 25.61 29.03 25.19 85 10 31.18 28.63 28.01 29.13 27.12 65 8 31.63 24.85 26.81 27.37 28.25 *With Roller dry cake to help seal the pores inside the cake. Overall, the use of roller resulted in additional moisture reductions from 3-4% to 15% at 0.5 lb/ton and 1 lb/ton of RV addition, respectively. Table 2.11 shows another series of tests were conducted to investigate the effect of the flocculant addition. The effect of roller was also tested in the presence of dewatering aid. The cake moisture was in the range of 24 to 29% with combined use of 5 g/t of flocculant and 1 lb/ton of RV. Yet again, increased cake porosity and the cracking was a problem; however, when the roller was applied in some cases moisture was lowered. j) Pilot-Scale Test Results (Series B – 50% Mixture of Fine and Coarse Coal) The next set of tests was conducting using an equal mixture of fine and coarse coal. The fine coal was obtained from the froth concentrate, while the coarse coal was intercepted from the screen-bowl feed containing approximately 28% solids by weight and 12% ash on dry basis. The tests were conducted over a range of filter feed rate that typically varied from 2, 3, 4 to 7 gal/min of coal slurry. Unlike the flotation product, it was found out that the 3 gal/min feed rate was optimal for the blend filtration tests, which would be sufficient to produce 1/3 to 1 inch cake thicknesses. Table 2.12 shows a summary of the pilot-scale test data obtained at the Mingo Logan plant spiral/flotation product mixture sample using RU at 3lb/ton and flocculant at 25g/t 78
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dosage at the feed rate of 3gal/min. Each series of tests were conducted as a function of total filtration time. This reagent reduced the cake moisture from about 30% down to 21% at 3 lb/ton dosage. Meanwhile, the cake formation time decreased by 20~50% with the addition of RU as dewatering aids. When used alone, it could produce a low-moisture cake (approximately 21~22% moisture), and the cake formation time was significantly reduced down to 14~75 seconds from approximately 85 seconds. The flocculant alone was not capable of reducing the moisture content to the level that RU achieved; although, they could reduce the formation time more significantly. The use of flocculants resulted in loss of vacuum pressure in the pump, an indication of increased cake porosity, but did not help to remove the surface water that was entrapped inside the flocs. However, the combined use of flocculants and RU could achieve a very short cake formation time. When used together with 25 g/t flocculants, RU reduced the cake formation time further to 7~24 seconds, while the final cake moisture remained at almost the same level. In this case, the cake formation time was reduced by 50~75% over the belt speed range under test, and the moisture was reduced from 30-34% down to 21~24%. Test work performed using RU showed that a filter cake with good handling characteristics could also be produced. Table 2.12 Effect of RU and flocculant on Mingo Logan flotation product sample Final Cake Moisture (%) Filter Cake 25 g/t Floc Time Thickness 3 lb/ton Control 25 g/t Floc & 3 lb/ton (sec) (mm) RU RU 184 25 34.38 26.6 25.05 24.96 120 15 29.62 26.9 21.8 24.66 85 10 30.78 29.1 21.3 18.7 65 8 29.99 28.81 21.5 21.7 Vacuum (Inch Hg) 16-14 11-5 15-11 7-5 79
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In comparison, RV was tested and the results given in Table 2.13 showed that RV was less effective in reducing moisture and increasing the kinetics of dewatering. However, the difference between RU and RV was narrowed when each of these two reagents were used together with low dosage (25 g/t) of flocculants. It was also noticed that in the presence of dewatering aids, change in belt speed made a slight difference in the moisture reduction, especially while operated at lower speeds. When the filter feed rate was fixed, the short retention time of the materials over the vacuum zone was compensated by the thin cake thickness at higher belt speed, and thick cake at lower belt speed. Table 2.13 Effect of RV and flocculant on Mingo Logan flotation product sample Filter Cake Final Cake Moisture (%) Time Thickness 25 g/t 3 lb/ton 25 g/t Floc & Control (sec) (mm) Floc RV 3 lb/ton RV 184 25 34.38 26.6 28.11 24.56 120 15 29.62 26.9 28.9 24.74 85 10 30.78 29.1 29.78 22.63 65 8 29.99 28.81 26.34 21.4 Vacuum (Inch Hg) 16-14 11-5 16-15 8-4 80
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2.3.3. Coal Clean Site a) Site Descripton The Coal Clean Panther Preparation Plant is located in Dry Branch, approximately 15 miles south of Charleston, West Virginia. The Panther Preparation Plant currently processes 63 mm x 0 raw coal for ultimate use in the metallurgical and steam markets. The minus 325 mesh size fraction material reports to the discard stream without any type of processing method. However, if this size fraction is recovered and dewatered, loss of valuable source could be turned into profit. For this reason the plant management looked for alternatives for the recovery of the minus 325 mesh coal that is presently discarded to refuse. To evaluate the feasibility of the recovery and dewatering of this size fraction, extensive pilot scale flotation and dewatering tests were conducted. A number of tests with pilot scale centrifuge unit were conducted for comparison reasons. b) Reagents In this investigation, majority of the pilot scale dewatering tests were performed with varying amounts of three types of dewatering aids, namely RW, RU and RA. Diesel was used as solvent at one to two (1:2) ratio (dewatering aid: solvent). Each of the reagents were tested over a range of dosages typically ranging from 0 to 20 pounds per ton for the ratios of the ultra-fine and fine products in the feed to the Filter Module and the Centrifuge Module. c) Coal Samples For this particular test site, pilot-scale dewatering tests were conducted on feeds comprised of different mixtures of coarse and fine coal feeds. These included (i) 100 mesh x 0 feed stream from the overflow of the primary classifying cyclones, (ii) 325 mesh x 0 feed raw stream, and (iii) blends of 100 mesh x 325 and minus 325 mesh product from the flotation column. The 81
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Column Conditioner Module Module Pilot-Scale Test Circuit Plant Feed Filter Module Centrifuge Module A Dewatered Product Dewatered To Product Conditioner Figure 2.12 Configuration of the mobile unit test modules evaluated at the Panther Preparation Plant site blends were established at ratios of 1:1 and 3:1 of minus 325 mesh material to the 100 x 325 mesh product. d) Pilot-Scale Procedures The column flotation, conditioner, disc filter, and centrifuge modules were set up at the Coal Clean Plant to accommodate the pilot-scale testing program. A total of 115 tests were run over a one month period to establish optimum conditions for the proposed plant upgrades that were under consideration to accommodate the proposed POC-scale test circuit. The arrangement of the modules for the tests is presented in Figure 2.12. For the majority of the test work, the plant supplied a relatively consistent feed stream of minus 325 mesh material to the Column Module from the overflow of the secondary classifying cyclones. The secondary classifying cyclones were fed from the overflow of the primary classifying cyclones which were separating a 82
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16 mesh x 0 slurry stream at a nominal size of 100 mesh. The underflow from the secondary classifying cyclones reported to a bank of conventional flotation cells and the overflow was discarded to the refuse thickener. A series of tests was also conducted on the 100 mesh x 0 feed stream from the overflow of the primary classifying cyclones. The minus 325 mesh raw feed was cleaned in the Column Module, with the clean coal routed to the Conditioner Module. The conditioned slurry was then dewatered in either the Filter Module or the Centrifuge Module. The Panther Preparation Plant offered a unique opportunity to conduct a series of tests with various blends of 100 mesh x 325 mesh conventional flotation product added to the minus 325 mesh product from the Column Module. The projected blends were established at ratios of 1:1 and 3:1 of minus 325 mesh material to the 100 x 325 mesh product. Maintaining the blend at the various ratios proved somewhat difficult due to the changing flows for the products, but most of the tests were conducted within 5% of the projected blend. Although the Filter Module and the Centrifuge Module were not operated at the same time, the tests included almost the same sweep of reagent tests for both modules. e) Pilot-Scale Test Results Table 2.14 presents the results for dewatering tests with various reagents while dewatering the minus 325 mesh product in the Filter Module. The sample was first floated using a mixture of Nalco 01DU113 (0.25 unit) + 01DU145 (1.0 unit) as collector and Nalco-948 as frother (9 units) in a flotation column. The solids content in the filter feed ranged from 4-5% by weight. For dewatering tests, RW, RU and RA were used as dewatering aids at various dosages. The vacuum pressure was approximately 20.5 to 23.0 inches Hg; and the cake thickness was around 6-7 mm. The results indicate that the baseline moisture content of the filter cake (with no reagent) was very consistent and it was approximately 29.0%. This value was reduced to 27.5%, 83
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TTaabbllee 22..1154 . CCooaall CClleeaann ccooaall ((5m0i%nu ms i3n2u5s m32e5s hm) edsehw aantedr 5ed0 %us 1in0g0 xR3W25, mRUes,h a) ndde wRaAte dreisdp uesrsinegd iRnW N aalncdo R01UD dWis1p1er0s ed in Nalco O1DW110 . ReRaegaegnetn t MoistMuroei sCtounret eCnot n(%ten) t (%) DoDsoasgaeg e RW RU RA RW RU (lb(l/bt)/ t) (1:4 Ratio) (1:2 Ratio) (1:2 Ratio) (1:2 Ratio) (1:2 Ratio) 0.00 29.10 0.00 19.98 3.08 27.01 1.98 19.82 6.08 26.04 4.47 17.76 9.75 24.66 0.00 19.98 0.00 29.28 2.80 18.26 2.80 27.28 5.40 17.93 5.48 24.71 7.95 17.65 9.43 23.42 0.00 29.05 1.62 28.47 2.19 27.49 7.50 27.49 24.7% and 23.4% with RA, RW, and RU, respectively. As such, RU provided the best overall performance for dewatering of the minus 325 mesh product. Considering the amount of the minus 325 size fraction in this feed, RU was capable of reducing the final cake moisture by 20%. Table 2.15 presents the results for dewatering tests using the Filter Module for a blend of the minus 325 mesh product with the 100 x 325 mesh product from the conventional flotation cells at a ratio of 1:1. For flotation tests, same procedure and collector and frother dosages were employed. As shown, the addition of the coarser material had a dramatic effect on the moisture content of the product. With no reagent added, the addition of coarser material reduced the baseline moisture from 29% (Table 77) to 20% (Table 78). As the reagent dosage was increased, the 20% moisture content was further reduced to 17.8% with RW and to 17.6% with RU. Table 2.16 presents the results for the dewatering tests using the Filter Module for a blend of the minus 325 mesh product with the 100 mesh x 325 mesh product from the conventional flotation cells at a ratio of 3:1. The solids content in the filter feed ranged from 5% to 6%. As 84
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Table 2.15. Coal Clean coal (50% minus 325 mesh and 50% 100x325 mesh) dewatered using RW and RU dispersed in Nalco O1DW110 . Reagent Moisture Content (%) Dosage RW RU (lb/t) (1:2 Ratio) (1:2 Ratio) 0.00 19.98 1.98 19.82 4.47 17.76 0.00 19.98 2.80 18.26 5.40 17.93 7.95 17.65 seen, when the amount of the minus 325 size material was increased, the baseline moisture value was also increased. The results, as expected, lie between those obtained in the two test series noted above. Of the dewatering aids, RU was the most effective and capable of reducing the cake moisture from 24.78% to 20.77 % which correspond to 17 % overall moisture reduction. Table 2.17 presents the results for dewatering tests for a minus 325 mesh product in the Filter Module with the filter disc speeds ranging from 4 to 1.5 min/rev. The sample was floated using a mixture of 01DU110 as collector and Nalco 01DU009 as frother in a flotation column. The solids content in the filter feed ranged from 9-10% by weight. The product rate increased from 43.78 to 59.18 lb/h with only a slight increase in the moisture content from 27.5 to 28.5% when using RU at approximately 2.0 lb/ton. 85
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Table 2.16 presents the results for pilot scale dewatering tests using RW for a blend of the minus 325 mesh product with the 100 x 325 mesh product at a ratio of 1:1 using the Centrifuge Module. The sample was floated using mixture of 01DU110 as collector and Nalco 01DU009 as frother in a flotation column. The solids content in the centrifuge feed ranged from 9-10% by weight. The 150 mm diameter centrifuge operated at approximately 480 rpm with a differential of 95:1 for the conveyor. The moisture of the product increased from 33.2 to 34.5% as the solids yield increased from 87.2 to 93.4% with the increase in reagent dosage. The higher Table 2.16 Coal Clean coal (75% minus 325 mesh and 25% 100x325 mesh) dewatered using RW, RU and RA dispersed in Nalco 01DW110 Reagent Moisture Content (%) Dosage RW RU RA (lb/t) (1:2 Ratio) (1:2 Ratio) (1:2 Ratio) 0.00 24.78 2 23.57 4.36 24.83 7.4 22.49 0.00 24.78 1.85 23.01 3.78 22.55 7.7 20.77 0.00 24.78 2.0 23.00 3.56 23.82 8.47 23.68 Table 2.17 Effect of disc speed on product rate and moisture content for Coal Clean coal (minus 325 mesh) from the filter module Disc Rotation Filter Cake Moisture Speed Production Content (min/rev) (lb/hr dry) (%) 4.0 43.78 27.49 3.0 44.86 27.76 2.0 52.94 28.63 1.5 59.16 28.47 86
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Table 2.18 Effect of Reagent 01DW133 on Coal Clean coal (50% minus 325 mesh and 50% 100x325 mesh) from the centrifuge module Reagent Nalco 01DW133 in 01DU110 (1:2 Ratio) Dosage Moisture Solids (lb/t) Content (%) Yield (%) 0.00 33.24 87.20 2.31 33.94 89.60 4.51 33.36 90.30 6.16 33.86 86.00 moisture and improved yield appear to be mostly due to an increase in the recovery of the ultra- fine material. Table 2.18 presents the results for dewatering tests using Reagent 01DW133 for a blend of the minus 325 mesh product with the 100 x 325 mesh product at a ratio of 1:1 using the Centrifuge Module. The sample was again floated using a mixture of 01DU110 as collector and Nalco 01DU009 as frother in a flotation column. The solids content in the centrifuge feed ranged from 9-10%. The moisture of the product increased slightly from 33.2 to 33.8% and the solids yield increased from 87.2 to 90.3% with the increase in reagent dosage. Once again, the increases in moisture and yield were attributed to increases in the recovery of ultra-fine material. During the continuous test work conducted at the Panther Preparation Plant site, a series of timed samples were collected periodically from various points around the pilot plant so that complete mass balances could be established for the different unit operations. The samples included representative splits for the column cell (feed, product and tails), filter (feed, product and filtrate), and the screen bowl centrifuge (feed, product, effluent and drain). The series of tests for the minus 325 mesh feed showed that the 300 mm (1 ft) diameter Column Module produced an average of 68.2 lb/hr of concentrate. Depending on the particular operating conditions, the clean coal capacity ranged from a low of 37.4 lb/hr to a high of 127.6 lb/hr. The 87
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2.3.4. Concord Site a) Site Description The Concord Coal plant is located near Birmingham, Alabama. This facility processed 50 mm x 0 coal for the metallurgical and steam markets, with a design plant feed rate of 1,000 tph and typical clean coal yields of 55%-60%. The intermediate/fine coal circuit consists of primary classifying cyclones (PCC), spirals, secondary classifying cyclones (SCC), froth flotation, and screen bowl centrifuges. The overflow from the PCCs is fed to the SCCs; the SCC underflow is the feed stream to flotation (4 banks of five 180-ft3 cells), while the SCC overflow is piped to a refuse thickener. The coal being processed is very soft and fine in size consist and the feed to the flotation cells can be as much as twice that of the design flowsheet rate (design 54 t/hr vs. actual 80-100 t/hr). The feed to the flotation cells is approximately 80% minus 325 mesh (0.045 mm). The flotation and spiral clean-coal products are combined and then dewatered via four 44” x 132” screen bowl centrifuges with a total design feed rate of 2,200 gal/min and 242 t/hr. The primary objectives of the test program were to determine whether (i) a thick and low- moisture filter cake and (ii) a filter cake with good material handling characteristics could be produced from the minus 100 mesh flotation feed stream (primary cyclone overflow) that is currently processed in conventional flotation cells and centrifuges at this plant. To meet these objectives, extensive laboratory and pilot scale flotation and dewatering test program was conducted at Virginia Tech Mineral Processing Facility in Virginia, and at the Concord coal preparation plant in Alabama. The laboratory tests included the performance evaluation of various types and dosages of dewatering aids to collect dewatering data that could be used in 89
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direct support of pilot-scale test work. The data obtained from the laboratory tests were used to provide a technical guidance for the pilot scale test program. b) Reagents The laboratory and pilot scale tests included both the flotation and dewatering tests. For laboratory flotation tests, diesel and MIBC were used as collector and frother, respectively. The floated sample was then subjected to dewatering tests using RW3 and RV. For pilot-scale flotation tests RW, RU, RV and diesel as collectors and Nalco DU009 as frother were used. The same reagents were used as the dewatering aids in filter tests. Each of the reagents was tested over a range of dosages that typically varied from 0 to10 lb/ton of dry coal. As mentioned elsewhere, these dewatering aids are insoluble in water. For all the tests, flotation and dewatering, diesel was used as solvent at one to two (1:2) dewatering aid-to-diesel ratio. c) Coal Samples The coal slurry samples for the flotation and dewatering tests were collected from the minus 100 mesh flotation feed stream (primary cyclone overflow) that was processed. The same coal slurry feed was used for the pilot-scale flotation and dewatering tests. d) Laboratory Procedures The flotation feed sample (minus 100 mesh) from the Concord plant was first floated in a laboratory mechanical flotation cell using 0.66 lb/t of diesel and 0.33 lb/t of MIBC to remove ash-forming minerals. The floated product was then subjected to dewatering tests at about 13.5% solids by weight. In these tests, RV and RW3 (both diluted to 33.3% in solvent) were used as dewatering aids. Immediately prior to each filter test, a known volume of slurry was conditioned for 5 minutes with the reagent in a mechanical shaker and then poured into a 90
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Buchner funnel before applying vacuum of 20 inches Hg. A constant drying cycle time of 2 minutes was used in all tests. The thickness of the filter cake varied from 7 to 9 mm. e) Pilot-Scale Procedures The on-site test work was conducted using the Column, Conditioner, and Filter Modules. In each test, the cyclone overflow from the plant was first upgraded using the Column Module (a 305 mm or 12-inch diameter Microcel column) using diesel and RW, RU and RV as collectors and Nalco DU009 as frother. The plant feed was reasonably consistent for most of the test work and contained 3.5-5.5% solids by weight and 23.3-26.5% ash. The column produced a clean coal product with 7-11% ash and 84-87% combustible recovery, depending on the reagent type and dosage used. The froth product was then dewatered using the Filter Module (i.e., 0.186 m2 (2 ft2) filter area, 10 sector Peterson disc filter). The same reagents listed above, namely RW, RU and RV, were also used as the dewatering aids in the filter tests. Each of the dewatering aids were tested over a range of dosages that typically varied from 0 to 10 lb/ton of dry coal. Timed samples were collected periodically from various points around the test modules to establish typical material balances and reagent addition rates for this particular coal. f) Laboratory Test Results Several series of laboratory dewatering tests were conducted to collect data that could be used as guidance for the pilot scale dewatering tests. Table 2.19 shows the laboratory test results obtained on the Concord Plant flotation feed sample using RV and RW3 as the dewatering aids. A 62.5 mm diameter Buchner funnel was used. The solid content of the flotation feed sample was 6%. It was increased up to 13.5% after flotation. 0.66 lb/t diesel and 0.33 lb/t MIBC was used during flotation. Vacuum setup point was 20 inches Hg. Cake thickness: 7-9 mm. Conditioning time: 5 minutes; drying cycle time: 2 minutes. The volume of the slurry was 100 91
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Table 2.19 Effect of reagent addition on Concord flotation feed (100 mesh x 0) using RV and RW3 Reagent Moisture Content (%) Dosage RV RW3 (lb/t) 0 24.6 24.6 0.5 21.3 23.2 1.5 19.6 21.0 2.5 18.1 19.4 10.0 18.2 18.6 ml. As shown, the moisture content of the filter cake was reduced as the reagent dosage increased. At dosages of 0.5 lb/t and 2.5 lb/t of RV, the moisture contents of the filter cake were reduced from 24.6% down to 21.3% and 18.1%, respectively. Similar results were obtained when RW3 was used as the dewatering aid. These values correspond to a 10-26% moisture reduction in the filter product. g) Pilot-Scale Test Results The first series of dewatering tests were conducted at various levels of vacuum pressures applied. The feed slurry was first floated using diesel collector and Nalco DU009 frother in flotation column. As shown in Table 2.20, there was a strong correlation between the cake moisture and vacuum pressure. The results showed that when the vacuum pressure was increased the cake moisture was decreased from 31.12% down to 24.18%. Table 2.21 provides an overall summary of the pilot-scale test data obtained at the Concord plant. In the first series of tests, RW, RU and RV were evaluated over a wide range of reagent dosages at a constant disc speed of 4 min/rev. The test data show that RW was the most effective of the three dewatering aids (Table 2.21a). This reagent reduced the cake moisture from 25.5% down to 20.2% at the highest reagent dosage of 2.7 lb/t. RU, which was rather less 92
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effective than RW, was not capable of reducing the moisture content to less than 21.5% (Table 2.21b). However, this moisture level was achieved at a very low reagent dosage level of just 0.88 lb/t. In fact, higher dosages of RU did not appear to be as effective in reducing moisture in this particular series of tests. RV was generally the least effective in reducing moisture (Table 2.21c). Table 2.20 Pilot-scale test results obtained on the Concord flotation feed sample (100 mesh x 0) using various vacuum pressures Vacuum Moisture Pressure Content (Inch Hg) (%) 10 31.12 15 26.83 20 24.18 Although less effective in reducing moisture, RV generally provided the best overall cake thicknesses (up to 12 mm) when compared to RW and RU. The thick cakes produced using RV also possessed the best material handling characteristics and were cited by plant personnel as the most suitable for their particular needs. Therefore, several additional tests were conducted using RV to determine whether lower moistures could be achieved by adding the reagent directly to the flotation column feed in place of the diesel collector. As shown in Table 2.22, this strategy significantly improved the moisture reduction and greatly reduced the total reagent requirement. More importantly, the lower moistures were obtained at relatively large cake thicknesses (i.e., 9- 10 mm). In one test run, the cake moisture was reduced from 25.1% down to 20.9% (a moisture reduction of 16.5%) while maintaining a cake thickness of 9 mm. The total reagent dosage 93
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2.3.5. Buchanan Site a) Site Description Consolidation Coal Company’s Buchanan Mine #1 is an underground coal mine located two miles south of Route 460, adjacent to State Route 632, at Mavisdale, Buchanan County, Virginia. Consol Energy Inc., located in Pittsburgh, Pennsylvania, is the parent company of Consolidation Coal Company. The Buchanan preparation plant processes approximately 5 million tons of 37.5 mm x 0 raw coal (2006) from the Pocahontas 3 Seam for use in the metallurgical and steam markets. The objectives of this study were to (i) identify the best possible reagents and combinations thereof for this specific coal and (ii) identify the conditions under which a given dewatering aid can give the best performance. To meet the objectives, laboratory and pilot scale tests were conducted to evaluate the performance of various types and dosages of dewatering aids. b) Reagents The investigation, both laboratory and pilot-scale, was performed with varying amounts of three types of dewatering aids, namely RW, RU, and RV. Since these dewatering aids are insoluble in water, they were dissolved in a solvent. In both laboratory and pilot scale experiments diesel was used as the solvent. The ratio of reagents-to-solvent was optimized in previous studies by varying the individual dosages (0.5 to 3lb/ton), while maintaining the total blend dosage constant. For this test program, the optimum combination for a given dewatering aid and solvent is one to two (1:2) dewatering aid-to-diesel ratio. 96
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c) Coal Samples The test work was conducted on different samples taken from Consolidation Coal Corporation’s Buchanan Preparation Plant in Mavisdale, Virginia. These samples included (i) a flotation feed sample, (ii) a grab sample of current flotation product, and (iii) a slip-stream sample of filter feed (all taken on various dates). d) Laboratory Procedures Prior to experiments sieve analysis was conducted for each sample by wet screening using 600, 300, 150, 75 and 45 micron sieves. Dewatering tests were mostly conducted on filter feed and flotation product samples. The solid concentration of Buchanan’s flotation product was about 25% by weight while maintaining approximately 25-30% of minus 45 micron material. Table 2.24 shows the sieve analysis results on flotation product sample. The flotation product sample was occasionally mixed with a portion of the spiral product at the plant at a ratio of 1:1 to have better dewatering kinetics. Table 2.25 shows the sieve analysis results of spiral/flotation product slurry collected from the plant. For the laboratory-scale batch dewatering tests, the samples were collected in 5-gallon buckets and to be able to receive a representative sample, samples were homogenized by mixer. When the plant flotation feed sample was used in the dewatering tests, the sample was first floated in a laboratory mechanical flotation cell using 0.66 lb/t of kerosene and 0.33 lb/t of MIBC to remove ash-forming minerals. The floated product was then subjected to the dewatering tests at about 20% solids by weight. Immediately prior to each filter test, a known volume of slurry (whether flotation product or mixture sample) was conditioned with the reagent in a mechanical shaker and then poured into a Buchner funnel before applying vacuum. The dewatering aids RW and RU, diluted to 33.3% in solvent, were used in these tests. The 97
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Table 2.24 Screen analysis of the Buchanan flotation product used for dewatering tests Particle Size Pipe 1 Pipe 2 Pipe 3 (Mesh) Weight (%) Weight (%) Weight (%) Plus 28 3.6 3.4 7.7 28x45 19.0 15.8 27.3 45x100 23.0 18.0 24.1 100x200 14.9 13.2 13.2 200x325 8.1 25.3 6.9 Minus 325 31.4 24.3 20.7 following conditions were kept constant during the tests: 20 inches Hg of vacuum, 2 minutes of drying cycle time, 10-15 mm of cake thickness, 100 ml volume of feed slurry and 5 minutes of conditioning time. e) Pilot-Scale Procedures In the pilot-scale dewatering tests, the Conditioner Module and Filter Module were required since the feed slurry for the tests was supplied directly from the Buchanan Preparation Plant. The pilot-scale disc filter tests were conducted on flotation product samples. Table 2.25 Screen analysis of the Buchanan filter feed used for dewatering tests Particle Size Pipe 1 Pipe 2 Pipe 3 (Mesh) Weight (%) Weight (%) Weight (%) Plus 28 6.0 6.3 5.5 28x45 23.4 23.3 21.8 45x100 21.7 22.5 19.9 100x200 14.7 14.8 14.6 200x325 8.2 6.9 8.9 Minus 325 26.0 26.2 29.3 98
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Table 2.26. Effect of reagent addition on dewatering of Buchanan’s filter feed Reagent Moisture Content (%) Dosage RW RU (lb/t) 0 18.1 18.1 1 17.58 17.5 3 15.2 16.78 5 14.9 16.58 f) Laboratory Test Results Table 2.27 gives the laboratory test results obtained on the Buchanan plant flotation product using RU and RW as the dewatering aids at 20 inches Hg vacuum. As shown, the moisture content in the filter cake was reduced with increasing reagent addition. At RU additions of 1 and 5 lb/t, the moisture contents of the cake were reduced from 17.6% to 16.1% and 14.4%, respectively. Similar results were obtained when RW was used as dewatering aid. These values corresponded to a 15-20% moisture reduction in the filter product. Similar dewatering tests were conducted on the filter feed sample (which contains approximately 10 g/t of Nalco 9806 polymer flocculant as the dewatering aid) using RW and RU as dewatering aids. Results for the filter feed sample are summarized in Table 2. The results show that the moisture content of the filter product again decreases with increasing RW and RU additions from 1 to 5 lb/ton. In this case, the addition of 5 lb/ton of RW reduced the cake moisture from 18.1 to 14.9%, giving a percentage moisture reduction of about 20%. The Table 2.27. Effect of reagent addition on dewatering Buchanan’s flotation product Reagent Moisture Content (%) Dosage RW RU (lb/t) 0 17.6 17.6 1 16.2 16.1 3 16.2 14.9 5 15.0 14.4 99
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moisture reduction is quite similar to that obtained for the flotation product, except that the moisture content of the filter cake product obtained using RU was almost 2 percentage units lower, i.e., 14.4% vs. 16.6% moisture in the filter cake (see Table 2.27 and Table 2.26). The reasons for the relatively poorer behavior of RU may be related to the presence of flocculant in this particular sample. Apparently, the polymer flocculant has an adverse effect on the performance of RU during dewatering. Those poor results are also due to the Ca2+ ions present in Buchanan plant water. Two series of laboratory filtration tests were conducted to determine the effects of agitation intensity on the dewatering performance of the Buchanan filter feed. The first series of tests were conducted using a laboratory shaker to condition the feed samples. The shaker was a low-energy conditioner that uses reciprocating motion (similar to wrist-action shaking) to gently mix slurry contained in a 100-ml glass conditioning flask. A second series of tests were conducted using a 100-ml Plexiglas cell equipped with a three-blade propeller-type mixer at 1000 rpm. The rotary mixer provided an intense agitation that is necessary for high-energy conditioning. The feed slurry was conditioned for 5 minutes in both series of tests. As shown in Table 2.28, the moisture reduction was substantially improved when high- energy conditioning was used. For example, the use of 5 lb/ton of dewatering aid reduced the filter cake moisture from a baseline value of 18.2% (no reagent added) down to 14.6% when using low- energy agitation. The cake moisture was further reduced to 11.7% moisture when high-energy agitation was used at the same reagent dosage of 5 lb/ton. Similar results were obtained using RW as the dewatering aid. With this reagent, the final cake moisture improved from 14.9% to 13.4% at 2 lb/t of dewatering aid and from 14.3% to 13.1% at 5 lb/t of dewatering aid. These results clearly demonstrate the importance of proper conditioning when using the novel dewatering reagents. The 100
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Table 2.28. Effect of mixing intensity on dewatering of Buchanan’s flotation product Moisture Content (%) Reagent RU RW Dosage High Energy Low Energy High Energy Low Energy (lb/t) Mixing Mixing Mixing Mixing 0 18.2 18.2 18.2 18.2 1 15.4 17.1 13.5 15.5 2 13.2 14.9 13.4 14.9 3 11.9 14.6 13.1 14.7 5 11.7 14.6 13.1 14.3 results also indicate that the high-intensity conditioning increases the adsorption density of dewatering reagents; as a result, lower moisture filter cake product can be obtained. g) Pilot-Scale Test Results Table 2.29 gives the results of pilot scale dewatering tests which were obtained using various dewatering reagents at different addition rates. The data indicate the moisture content of the filter cake decreased from a baseline (no reagent) value of 16.9% to 14.5% with 5 lb/ton of RU and to 15.0% with RW. Likewise, Table 2.27 gives the laboratory test results obtained on the Buchanan plant flotation product using RU and RW as the dewatering aids at 20 inches Hg vacuum. As it can be seen from the table, the moisture content in the filter cake was decreased with increasing reagent addition. At RU additions of 1 and 5 lb/t, the moisture contents of the cake were reduced from 17.6% to 16.1% and 14.4%, respectively. Similar results were obtained when RW was used as a dewatering aid. These values correspond to a 15-20% moisture reduction in the filter product. 101
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Table 2.30. Effect of pilot-scale filter disc speed on filter cake production rates and moisture content Filter Disc Product Moisture Speed Rate Content (min/rev) (lb/hr) (%) 3.0 182.6 16.9 2.0 238.9 16.7 1.0 256.5 17.3 The effect of filter disc speed was also investigated in the pilot-scale tests. Table 2.30 summarizes the results obtained by increasing the filter disc speed from 3 to 1 min/rev for dewatering of the plant flotation product. The product rate increased from 182.6 to 256.5 lb/hr, with a small change in the moisture content of the filter cake. The results show that it would be possible to increase the filter capacity by 28% without adversely impacting the moisture content of the filter cake. Tests were conducted on Buchanan plant flotation product without dewatering reagents. A series of pilot-scale dewatering tests were conducted to study the effects of different Table 2.29 Effect of reagent addition on the pilot-scale dewatering of Buchanan’s flotation product Reagent Moisture Content (%) Dosage RU RW (lb/t) 0.0 16.9 1.43 15.7 3.08 15.2 6.05 14.5 0.00 16.9 1.47 15.8 3.19 15.5 6.31 15.0 102
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vacuum levels on moisture reduction. The initial results, which are presented in Table 2.31, were obtained without dewatering aid addition. The data show that it is possible to reduce the product moisture from 19.7% to 17.1% by simply increasing the vacuum level from 5 to 15 inches Hg. It seems that a further increase in vacuum is not advantageous in terms of further lowering the moisture contents of the filter products. It should be mentioned here that the disc filters in the Buchanan preparation plant are currently operated at vacuum levels of only 10.5- 11.0 inches Hg. Because of such low vacuum levels, the plant filter product typically contains 21-22% moisture. The present work shows that by increasing the vacuum levels from 5-11 in Hg, the plant could probably obtain a filter product with 17-18% moisture. Besides dewatering aid addition, vacuum level is one of the important operating conditions determining the final product moisture in the filter cake. Table 2.32 gives the pilot-scale test results obtained on the Buchanan plant flotation product using RW as the dewatering aid at various vacuum pressures. As shown, the moisture content in the filter cake was reduced with increasing vacuum pressure. At vacuum pressure increasing from 10-20 in Hg, the moisture contents of the cake were reduced from 18.2 to 16.8% and 16.3%, respectively. The test results given in Table 2.33 indicate that a further improvement in filter cake moisture (about two percentage points) was obtained when using RU as dewatering aid. As the vacuum levels increased from 10 to 20 in Hg, the moisture content of the cake were reduced from 16.8 % to 14.5% and 14.3%, respectively. 103
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2.3.6. Elkview Site a) Site Description The Elkview coal cleaning plant, B.C Canada, is processing 1,400 metric tons per hour (t/hr) of run-of-the-mine (ROM) coals. The materials that are floated and dewatered are classifying cyclone products. The cyclone overflows (O/F) are fed to five banks of mechanically agitated flotation cells, while the underflows (U/F) are fed to sieve bends (60 mesh). The sieve bend U/F joins cyclone O/F and are fed to the flotation cells, while the sieve bend O/F bypasses the flotation cells. The froth product and the sieve bend O/F’s are combined and fed to vacuum disc filters to reduce the moisture to approximately 21.5%. The filter cake is then fed to a thermal dryer to further reduce the moisture to 8.4%. Typically, the thermal dryer is operating at its maximum capacity, i.e., 65 t/hr of water evaporated, and cannot handle additional froth product. Under this condition, operators cannot pull the flotation cells hard, causing a significant loss of fine coal. The primary objective of the project was to develop appropriate methods of reducing the filter cake moisture to the level that can eliminate the situation where the thermal dryer is acting as a bottleneck for increased production. These novel dewatering aids are designed to increase hydrophobicity. As such, the dewatering aids can be added to a flotation cell displacing some, or perhaps even all, of the conventional collector (kerosene) that is currently used. This can result in a higher flotation recovery while at the same time improving dewatering. However, the novel dewatering aids would work better if they were added to a separate conditioner with a strong agitation since the energy dissipation in a flotation cell is generally less than that in a well- designed conditioner. Therefore, the extent of moisture reduction may be less when the froth cell is used for conditioning. Adding the dewatering reagent in place of collector for flotation 105
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may be sufficient since relatively small moisture reduction may be sufficient in eliminating the bottleneck at the thermal dryer and thereby allowing operators to pull the flotation cell hard and increase the recovery. To meet this objective, a series of dewatering tests have been conducted at Virginia Tech. The present work was limited to testing the novel dewatering aids to reduce the moisture of the filter cakes produced from the vacuum disc filters at Elkview. b) Reagents The investigation, both laboratory and pilot-scale, was performed with varying amounts of three types of dewatering aids, namely RW, RU and RV. Since these dewatering aids are insoluble in water, they were dissolved in a solvent. In both laboratory and pilot scale experiments diesel was used as the solvent. The ratio of reagents-to-solvent was optimized in previous studies by varying the individual dosages (0.5 to 3 lb/ton), while maintaining the total blend dosage constant. For this test program, the optimum combination for a given dewatering aid and solvent is one to two (1:2) dewatering aid-to-diesel ratio. When flotation feed was used, the sample was subjected to laboratory flotation tests using 0.66 lb/t of kerosene or RV as collectors and 0.44 lb/t of MIBC as frother. c) Coal Samples Two types of samples were received from the Elkview site, i.e., a standard metallurgical coal (Std-Met) and a medium-volatile metallurgical coal (Mid-Vol Met). In each case, both flotation feed (minus 60 mesh, 2-3% solid by weight) and vacuum filter feed (67% froth product and 33% sieve bend overflow, 25% solids by weight) samples were received. d) Laboratory Procedures Most of the laboratory filtration tests were conducted using a 2-inch diameter Buchner vacuum filter at 20-inch vacuum pressure (68 kPa) and 2 minutes of drying cycle time. To 106
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compare the effect of pressure drop on filtration, a few tests were also conducted using a 2-inch diameter pressure filter at a 30 psi of compressed air. In each dewatering test, a coal sample was conditioned in a mixing tank for 2 minutes. The cake thicknesses were varied in the range of 15 to 25 mm by varying the slurry volume. To prepare the test samples, a series of flotation tests were conducted using a Denver laboratory flotation cell. In each test, a known amount of a dewatering/flotation aid was added to the flotation cell and the slurry was agitated (or conditioned) for 2 minutes before introducing air to the slurry to initiate flotation. When the froth product was to be used for dewatering tests, the flotation tests were conducted until exhaustion and the froth product was used for filtration tests in the same manner as described above. In this procedure, the flotation cell was used effectively as a conditioner. In this series of tests, the flotation products were not analyzed for ash to determine the recovery. e) Laboratory Test Results (Filter Feed – Standard Metallurgical Coal) Table 2.34 gives the results obtained on the filter feed sample using RW and RV as dewatering aids. The tests were conducted at 22-24 mm cake thickness by varying the reagent dosages. The reagents were used as 1:2 blends with diesel, and the dosages given refer to the Table 2.34 Effect of reagent addition on dewatering of Elkview’s filter feed sample (standard metallurgical coal) Reagent Moisture (%) Dosage RW RV (lb/ton) 0 20.17 20.17 0.1 17.92 17.72 0.5 15.82 16.06 1 14.73 15.43 2 13.11 13.88 3 12.73 13.84 107
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Table 2.35. Effect of using RW, RU and RV on the dewatering of Elkview’s filter feed (STD Met Coal) Reagent Moisture (%) Dosage RW RU RV (lb/ton) 0 25.56 25.56 25.56 0.1 18.04 17.69 17.99 0.5 15.83 15.45 15.49 1 14.39 13.73 15.36 2 11.93 12.97 13.82 3 11.93 12.32 12.92 active ingredients only. As shown, the cake moistures decreased from 20.17% to 12-14% range. Table 2.35 gives the results of the laboratory vacuum filter tests conducted on the filter feed (STD met coal) sample using RW, RV and RU as dewatering aids. The tests were conducted at approximately 15 mm cake thicknesses. The moisture was reduced from 25.56% to the 12-13% range, which represents approximately 50% moisture reduction. The higher moisture obtained at the control test was probably due to the fact that the tests were conducted a few days after receiving the sample. The results showed that RW was most effective, followed closely by RU and RV. f) Laboratory Test Results (Filter Feed – Medium Volatile Metallurgical Coal) Table 2.36 gives the laboratory test results obtained on the Mid-Vol filter feed using RW, RV and RU as dewatering aids. The tests were conducted at approximately 15 mm cake thickness by varying the reagent dosages. Cake moistures were reduced from 23.34% to 13-14% range, representing approximately 43% moisture reductions. 108
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g) Laboratory Test Results (Flotation Feed) The two flotation feed samples (Std-Met and Mid-Vol-Met) were subjected to a series of dewatering tests. As shown in the previous sections of this report, cake moistures can be reduced to the 12-14% range by weight using 2 to 3 lb/ton (active ingredient) of the novel dewatering aids. This was achieved by adding the dewatering aid to a conditioning tank so that it is readily dispersed in the slurry. It was found in our previous work that moisture reduction improves with increasing energy input during conditioning. Figure 2.13 shows a relationship between moisture reduction and energy input. The results presented in this figure have been obtained on a clean bituminous coal sample (from Moss 3 preparation plant, Virginia) that has been pulverized before dewatering tests. In the present work, it was decided that dewatering tests be conducted without using a stand-alone conditioning tank. Instead, the coal samples were conditioned during flotation with varying reagent dosages. The energy dissipation imparted by a flotation cell is substantially 16 14 12 10 8 6 4 2 0 0 10 20 30 Figure 2.13 Effect of conditioning on moisture (Middlefork coal) 110 )%( erutsioM Power x Time1/2
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lower than that of a conditioner. Therefore, the results would not be as good as the case of using a conditioner, but the moisture reduction may suffice the needs at Elkview. One concern we had with this approach was the possibility that we would have to use a higher dose of frother when using a higher dose of collector/dewatering aids. Figure 2.14 shows the results obtained with the standard metallurgical coal and the Mid- vol coal using RV. The reagent dosages given in the figure include both active ingredient and solvent. The ratio of the active ingredient and solvent ratio was 1:2. Cake thicknesses were approximately 20 mm and two minutes of drying cycle time was employed. In the control test conducted with kerosene as collector, the cake formation time was one minute, which was reduced to 25-35 seconds when using RV. The tests were conducted on the flotation products without conditioning. The flotation tests were conducted using various amounts of collectors. In all flotation tests, 0.33 lb/t of MIBC was used as frother. With this coal, it was not necessary to increase frother dosage at higher collector dosages. As expected, moisture reductions improved substantially with increasing collector dosage. The reagent dosages given are inclusive of the solvent, which comprised 66% of the total reagent addition (the results are plotted in metric units). At 1,500 g/t (3.3 lb/t), which was the highest dosage employed in these series of tests, the cake moistures were 15.9% for the Mid-vol coal and 16.6% for the standard metallurgical coal. These values are comparable to those obtained with the filter feeds. At the 1,500 g/t (3.3 lb/t) dosage, which is equivalent to 500 g/t (or 1 lb/ton) active ingredient, the dewatering tests conducted on the filter feeds after stand-alone conditioning gave moistures of 15.56% for the standard metallurgical coal and 16.46% for the Mid-Vol coal. Note that the moistures of the floated products are comparable to those of the filter feeds despite the facts that the separate conditioning step was omitted and that particle size was finer. Recall that the filter feed was 0.6 111
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mm x 0 while the flotation product was 0.3 mm x 0. It appears, therefore, that the conditioning step can be omitted for the Elkview coal, which is a significant advantage. 23 22 21 20.6 20.3 20 19 18 17 16 15 100 400 700 1000 1300 1600 Reagent Dosage (g/t) Figure 2.14 Results of the low-pressure pressure filter tests conducted on the Elkview coal sample (filter feed). It would be of interest to compare the results obtained with RV with those obtained with kerosene. The froth products obtained using 700 g/t (1.4 lb/ton) of kerosene gave moistures of 20.6 and 20.3% for the standard metallurgical coal and medium volatile coals, respectively. At present, Elkview is using 600 g/t (1.3lb/t) kerosene as collector and 60 g/t of MIBC as frother. At 700 g/t RV and 120 g/t MIBC, we obtained 17.9 and 17.4% moistures for the standard metallurgical (1.4lb/t) coal and Mid-vol coal, respectively. Thus, the use of RV can reduce moistures by 2.7 to 2.9 percentage points absolute over the case of using kerosene as collector at 112 )%( erutsioM RV (MidVol) RV (STD Met Coal) Kerosene (Mid Vol) Kerosene (STD Met Coal)
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2.3.7. Smith Branch Site a) Site Description One of the most promising coal samples evaluated in this project was obtained from the Smith Branch impoundment located near the Pinnacle Mine Complex. The complex, which is owned by Cleveland Cliffs Mining, consists of an underground mining operation, a surface wash plant, and the waste coal impoundment. The Pinnacle site contains approximately 100 million tons of unmined coal reserves of which 3.3-4.0 million tons are processed annually by the wash plant. The waste coal from the plant is diverted to the Smith Branch Impoundment, which is believed to contain 2.85 million tons of potentially recoverable fine coal. b) Coal Samples A number of coal samples were used to conduct dewatering tests during the evaluation and scale-up tests. Samples were taken from the PinnOak Company’s Pinnacle Plant site and Smith Branch Impoundment near Pineville, WV. The samples consisted of a Vibracore composite sample taken from the Smith Branch Impoundment, a grab sample of current thickener underflow (taken in 2002), and a slip-stream sample of current thickener feed. All of these samples were tested in both the laboratory and pilot scale using newly-developed dewatering aids. Shown below is an overview of the samples used in dewatering tests. i) Laboratory Tests Smith Branch Vibracore Composite Sample (68% solid, 30% ash) Plant’s Thickener Underflow Sample (12% solid, 33% ash) Plant’s Thickener Feed Sample (1.6% solid, 46% ash) ii) Pilot Scale Tests Smith Branch Vibracore Composite Sample (68% solid, 30% ash) Plant’s Thickener Feed Sample (1.6% solid, 46% ash) 114
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Vibracoring is a technology used to extract core samples of underwater sediments and wetland soils. The vibrating mechanism of a vibracorer, sometimes called the "vibrahead," operates on hydraulic, pneumatic, mechanical, or electrical power from an external source. The attached core tube is drilled into sediment by gravitational force and boosted by vibrational energy. When the drilling is completed, the vibracorer is turned off, and the tube is pulled out with the aid of hoist equipment. Extracting core samples via the Vibracore sampling method assessed the quality of fine coal contained in the impoundment. The 2.5 inch diameter cores were extracted down to depths of 25 to 30 ft. and subjected to size and ash analyses. Figure 2.15 shows a typical set of size-by-size analyses that were obtained from one set of core samples. Error bars are provided to illustrate the high, average, and low values obtained for each size class. This particular set of data shows that the minus 270 mesh fraction contains about 60% of the coal tonnage, with an average ash content of about 33-35%. The raw quality within the impoundment was found to vary greatly, dependent on the distance from the discharge point into the impoundment. In general, coal extracted near the discharge point was found to be 80 70 60 50 40 30 20 10 0 Plus 28 28x100 100x270 Minus 270 Size Fraction (Mesh) Figure 2.15 Weight and ash distributions of slurry from the Smith Branch impoundment 115 )%( thgieW 40 35 30 25 20 15 10 5 0 Plus 28 28x100 100x270 Minus 270 Size Fraction (Mesh) )%( hsA
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coarser and higher in ash, while the coal extracted farther away from the discharge point was finer and lower in ash. Also, coal fines extracted from a greater depth were found to be of better quality than coal taken from more shallow locations. This was expected because the coal fines deposited earlier in the life of the mine were discarded before several improvements were made to the fine coal circuits in the existing preparation plant. The average ash content of the remaining 40% had an ash content of less than 15%. c) Laboratory Procedures The laboratory flotation and dewatering equipment consists of a Denver laboratory flotation cell, a vacuum pump, a mechanical shaker, a stand-alone mixer – in some cases – and a Buchner Funnel with a fitted filter medium. All the vacuum filtration tests were conducted using a 2.5 inch diameter Buchner Funnel at 20-25 inch Hg (68 kPa) with a 40X60 wire screen mesh filter medium. The dewatering tests were conducted to determine the best reagents and dosages for different samples and to investigate under what conditions a given dewatering aid can give the best performance. All the coal samples were tested within three days of receipt in order to minimize any artificial negative effects of aging or surface property changes on dewatering. Because the samples were taken from the waste pond, thickener feed discharge, and thickener underflow discharge, they possessed high impurities. For this reason, a cleaning step was employed before the filter tests. Depending on the solid content, the samples were prepared first by either diluting or decanting to 16-17% solids and floated in a laboratory Denver flotation cell approximately at 1000 rpm using 0.88 lb/t kerosene and 0.33 lb/t MIBC to remove ash. A limited number of flotation feed and product samples were analyzed for ash. Then, the samples were collected in a separate container to be used in filtration tests. The dewatering aids RW, RU, 116
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and RV were tested and diluted to 33.3% in solvent. When using the dewatering aids, conditioning is critical, and increased energy input in conditioning yields improved moisture reductions. For this reason, prior to each filter test, a known volume of slurry was conditioned with the dewatering aids in the mechanical shaker and, in some cases, the stand-alone mixer. When the mechanical shaker was used, the conditioning time was kept at 5 minutes, and when the stand-alone mixer was used, the conditioning time was kept at 2 minutes. Then, the conditioned sample was poured into the Buchner funnel for filtration. During the tests, the cake thickness was determined by the amount of the slurry sample used. Some of the conditions were kept constant during the tests. For example, a 7-10 mm cake thickness was determined for 2 minutes of drying time. d) Pilot-Scale Procedures The continuous dewatering test rig used at the Smith Branch site incorporated three main components, a column module, conditioner module, and a disc filter module, along with some other ancillary components. The details about the modules were described previously. For the pilot-scale tests, feed slurry was supplied from either the existing preparation pond reclaim facilities or in barrels and directed into the circuit feed sump. During the tests, the slurry was fed at a constant rate into a 12 inch diameter column by means of a peristaltic pump and flexible piping. The flotation column was used to produce a filter feed and reject ultra-fine hydrophilic clay that negatively impacts the effectiveness of some of the dewatering aids. Then, the clean coal froth was routed to the multi-stage conditioner module by gravity while the column reject slurry flowed, also by gravity, to a refuse sump. After adding appropriate dewatering reagents, the conditioned slurry was pumped at a constant rate into the filter test module. Next, the conditioned slurry was dewatered in the filter module. The filter cake was discharged into a 117