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CHAPTER 4. DETAILED TESTING OF FLOTATION ROTOR DESIGN at high tip speeds while drawing low power. Furthermore, the drastic phenomenologi- cal difference in power reduction and gas dispersion (Figure 5.9) may provide insight on the operational advantages present in this rotor. 4. Intermsoffloodinglimit, solidsuspension, andoverallareaofstableoperation, theVT - B2 substantially outperforms its counterparts. This rotor is capable of suspending solids at a relatively low power draw, and this suspension capacity is not as sensitive to airadditionastheotherrotors. ThetwoadditionalbladesoftheVT-B2provideaddi- tional area for gas dispersion. This mechanical feature necessitates an increased power number, but it also provided additional capacity to overcome the flooding condition. 5. Bulk comparisons of the air holdup versus power data and the rate constant versus power data show strikingly similar trends. While a one-to-one correlation is not neces- sarily suggested, the same results are determined from test. Theoretically, this result is justified since air holdup is related to the available surface area which is related to flotation performance. 6. FactorssuchasS andotherdimensionlessparameters(Reynoldsnumber, PowerNum- b ber, and Aeration Number) are capable of producing consistent relationships to perfor- mance criteria for each rotor. The magnitude of the laboratory values generally match those reported for industrial machines. The continued use of these values in scaling studies is recommended. 4.5 Bibliography Banisi, S., & Finch, J. (1994). Technical note reconciliation of bubble size estimation methods using drift flux analysis. Minerals Engineering, 7(12), 1555–1559. Fitzgibbon, A., Pilu, M., & Fisher, R. (1999). Direct least square fitting of ellipses. Pattern Analysis and Machine Intelligence, IEEE Transactions on, 21(5), 476–480. Hernandez-Aguilar, J., Gomez, C., & Finch, J. (2002). A technique for the direct mea- surement of bubble size distributions in industrial flotation cells. In Proceedings of the 34th annual meeting of the canadian mineral processors (pp. 389–402). Silva, R., Echeverri, L., Olson, T., Foreman, D., Yang, Y., & Caldwell, K. (2012). The effect of laboratory cell design on flotation machine hydrodynamics, solid suspension and particle recovery. In 2012 sme annual meeting and exhibit preprints (pp. 452–457). SME. 122
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Chapter 5 Conclusions and Recommendations The primary objective of this research was to characterize and compare small-scale flotation rotors while developing scaling relationships and future design criteria. In order to complete this task, several experimental setups were initially constructed to measure various flotation performance parameters. In choosing the appropriate parameters to measure, the- oretical factors, practical limitations, and industrial experience were equally acknowledged. As a result, most testing focused on four distinct evaluation criteria: power draw, gas disper- sion, operational robustness, and flotation performance. The measurement and analytical approach to these criteria needed to provide reliable data which retains significance as the rotors are scaled to the industrial size. Furthermore, the data must provide a basis for fair comparison among the alternative rotor designs, and the experimental techniques must coincide with the expected paradigms and costs of a typical flotation laboratory. This report extensively described the experimental techniques used to evaluate the four performance criteria. The theoretical background was first established, and the required equipment and analytical means were explained. When applicable, measurements were nor- malized by or compared against power input. In the laboratory setting, power input is the most easily determined cost associated with flotation equipment, and this measurement may be scaled to the full-size by dimensionless relationships. Furthermore, when comparing alter- native rotors, differences in power draw measured at the laboratory scale will retain relative relationships as the scale is increased (although the absolute magnitude of the difference may radically change). Testing for this project task was primarily conducted in two campaigns. The original, exploratory campaign focused on the analysis of 14 rotors in a select range of operating conditions. The second, detailed campaign included on a more rigorous analysis of three 123
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CHAPTER 5. CONCLUSIONS AND RECOMMENDATIONS selectrotorsinseveraloperatingconditions. Alltestswereperformedwith2.75inchdiameter rotors in tanks 10 and 14 inch diameter tanks (9 - 35 liters). The goals of the exploratory campaign were to establish and refine the experimental procedures, verify the existence of performance difference between rotors, and narrow the field of potentially viable prototypes by eliminating underperforming or “fatally-flawed” alternatives. From this campaign, the SP - A1, VT - A4, and VT - B2 were selected for further experimentation. The goals of the detailed campaign were to implement standard modes of evaluation and analysis, examine uncertainty and repeatability in the measurements, thoroughly characterize the remaining rotor prototypes, and establish insight on the causes of performance differences. Following the successful completion of both laboratory campaigns, the following obser- vations and design criteria are derived: 1. Given the strengths of the VT - A4 in the areas of power-normalized gas dispersion andflotationperformance,flotationsystemsdesiringthesecharacteristicsshoulddesign rotors to exhibit low inherent power numbers and operate near the boiling condition (seeFigure4.3, Figure4.12, Table4.6, andFigure4.22. Unfortunately, theseattributes general realize a reduction in operational robustness, especially with regard to the sanding condition (see Figure 4.15, and Figure 4.16). 2. Alternatively, the strengths of the VT - B2 rotor in the areas of operational robustness should entice high power numbers and operational away from the boiling condition with solid suspension is problematic (see Figure 4.3, Figure 4.14, Figure 4.15, and Figure 4.16). 3. Given the measured linear relationship between k and S , rotors desiring high flotation b rates should seek to maximize S (see Figure 3.13, Figure 3.14, and Figure 4.18). b 4. Plots showing global air holdup plotted against power show striking general similar- ity to plots showing flotation rate constant plotted against power. Consequently, air holdup can be used as an acceptably surrogate to flotation testing when comparing machine designs (see Figure 4.20 and Figure 4.22). 5. Care should be taken when comparing batch and continuous data. S ratios should b be used to scale the measured flotation rates, and appropriate plug-flow or perfectly- mixed models should be selected. Note that in order to achieve the same recovery up to a seven-fold increase may be necessary in residence time when changing from batch to a continuous reactor (see Figure 4.23, compare residence time at 65% recovery). 124
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CHAPTER 5. CONCLUSIONS AND RECOMMENDATIONS Finally, the author of this thesis recommends the following three topics for further and continued study: 1. Additional quantification of scale factors and verification of lab-scale to full-scale ap- plicability. While the tested rotors consistently show variations in performance criteria on the lab scale, the absolute magnitude of these differences is not expected to remain proportional as the scale is increased. Testing and characterization at the larger scales may assist in identifying scale-factor which can reliably predict the magnitude of these differences as the scale is increased. 2. Larger scale implementation of the prototype rotors. Given the strengths each rotor has consistently manifested at the laboratory scale, further development and imple- mentation at a larger scale is recommended. 3. Additional refinement of laboratory testing and analytical techniques. While the meth- ods described in this report have fulfilled the goals of obtaining a fair and consistent basis of comparison between the rotor alternatives, further development and revision may provide additional insight to the fundamental difference between each rotor. Also, byincorporatingautomation(levelcontrols, airholdupmeasurements, solidsuspension determination), the degree of testing reliability and reproducibility will be enhanced. 125
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Elutriation Technology in Heavy Mineral Separations Matthew Donnel Eisenmann ABSTRACT Hindered-bed separators have been used in several different mineral processing fields for many years. Recent improvements in designs have led to the development of the CrossFlow separator. This new design employs a tangential feed system that has shown promise in several applications. This paper investigates the use of this relatively new technology to upgrade heavy mineral concentrates using Florida type ores. The intended use of this separatory device in this particular application is the removal of gangue quartz from other valuable heavy minerals such as ilmenite, leucoxene, rutile, zircon, and staurolite. The results of two different pilot-scale in-plant testing investigations are discussed. In general, quartz rejections in excess of 80% were achieved while maintaining TiO and heavy mineral 2 recoveries above 98% and 99%, respectively. In addition to field test work, two separate unit models have been developed. The first model is an empirical investigation into understanding unit operation and functionality. The second model is a statistical prediction of unit operation based on specific field test work. These models can be used to effectively scale-up a CrossFlow unit for full-scale installation at any Florida heavy mineral sands operation. Emphasis is placed on unit capacity and other operational parameters such as elutriation flowrate and bed level. i
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ACKNOWLEDGEMENTS The author wishes to express his deepest appreciation to Dr. Gerald Luttrell. His support, guidance, and knowledge throughout this thesis work was invaluable. The author would also like to thank Dr. Greg Adel and Dr. Roe-Hoan Yoon for their advice throughout undergraduate and graduate studies. The author would like to thank Dupont White Pigments and Mineral Products for their continued support. Special thanks to Vincente Stutts, Process Engineer, and Francisco Parisi, R&D Supervisor, for their understanding, guidance, and assistance. Sincere appreciation is extended to all those graduate students who spent many late nights at the Plantation Road Laboratory including: Jaisen Kohmuench, Tim McKeon, Ian Sherrell, and even Brian Halford. Special thanks to the Department of Mining and Minerals Engineering Administrative and Secretarial Staff. The author would also like to express his thanks to his parents, siblings, and God; for their constant influence on his continued education. They all provided love and support throughout this entire process, as well. Lastly, the author would like to express his love and appreciation to his wife, Colleen, for her love, support, understanding, and caring attitude that made this entire thesis possible. ii
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CHAPTER 1 1.1 Introduction Titanium Dioxide (TiO ) is a material used in a variety of commercial products. 2 Relatively pure titanium dioxide is used extensively as a pigment in the food, ceramics, paper, and paint industries. Titanium is also used in metal production where its low weight and high strength are beneficial in many different applications. The primary source of TiO 2 is a mineral called ilmenite. In 1998 the world production of ilmenite was over 4 million metric tons. Along with the United States, other major producers include South Africa, Australia, and Canada. In the United States, Florida and Virginia are the two key production areas for titanium bearing minerals. These sites occur primarily as placer type deposits and span several miles. The TiO in these deposits is primarily contained within the heavy minerals 2 ilmenite (FeTiO ), rutile (TiO ), and leucoxene (FeTiO ). Also contained within these 3 2 3 deposits are significant amounts of zircon (ZrSiO ) and staurolite (Fe+2Al [SiO ] O [OH] ). 4 4 4 2 2 2 Zircon is used in zirconium metal and various abrasive and foundry applications; and staurolite is used primarily as an abrasive in the sand blasting industry. Due to their high specific gravities, the above listed specific minerals are termed heavy minerals throughout the industry. The initial processing of these heavy mineral sands is done primarily by the use of spiral separators. This type of separatory equipment uses the differences in densities of the material to concentrate the heavy minerals through low gravity means. Characteristics such as low unit efficiency and low capacity have plagued this type of wet separation in the past. 1
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Until recent years, heavy mineral concentration was performed solely by spiral separators. However, several different gravity based separation techniques have been developed and implemented in various mineral processing applications. Of these techniques, hindered-bed classifiers have been used quite frequently in various sections of the heavy mineral industry. Their low capital cost, ease of operation, and high capacities has led to promising results in several different applications. These devices have also been used quite successfully in other industries such as coal, mica, sand and gravel, and phosphate. This type of density based separator relies on two key physical properties of the mineral being separated, size and density. In a mono-density application this device is quite efficient in performing a size separation of the feed material. In a mono-size application a hindered-bed classifier is extremely efficient in performing a density separation. However, when the feed material contains varying mixtures of both size and density, unit performance is significantly reduced. Several investigations have been performed on the implementation of hindered-bed separators and their use within the heavy minerals industry. They have proven to be successful when used in combination with the spiral circuits. Recent work has shown promise in specifically using this device as a final stage in order to upgrade the concentrate generated by the spiral circuit. A novel device known as the CrossFlow has been examined for this particular application. The CrossFlow uses a new feed introduction system which has been proven effective in several heavy mineral applications. Both laboratory and pilot- scale test work in this application are discussed within this report. 2
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1.2 Literature Review Hindered-bed classifiers have been used extensively throughout the minerals industry for several years. These classifiers are typically used to categorize mineral particles according to both size and density. They have been proven useful in recent years for density based separations in fine coal applications (Mankosa et al., 1995; Reed et al., 1995; Honaker, 1996). Also, these devices have been of particular interest for carbon recovery from both active fine coal streams and refuse ponds. With low capital cost and high capacities, hindered-bed classifiers have found their way into many different sectors of the mining industry. Most hindered-bed classifiers operate on the same basic principles. First, material is introduced into a tank in slurry form. Water, termed teeter water, is then injected into the tank bottom. This process generates a zone of fluidized particles above the teeter water injection point. This zone is where separation of the particles takes place based on both differences in gravity and particle size. Within the fluidized zone, particles with a low settling velocity report to the unit overflow. Under normal operation, both fine particles and lower density particles have low enough settling velocities to report to this location. During the same process, coarser particles and heavy material with much greater settling velocities work their way through the unit and are eventually ejected from the bottom outlet of the device. The quantity of teeter water added to the unit and height location of the fluidized bed are the two main factors that determine the separation process. These separators typically work quite efficient in applications where the feed material is either mono-density or mono-size. However, when the feed presented to the unit is varied in both size and density, efficient separation becomes difficult. Under this application the 3
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shortcoming of this particular unit is that coarse low-density particles tend to accumulate in the teeter bed region. As other particles begin to congregate in this same zone, these coarse low-density particles are ultimately forced through the bottom unit discharge by mass action. To compensate for this unit phenomenon, the teeter water rate is typically increased, but this causes fine, dense material to become misplaced to the overflow. Both of these processes adversely affect the unit’s overall separation efficiency. Recent test work with Australian based mineral sands concentration has shown several successful circuit combinations using both spiral and hindered-bed separation technology (Elder et al., 2001). This test work employed the use of a typical hindered-bed separator as a final upgrading step after spiral concentration of heavy minerals. Although the results were promising, high heavy mineral recovery was only successful for low levels of quartz rejection. Table I shows the data derived during this investigation. For higher rejection levels of 81.7%, heavy mineral recovery drops to 96.6%. It may be possible that Australian mineralogy adversely affects the performance of this particular setup. The specific unit design employed for this testing could also negatively impact performance. Table I: Investigative Hindered-bed Separation Test Work on Heavy Mineral Concentrate (Elder et al.,2001) 4
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Pilot-scale testing of a conventional hindered-bed separator for heavy mineral separation, which later developed into full-scale installation, was performed by McKnight et al., 1995. This particular application was the removal of quartz gangue from zircon rich tailings. These tailings contained approximately 3-8% Zircon, 18-22% Al O , and 1% TiO . 2 3 2 Quartz rejections above 80% were achieved with zircon recoveries higher than 90%. In this particular application the density difference between zircon, 4.7, and quartz, 2.7, was sufficient to allow proper separation despite the tremendous size discrepancies between the two minerals. However, in near-density applications this conventional hindered-bed approach would prove insufficient (Dunn et al, 2000). To overcome the shortcomings with typical hindered-bed separators, a novel device known as the CrossFlow separator was developed. This unit relies on an alternate feed presentation system that reduces the amount of fine, dense particles that become misplaced to the overflow launder. The CrossFlow is comprised primarily of a rectangular tank, as seen in Figure 1, that is divided into two regions; an upper separation chamber and a lower dewatering cone. Within this novel device, feed is presented tangentially across the upper portion of the unit. This tangential feed entry system allows for a lower velocity introduction of feed across the top of the classifier. This feed presentation design allows the unit to operate more efficiently than other conventional apparatuses. 5
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Given the advantages of the CrossFlow elutriator, testing began on various samples of heavy mineral concentrate from a typical Florida mineral sands operation (Dunn et al, 2000). The samples were comprised of several different minerals with differences in both size and density. The majority of the concentrate samples were comprised mostly of ilmenite, leucoxene, zircon, staurolite, and quartz. In this particular application, quartz represents the gangue/trash material that must be removed in order to produce pure heavy mineral products. Individual mineral characteristics are discussed later within this report. 1.3 Typical Heavy Mineral Operations 1.3.1 Processing Overview Several heavy mineral operations are located in northern Florida. The deposits are relatively shallow and span many hundreds of acres stretching from south to north. The majority of heavy minerals contained within these deposits are present within the first 50 feet of ground depth. This thickness reduces to a mere 15 feet toward the outer edges of the deposit on both the west and east sides. The in-situ feed matrix is comprised mostly of sand, clay, and “hard pan”. Hard pan is a composite material containing individual sand grains cemented together by humate, clay, and fine organics. This cemented material is located throughout the deposits in thin veinlets ranging from 1 to 4 feet thick. The in-situ sand matrix is first excavated by means of a dredge. This dredging technique involves the use of a rotary cutter head to excavate and loosen the feed matrix. The dredge pivots around a spud system through use of several different swing lines. The dredging techniques developed by the mining industry are basically retrofitted canal dredging systems. The excavated material is then pumped directly to a rotating trommel, which 7
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removes plus 1/4” material. The oversize material is primarily made up of roots, other organic material, and hard pan. Although hard pan contains economic levels of TiO bearing 2 minerals, it is extremely abrasive and difficult to process, and is thus rejected from the process immediately. After the oversize has been removed, the feed material is sent through several stages of spiral classifiers. This spiral circuit is responsible for upgrading the feed from approximately 3-5% heavy mineral to a concentrate grade of 75-85%. The spiral circuit consists of four stages with numerous re-circulating loads. The four circuits used in this process are rougher, cleaner, finisher, and scavenger. Each of these stages consists of spirals specifically designed for certain separations. This circuit configuration is extremely effective in generating low grade, “throw away” tailings. These tailings are immediately pumped for re-contouring and subsequent reclamation activities at the mine site. However, this four stage configuration has proven inefficient in upgrading the concentrate above 85% heavy mineral without suffering high losses in both TiO and heavy mineral recovery. Figure 2 2 shows the general flowsheet for this concentrate after gravity separation. 8
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important, as it also adversely affects dry mill separation. The “clean” concentrate is then transported to several dry mill facilities, where electrostatic and magnetic separation techniques are used to segregate the various titanium bearing minerals and staurolite products. Tailings generated from the dry mill consist mainly of quartz, zircon, and alumino- silicates. However, small amounts of TiO bearing minerals and staurolite are still present 2 from the previous imperfect separation. These dry mill tailings are further processed using spirals and additional dry milling equipment to produce a saleable zircon product. This zircon product must be extremely low in trash material such as alumina, iron, and titanium. The extremely high product quality required makes recovery of zircon a difficult process. Many stages of spirals and dry milling equipment are required to meet these specifications. 1.3.2 Florida TiO Mineralogy 2 In the formation of these placer type deposits, the heavy mineral grains were selectively concentrated during various geologic transportational mechanisms. Evidence of these processes can be readily seen in “black sand” concentrations commonly found in most ocean beach environments. However, millions of tons of heavy mineral concentrate are required for deposits to be economically justifiable. Such deposits must have undergone lengthy geologic conditioning in order to reach concentrations of this magnitude. One example of this process is the Old Hickory Deposit owned and operated by Iluka Resources Limited, located in southeastern Virginia. Other deposits are located throughout northern Florida which are owned and operated by both Iluka Resources Limited and DuPont White Pigment and Mineral Products. 10
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The heavy mineral assemblages contained within these deposits are comprised mostly of ilmenite, leucoxene, rutile, zircon, staurolite, and kyanite. Other minerals such as monazite, spinel, and garnet are also present, but in relatively low quantities. Table II gives general information on the density and composition of these minerals. The TiO minerals 2 which comprise the majority of production from these deposits are ilmenite, leucoxene, and rutile. Zircon and staurolite products are also produced in significant quantities from these deposits. Table II: Summary of Mineral Characteristics Chemical Specific % of HM Mineral Type Composition Gravity Suite Ilmenite FeTiO 4.2 - 4.5 30 3 Leucoxene TiO 3.6 - 4.3 10 2 Rutile TiO 4.2 - 4.3 3 2 Zircon ZrSiO 4.7 16 4 Staurolite Fe,AL(SiO )4(OH) 3.7 18 4 Kyanite Al O (SiO ) 3.2 - 3.7 15 2 3 4 Of these minerals, the four that are of most economic interest are ilmenite, rutile, leucoxene, and zircon. Many other heavy minerals are present in this deposit, but are not of sufficient economic interest. The heavy mineral concentrate generated from the wet mill process also contains small amounts of clay and quartz, which were not properly separated. A set of four samples from this deposit where used for investigation using reflected light microscopy techniques. The textures and assemblages found within these samples are discussed. 11
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For both primary products, ilmenite and zircon, chemical make-up as determined by x-ray fluorescence (XRF) is of much importance. The stoichiometric amount of iron (Fe), aluminum oxide (Al O ), and zirconium oxide (ZrO ) are also of importance. It is thus very 2 3 2 important to determine what characteristics of the heavy mineral feed affect its chemical composition and separation efficiency. Stoichiometric ilmenite contains 53% TiO , while, ilmenite in placer deposits varies 2 widely in its actual titanium concentrations. This titanium concentration is dependent upon both the initial factors that occurred during deposition and those from subsequent weathering. Ilmenite is particularly resistant to weathering and displays a wide variety of textures in placer deposits. These textures can range from single crystals to polycrystalline aggregates. At very high temperatures ilmenite and hematite are in solid solution with one another. At lower temperatures the hematite will exsolve out of the solution and form lamellae structures within grains and at grain boundaries. These exsolution lamellae of hematite are often formed in crystallographic orientations. During weathering and erosion, selective dissolution of the more soluble hematite proceeds from the margins of the grains and continues inward. This process leaves behind empty pits within the ilmenite grains. During this process of leaching, the ilmenite grain becomes increasingly enriched in its titanium concentration. The degree to which this leaching has occurred is important because iron is not a desired constituent of the ilmenite product. Figure 3 shows reflected light microscopy slides of an ilmenite grain that has not undergone complete leaching. The leaching and removal of iron occurs primarily at the grain boundaries and along internal discontinuities. Hematite is dissolved first from the ilmenite grains due to its greater solubility. 12
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pale cream color under reflected light microscopy. Typical zircon grains are both nonmagnetic and nonconductive, although some grains exhibit para-magnetic properties due to small internal impurities in their grain structure. Zircon grains are often elongated and more angular than ilmenite due to breakage along cleavage planes during weathering. These grains show strong white internal reflection under crossed polars, as seen in Figure 6. Reflected light microscopy is a very important diagnostic tool in identifying various levels of internal impurities that may affect both separation and recovery. FIGURE 6: ZIRCON GRAIN SHOWING CHARACTERISTIC WHITE INTERNAL REFLECTIONS Rutile is also present in the mineral samples, but in much lower concentrations. Rutile has almost a pure TiO assemblage. It is a non-magnetic, conductor which often tends 2 to be finer in nature than the other heavy minerals present. Under reflected light, rutile is most noticeable by its internal reflections that are reddish brown. The existence of twinning is also an important diagnostic tool when locating rutile under the microscope. Figure 7 15
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total grain structure. In this circumstance, the specific gravity of the grain becomes 2.8, instead of 3.7 for a uniform ilmenite grain. When submersed under water, these void spaces also generate buoyancy forces. The existence of buoyancy forces within dense minerals present in an elutriation device, cause significant reduction in unit separation efficiency. These grains are inherently more difficult to separate in a density based separatory device. 1.4 Problem Statement Typical concentrate generated from the wet mill facilities is comprised of only 70- 85% heavy mineral. This particular composition is the maximum concentration possible using the existing spiral circuits without suffering excessive recovery penalties. The excess quartz fraction present must be scrubbed, hauled, and dried along with the valuable heavy minerals prior to dry mill separation. This quartz fraction also reduces dry mill capacity and lowers the magnetic and electrostatic separation efficiencies. The potential benefits of installing an effective upgrading technology at the wet mill facilities are numerous and include: • Reduced haulage costs • Reduced chemical consumption during attrition scrubbing • Reduced drying costs • Increased dry mill TiO recovery as a result of higher grade feed 2 Due to space restrictions at both wet mills, the addition of a fifth spiral circuit to achieve the required concentrate upgrade is not seen as a feasible solution. Another negative for spiral separation is the need for many secondary devices such as distributors, launders, piping, and additional pumps if gravity flow is not possible. The addition of another stage of 17
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spirals would also complicate the existing circuit quite drastically making the selection of overall circuit optimum settings extremely difficult. The particular properties of the concentrate produced through the current circuit are such that an alternate separation device would be required to achieve the desired results. Based on available data, an elutriator is one such device that employs different separation mechanisms to achieve mineral separation than the current spiral technology employed. Installation of an elutriation device would require less space and less ancillary equipment. The device would also be considerably less difficult to operate and maintain. The goal of this final elutriation stage would be to generate a “throw away” tailings stream with maximum recovery of the valuable TiO bearing minerals present in the feed material. 2 1.5 Heavy Mineral Upgrading – Initial Test Work Initial testing of the CrossFlow separator as an effective separation device for Florida heavy minerals began by using lab-scale equipment (Dunn et al, 2000). The goal of these initial tests was to evaluate the potential for effective heavy mineral upgrade by means of hydraulic classification. This test work used a 5 x 15 cm laboratory scale CrossFlow unit to simulate the process. The design of the unit was typical of the CrossFlow design principles, an upper tangential feed presentation system and a lower dewatering zone. Figure 8 shows a picture of the lab-scale CrossFlow used for testing. The disadvantage of this setup was the use of a manual control valve to regulate the underflow rate and fluidized bed level. The unit was initially fed at a target nominal feed rate of 1 tph/ft2. Efforts were made by the operators to ensure the teeter water rate was minimized for the desired amount of quartz rejection required. 18
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CHAPTER 2 2.1 CrossFlow Testing 2.1.1 Overview The first stage in scale-up elutriation test work began with continuous open circuit testing on a small lab/pilot-scale device. The CrossFlow unit used during this period of testing was installed for continuous field operation. It was installed directly in line with the final wet mill concentrate. This particular location was placed directly after the attrition scrub system and prior to dewatering and stacking. This positioning allowed introduction of clean “scrubbed” concentrate into the test unit. Clean well water was used for the elutriation network in order to additionally scrub and rinse the individual concentrate grains, thus enhancing downstream dry processing. 2.1.2 Equipment Setup The test unit was constructed by Eriez Magnetics and designed for continuous operation for approximately 0.5 to 1.0 tph of feed material. To accomplish this task, the unit was constructed with a cross-sectional area measuring 4” x 16”, allowing for feed introduction of approximately 1.0 to 2.0 tph per ft2 of cross-sectional area. The unit was constructed from stainless steel in order to prevent erosion and rust from any residual caustic (NaOH) still present in the feed stream due to attrition scrubbing. An engineering diagram of the unit constructed can be seen in Figure 11. To facilitate continuous operation, the unit was outfitted with a pneumatic underflow valve controlled through use of a microprocessor based controller system. 23
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The unit was fed directly from the final wet mill concentrate piping system. This particular point in the process circuit was located directly after the attrition scrub system and prior to dewatering and stacking. To accomplish installation at this particular location, a 2” bypass line was installed on the pipe feeding the stacker cyclone. This bypass feed contained significant amounts of pressure and was far lower in percent solids than desired. Because of these reasons, it was necessary to install an intermittent sump that could store material from the bypass and allow for greater control of the unit feed. This setup allowed the user to adjust feed rate with ease and also allowed the feed material to dewater to the necessary process percent solids. Elutriation water was delivered to the process from a fresh water well located onsite by over 600 feet of high-pressure hose. Although the pressure and flowrate in this particular line fluctuated quite drastically, a 500-gallon intermittent storage tank was installed which could pump water directly to the elutriation network. This storage and pumping system allowed for a relatively constant volume and pressure to be delivered to the unit elutriation network. The water fed to the unit through this system was extremely clean, showing no signs of added viscosity affects from humate and clay loading. All other process water located onsite contained varying degrees of humate and clay, making use of well water most desirable. The well water used typically had a pH of 5.5 and a viscosity of 1.0 cp for the majority of test work. The acidic nature of the well water used for testing was expected from prior experience with typical Florida ground water. Elutriation flowrate was controlled by use of a Cole Parmer flow meter. This particular unit is a fixed orifice flow sensor, which allows greater ease of operation compared to mechanical or ultrasonic sensors. 25
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This particular lab-scale CrossFlow was identical in design to the previous unit used, however, the underflow was controlled by a pneumatic actuator, which was regulated by a pressure sensor. The use of this particular valve control system allowed for continuous adjustment of the underflow rate in order to maintain a specified bed level and pressure within the unit. The pressure sensor used in this process correlates the pressure at a particular point within the tank to the underflow rate necessary to maintain this setting. This measurement is an indirect reading of the teeter bed interface location/height within the unit. Being able to control elutriation water rate and bed level/pressure independently is extremely important to achieve proper testing conditions. The unit was fitted with an industrial pressure transmitter capable of monitoring the ranges of pressures expected during testing. As stated previously, these pressure readings are an indirect measure of the actual teeter bed level within the unit. The transmitter selected for this application was manufactured by Omega, model #PX726-300WCGI. This particular transmitter was fitted with a weatherproof enclosure and all wetted parts were compatible with corrosive media. The most important factor for selection of this model transmitter was its rated 0.15% accuracy while used in difficult and hazardous conditions. Installation of this instrument was made possible by use of the ½” npt adapter located on the test unit’s exterior. More detailed information on this particular model can be seen in Table III. Table III: Detailed Specifications on Pressure Transmitter Output Accuracy Repeatability Stability Respons Time 4 - 20 mA 0.15% 0.05% 0.25% of URL 50 ms 26
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Required adjustments to the process are based on the information available from the transmitter output. To accomplish this task, a 2600 series microprocessor based controller manufactured by Love Controls was selected. This particular controller was capable of both manual program functions and fuzzy logic control. It allowed for direct input of process rate functions, allowing for more user defined process control. The controller output was connected directly to the pneumatic pinch valve, allowing for teeter bed level control. Extensive work was required in order to calibrate the valve functions for use with the controller output. Feed material provided by the intermittent sump was sent directly to a 2” Mosley Hydrocyclone. This device allowed significant increase in feed percent solids, which is known to be beneficial to unit operation. The underflow from this hydrocyclone was fed directly into the feed box on the CrossFlow unit. Overflow from this hydrocyclone was sent to a tank to be discarded later. Although very small portions of the feed material did report to this overflow stream, it was decided that this loss was inconsequential to the overall performance of this equipment setup. Pilot-scale and full-scale installations would require a properly sized hydrocyclone to ensure minimal loss of material during the dewatering process. 2.1.3 Testing Program Initial unit application began with preliminary testing aimed at identifying relative high and low operational conditions. The conditions tested included feed rate, teeter water rate, and bed level. Although other variables existed, they were not directly controllable with 27
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the current testing arrangement. Given this specific testing arrangement, examples of such uncontrolled variables are feed grade and feed percent solids. The feed rate used during this test program varied from 1.0 to 1.5 tph/ft2. This tonnage range appeared to offer the most quiescent flow in the separation tank. The target percent solids for this tonnage, given the cyclone feed system used, was approximately 50%. The elutriation flowrate necessary for separation given these conditions was 2.0 to 4.0 gpm/ft2. Flowrates below 2.0 gpm/ft2 caused the separation tank to clog and those above 4.0 gpm/ft2 led to significant unit overflow of heavy mineral. A total of 72 individual tests were conducted. Sampling was done approximately every four hours of unit operation. This practice allowed for the unit to experience a wide variety of feed conditions and operational fluctuations. However, this timed procedure generated occasional data points during both wet mill startup and shutdown. This led to drastic changes, beyond expectations, in unit feed heavy mineral grade. The feed rate, teeter water rate, and bed level previously used for normal process operations were incorrect for these particular periods. Inability to control these variations in unit feed grade led test operators to make small adjustments to teeter water rate and bed level. The majority of these changes were done by visual observation of the heavy mineral present in the unit overflow. Future test work will be focused around development of models capable of determining optimum operational settings for use during periods of such drastic changes in concentrate grade. Samples were taken at three different locations around the CrossFlow separator. The first sample taken was located at the CrossFlow overflow stream. A bypass valve was installed in order to facilitate sample collection. The second sample, CrossFlow underflow, 28
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was also taken at this time. The last sample point was unit feed located at the underflow of the hydrocyclone. This process stream was simply diverted for sample collection. This sample was taken last due to its drastic influence on the unit overflow. Collection of this stream prior to the overflow would have resulted in erroneous readings of the overflow stream if steady state had not resumed within the unit. The diamond symbols shown in Figure 12 represent the sample points used during this phase of test work. FIGURE 12: LAB SCALE CIRCUIT DESIGN AT THE MAXVILLE WET MILL STACKER The samples taken from these locations were decanted and promptly sent for drying. Temperature during the drying process was not an important factor since no degradation of the material is experienced at high temperatures. Frequent stirring of the samples during the initial part of the drying process was necessary to prevent “popping” of the material. The samples were next weighed in order to obtain dry weight values, and then split into smaller 29
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representative samples by use of a Jones Riffler. Approximately 100 grams of material was needed for the heavy mineral analysis for low grade samples, 0-15% HM, and about 50 grams for higher grades, 15-100% HM. Another 50 grams of sample was required for TiO 2 analysis by x-ray fluorescence techniques. Retains were also split out from the original sample and stored for various analysis which might become necessary at a later date. Heavy Mineral analysis is accomplished by using a material of known specific gravity to separate the various minerals. Current industry standards are to use LMT, Lithium Metatungstate, as the separation media. This particular chemical can be heated in order to alter the specific gravity to the required value. Typically a value of 2.7 is used for this particular analysis. At this value, light material such as quartz and other gangue minerals are removed from the heavy mineral assemblage. Two separate fractions are retained from this process, a light mineral fraction and a heavy mineral fraction. These samples must be rinsed with warm water in order to remove the excess LMT left on individual mineral grains. The samples are then dried and weighed, in order to compare with each other, so that the percent heavy mineral of the original sample may be determined. This analysis procedure is used quite frequently for exploratory drilling programs as well as wet process analysis. This procedure is not typically used for material once it enters the dry mill processing facilities. During dry mill separation, other characteristics such as conductivity and magnetic susceptibly are more useful in understanding the individual sample characteristics. TiO analysis is accomplished by using x-ray fluorescence technology. Wavelength- 2 dispersive x-ray fluorescence spectrometry, “XRF”, is a non-destructive analytical technique used to identify and determine the concentrations of the elements present in solids, powders and liquids. XRF is capable of measuring all elements from beryllium (atomic number 4) to 30
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uranium (atomic number 92) and beyond (at trace levels, often below one part per million, and up to 100%). Figure 13 depicts the equipment setup and process used for this measurement process. FIGURE 13: DEPICTION OF THE XRF PROCESS 2.2 Mass Balancing 2.2.1 Introduction The primary focus of the sampling and laboratory work done during testing is to generate viable data in order to allow for interpretations and conclusions of the process under investigation. In order to achieve this, the data must fit some predetermined level of quality and accuracy. Test work designed to compare extremely small process variations must be handled in a more controlled fashion than those of a large process simulation. To this end, the level of accuracy needed to draw the desired conclusions from an experiment will dictate the procedures used during sampling and laboratory processing. The usefulness of sampling data as a process-modeling tool is drastically dependent on the quality of the input data. The data used for modeling can come from a number of 31
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different sources, such as human sampling, automated sampling, process outputs, and process inputs. Data collected from these various sampling and testing procedures is quite frequently susceptible to many different forms of errors. While some of these can be attributed solely to human error, others are more innate within the sampling and laboratory processes themselves. These errors have many different underlying causes, but the majority can be characterized as follows: • Statistical Effects • Sampling Procedures • Assay Procedures • Sizing Procedures • Plant Process Fluctuations Due to the innate nature of these errors, various mass balancing programs/models are used within the industry. The purpose of these mass balancing techniques is to generate statistically viable data which remains as close as possible to the actual measured data. The overall procedure for mass balancing is as follows: • Data Collection • Data Analysis • Observation of Data Fit • Statistically Refine Experimental Values The basis for mass balancing algorithms used within industry are compositional differences of the various streams generated by the process equipment. A typical mass balancing routine takes all selected streams and calculates the smallest set of data adjustments required, which in turn make the total data set consistent. Consistency of the 32
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sample data is based on a simple principle, input must equal output. An example of this principle would be that the TiO content entering the CrossFlow must equal the unit’s output 2 of TiO . Information such as this is fundamental throughout the entire mass balancing 2 routine. Consider a process which contains three streams having assays of a, b, and c (where a, b and c may be assays of size, TiO , or any other conserved property specific to the 2 process). A simple schematic of this situation is seen in Figure14. If we assume the flowrate in stream of assay a is 100 tph, then: 100a = x*b + (100 - x)*c where x is the flowrate in stream of assay b, then: x = 100(a-c)/(b-c) The most important aspect of this equation is that there must be some differences between the assay values. If the process where simply a splitter device and the assays remained constant: a = b = c and therefore x = 0/0 which is undefined. Expressed in a different way, values can only be estimated for mass balancing if a process imposes a difference on its product streams. If no difference is imposed, the information obtained by sampling cannot be used to calculate erroneous or missing data. It follows that the most useful properties used for mass balancing are those that generate the largest difference in the process streams sampled. This means that heavy mineral assays work well around a spiral circuit while size analysis works well around a hydrocyclone 33
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circuit. The true ability of a mass balance program lies in its capacity to use a wide range of assays and flowrates over an entire process flowsheet. FIGURE 14: SIMPLE PROCESS DEFINITION FOR MASS BALANCING 2.2.2 Mass Balance Program Design In an effort to better understand and draw statistically viable data from the samples taken during testing, a mass balance spreadsheet was constructed. The spreadsheet designed was written in Microsoft Excel format. It was designed to take user defined sample data and convert it to statistically viable data. The developed mass balance spreadsheet first takes user entered experimental data into the Experimental Values section. This data is then duplicated into the Adjusted Values section. From these values, the relative change and weighted sum of squares are calculated. Several constraints have been entered into the spreadsheet. A total of four constraints dealing with mass, HM tonnage, TiO tonnage, and ZrO tonnage are used in this program. 2 2 These constraints force the output of the system into equaling the input for both mass and assay values. Next, a “solver” routine is used which alters the data in the Adjusted Values section. The goal of this solver routine is to calculate the experimental values needed to meet 34
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Complete mineral composition analysis using XRF analysis was run on each of the individual test runs. Figure 15 shows the various data for these runs. It can be seen that ZrO , zircon, generally maintained higher recoveries than TiO . This phenomenon was 2 2 expected and can be attributed to the higher specific gravity of the zircon grains, 4.7. Rejection of the alumino-silicates, AL O , was typically less than 10%. Alumino-silicates 2 3 are significantly less dense than other heavy minerals, 3.2 – 3.7 specific gravity, and would normally be expected to report to overflow in an elutriation system such as the one tested. These particular heavy minerals, specifically kyanite and sillmanite, have no significant value and must typically be removed during subsequent processing. Removal of this material is another beneficial feature of the proposed elutriation system. The average TiO recovery and ZrO recovery experienced during the test work were 2 2 97.68% and 98.05%, respectively. At these levels of recovery, TiO in the unit feed was 2 upgraded from an average 26.01% to an underflow grade of 31.18%. The average overflow experienced during the testing program was only 2.95% TiO . Although these results are 2 typically better than those achieved by Dunn et al, the same degree of upgrading needs to be achieved while generating an overflow stream less than 2% TiO in order for this project to 2 become industrially feasible. 36
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also scattered in this testing range. It is believed that the +30 mesh quartz present in the feed and underflow causes this scatter of the data. This coarse quartz fraction, known as “rice rock”, is extremely sporadic in quantity and thus difficult to accurately evaluate. Future testing will remove this material prior to laboratory analysis in order to achieve more accurate quartz rejection information. Using the SiO data obtained through XRF analysis, a less sporadic trend can be seen 2 in Figure 16 (B). The only mineral present in the heavy mineral concentrate which contains specific levels of SiO is quartz. However, the SiO data and heavy mineral separation data 2 2 show limited correlation to one another. It is believed that the particular SiO analysis 2 program used during the XRF analysis incorporates silicon readings from other minerals such as staurolite, kyanite, sillminite, and zircon. Therefore, the SiO data obtained from XRF for 2 this test program cannot be used as an accurate indication of quartz content. Although some correlation of SiO to the content of quartz, staurolite, kyanite, sillminite, and zircon can be 2 achieved, it is neither recommended nor needed for this test program. 38
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100 90 80 70 60 50 40 30 20 10 0 0 10 20 30 40 50 60 70 80 90 100 Quartz Rejection (%) 39 tnecreP 100 90 80 70 TiO2 Recovery 60 OverFlow Mass Yield 50 40 30 20 10 0 0 10 20 30 40 50 60 70 80 90 100 SiO Rejection (%) 2 tnecreP TiO2 Recovery OverFlow Mass Yield (A) (B) FIGURE 16: TIO 2 RECOVERY AND OVERFLOW YIELD VERSUS QUARTZ AND SIO 2 REJECTION Further examination of TiO recovery shows a relatively strong trend when compared 2 to overflow mass yield. Although test work was carried out at several different operational settings and feed grades, the data suggests that TiO recovery is directly related to the 2 quantity, or percentage, of material being forced into the unit overflow stream. In order to accomplish the different levels of mass rejection, an operator can manipulate both elutriation flowrate and bed level. Feed grade in terms of heavy mineral content, as seen in Figure 17, also exhibits drastic influence over the percentage of material in the unit overflow. It is plausible for high levels of quartz flowing upward in the test unit toward the overflow to trap
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or entrain large amounts of fine heavy mineral. The majority of these lost heavy minerals, when introduced into an empty elutriation system under the same operational settings, typically would report to the underflow stream. Feed grade, however, is relatively uncontrollable using the testing setup developed for this stage of test work. In order to affect feed grade, drastic changes to the multi-stage wet mill spiral circuit supplying this test setup would be required. Quartz rejection as a function of overflow mass yield gives insight into the size of quartz present in the concentrate. The largest portion of quartz rejection occurs in the initial, lower levels of mass rejection. This phenomenon would tend to describe the easy removal of fine/medium quartz grains. However, as mass rejection increases, the rate of quartz rejection decreases significantly. The medium/coarse quartz remaining in the concentrate becomes increasingly difficult to separate above mass rejections of 20%, resulting in the associated loss of fine heavy minerals such as leucoxene and rutile. It can be stated that the most efficient rejection of quartz occurs were less than 20% mass rejection is desired. Operation above these settings results in significant recovery penalties for both heavy mineral and TiO . 2 40
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a function of these dramatic fluctuations would need to be reduced. A constant recovery above 97% would be a successful achievement under these circumstances. FIGURE 18: CROSSFLOW TIO 2 RECOVERY TIME SERIES PLOT The average heavy mineral feed grade encountered during this stage of test work was 72.57%. This value was much lower than expected, when compared to the plant performance goal of 85%. While some of the lower grades experienced may be due to plant operational conditions, others may be associated with the location of the bypass line feeding the CrossFlow unit. One possibility is that heavy minerals in slurry tend to settle towards the bottom of the flow in a horizontal pipe, making collection of representative unit feed difficult. Another possibility for this lower than expected feed grade might be due to the presence of large amounts of coarse quartz. This coarse material is not considered part of the heavy mineral concentrate assemblage and is typically dry screened before any dry mill 42
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separation occurs. For this reason, future test work will remove this material from heavy mineral determination. Although the feed encountered during test work was lower than expected, the CrossFlow unit was successful in upgrading this material to an average grade of 86.84% heavy mineral. Figure 19 shows trend fit data for the CrossFlow feed and product streams encountered during testing. The average heavy mineral concentrate upgrade produced during the entire testing was 14.27%. The upgrade produced during periods of low feed grade was much more pronounced than during periods of high feed grade. However, during these periods of high upgrading, heavy mineral recovery decreased significantly. This can be attributed to an increase in retention time of the heavy mineral matrix within the unit. Operation under these particular conditions would require decreased unit bed pressure in order to reduce the amount of heavy mineral present in the upper separation zone. These lower grade periods operating at low pressure levels allow a thicker bed of light material to develop within the separation zone. It is also feasible that during periods of high overflow rates, fine heavy mineral particles tend to become trapped in the upward movement of light material being rejected to the overflow stream. It may prove beneficial to unit performance to lower teeter water rates and/or bed levels during these situations, reducing particles caught in carryover and those lost due to increased retention time. 43
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remained in a relatively narrow range. A normal probability plot of the experienced TiO 2 recoveries is shown in Figure 27. The standard deviation of 2.07% for this process was much higher than expected. The probability plot for TiO recovery does not exhibit a typically 2 normal pattern. Few points fall within the 95% confidence intervals predicted by a normal distribution function. There are too many points in the left tail (points above the limits) as well as too many points in the right tail (points above the limits) compared to that of the expected normal distribution function. The Anderson-Darling statistic for this situation is 3.304. This measurement is an interpretation of how far the plot points fall from the fitted line for the probability plot. The statistic is a weighted squared distance from the plot points to the fitted line with larger weights in the tails of the distribution. A smaller Anderson- Darling statistic indicates that the distribution fits the data better. For some limited purposes, assuming a normal distribution for this data would be acceptable. However, an attempt was made to find a better result using six other common distributions including: lognormal base 10, lognormal base e, Weibull, extreme value, exponential, logistic, and loglogistic distributions. Of these distributions, extreme value exhibits the best Anderson-Darling statistic, 1.16. Thus for determining maximum likelihood estimates of the population parameters and percentiles of the distribution for this data, an extreme value distribution should be used. 52
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99 95 90 80 70 60 50 40 30 20 10 5 1 90 95 100 105 Data 53 tnecreP Normal Probability Plot for TiO2 Rec. ML Estimates - 95% CI ML Estimates Mean 97.6848 StDev 2.07446 Goodness of Fit AD* 3.304 FIGURE 27: NORMAL PROBABILITY PLOT FOR TIO 2 RECOVERY A normal probability plot of the experienced HM recoveries can be seen in Figure 28. Standard deviation for this process is slightly higher than the TiO data, 2.72%. The 2 probability plot for HM recovery also does not exhibit a typical normal distribution pattern. The majority of the points fall outside the 95% confidence intervals predicted by a normal distribution. There are too many points in the left tail (points above the limits) as well as too many points in the center (points below the limits) compared to what is expected in a normal distribution function. Assuming a normal distribution for these data would not be acceptable, given the AD value of 4.97. After examining all other typical distributions, it was found that an extreme value distribution gives a slightly better AD value of 3.54. Neither the normal or extreme value distributions appear to accurately predict HM recovery for this test work.
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CHAPTER 3 3.1 Model Development 3.1.1 Overview and Objectives For this particular set of test work, two individual unit models will be developed. The first model is based on numerous empirical equations that together represent the intricacies involved in a CrossFlow elutriation device. This model will allow the reader general understanding of unit operational functions, however, will not attempt to answer or predict exact unit operational outputs. The second model developed will be based entirely from field testing data obtained from a pilot-scale unit. This field data will be input into statistical software, MiniTAB, and used to model the particular pilot-scale unit given the same operational conditions. Data obtained from this model should be able to accurately predict unit operation and allow the reader to properly scale-up a production size unit. The testing program and developments will be discussed later. 3.2 Empirical Modeling 3.2.1 Model Introduction The primary object of the proposed empirical model is to develop a mathematical description of the processes involved within the CrossFlow unit. The goal of the model is to represent the particle size and density within the cell as a function of height, z. This information can then be used to estimate the particle concentrations anywhere within the cell and also determine the concentrations within the overflow and underflow. The proposed model will assume that the unit has been operating at steady state, therefore, the teeter-bed has already been formed. In this case, the initial fluid flow conditions while the bed is 56
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forming will not be required. The proposed model will encompass the entire unit above the elutriation network. Two sections in the model will separate this zone, the area above the teeter-bed and the area below the teeter-bed. A second model for the dewatering cone is not necessary since no settling occurs, velocity is constant, and the feed material entering equals the underflow material exiting. The proposed setup of the model is quite similar to that of the actual CrossFlow unit, as seen in Figure 30. Feed enters through the center of the cell and discharges at the teeter- bed level. The feed material then flows in the positive and negative x directions as separation occurs. Both water and air addition to the cell occurs at the elutriation network level, z = 0. Material that rises, due to low density or attachment to bubbles, reports to the overflow product stream. Material that does not rise, eventually settles into the teeter-bed reports to the underflow via mass-action. 57
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3.2.2 Microscopic Population Balance Model of the CrossFlow Separator Given a general microscopic population balance model as follows: dy d ( ) d ( ) d ( ) (cid:229) J d ( ) • • + v y + v y + vy + vy + D- A = 0 d ( it ) dx ( ii)x dy ( iii)y dz ( iv)z j=1 dz ( vj ) j ( vi) ( vii) where: dy = Accumulation dt d ( ) d ( ) d ( ) v y , v y , vy = Continuous changes due to particle motion dx x dy y dz z (cid:229) J d ( ) v y = Continuous changes in property space dz j j=1 j • D = Disappearance • A = Appearance The assumptions which must be used in order to analyze the population balance are: 1. Two properties of interest; size, d , and density, r . 2. The bank is completely mixed in the y direction. 3. The bank is completely mixed in the x direction. This assumption, although somewhat incorrect, simplifies the preliminary model development. 4. Particle size does not change continuously. 5. No disappearance of particles from one density class or size class to another exists 6. No appearance of particles from one density class or size class to another exists. 7. The cell is operating under steady state conditions. 59
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• Q volume flow rate of water addition at z = 0 w : • Q volume flow rate of underflow at z = 0, same as flow rate through dewatering cone u : d ( ) • f ; volume fraction solids as a function of height, z, within the cell; requires sampling dz at various heights throughout the cell at various flow and feed rates d • Re; Reynolds Number as a function of height, z, within the cell; determination of dz d ( ) f and flow and feed rates will allow calculation of this term dz 3.2.3 Model Conclusions The developed CrossFlow model contains many unknown quantities and functions. While some are relatively simple to calculate, although time consuming, others are much more involved. While the determination of the volume fraction solids and Reynolds numbers as a function of height z within the cell are beyond the scope of this project, it is hoped that an analytical solution to these terms can be achieved in the near future. Use of this model should aid the reader in the general understanding of the CrossFlow unit. However, exact predictions of unit recovery performance and operational settings are outside the range of the particular model developed. Additionally, a unit model that determines conditions without the assumption of complete mixing in the x direction. This assumption makes computation much simpler, however, recent studies by Komuench et al. have shown this assumption to be incorrect. This model enhancement would allow for more realistic model calculations, but requires significantly more computations. 65
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3.3 Statistical Unit Modeling 3.3.1 Response Surface Modeling In order to accurately predict unit performance and determine scale-up information, a more elaborate model for unit operation was required. Statistical modeling of unit operation would allow the precise predictions of unit operational conditions needed for engineering analysis. Response surface modeling techniques were employed through use of statistical software, primarily MiniTAB. These techniques were used throughout the testing and analysis programs. Response surface methods are used to examine the relationship between one or more response variables and a set of quantitative experimental variables or factors. These methods are often used after identification of specific controllable factors has taken place. They are then used to find the particular settings that optimize the response (recovery, rejection, etc.). Response surface designs are usually chosen when curvature, or nonlinear interaction, is suspected within the response surface. Response surface methods are typically employed in order to: • find operating conditions that produce the desired response • find operating conditions that satisfy operating or process specifications • identify new operating conditions that produce demonstrated improvement of the response • develop a model of the relationships between defined operational conditions and the response 66
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Many response surface applications are sequential in nature in that they require more than one stage of experimentation and analysis. The steps shown below are typical of a response surface experiment. • Choose a response surface design for the experiment. • Create a response surface design, central composite or Box-Behnken. • Modify the design by renaming the factors, changing the factor levels, replicating the design, and randomizing the design. • Perform the experiment and collect the response data. • Enter the data into MiniTAB. • Analyze the response surface design in order to fit a model to the experimental data. • Generate wireframe plots in order to visualize response surface patterns. • Optimize the desired responses by using a response optimizer to obtain a numerical and graphical analysis. Depending on the experiment, steps can be performed in different orders, a given step can be performed more than once, or a step can be entirely eliminated. 3.3.2 Response Surface Design Selection Before the use of statistical software, determination of the most appropriate design for the particular experiment is required. Choosing the correct design for a given experiment ensures that the response surface is fit in the most efficient manner. MiniTAB’s software package provides both central composites and Box-Behnken designs. When choosing a design it is most important to: 67
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• Identify the number of factors that are of interest. • Determine the number of test runs physically possible, given time and sampling requirements. • Ensure adequate coverage of the region of interest on the response surface. • Determine the impact that other considerations (such as cost, time, or the availability of facilities) have on your choice of a design. Depending on the particular experiment, there are other considerations that make a particular design most desirable. It is important to use designs that show consistent performance in the criteria considered important, such as the ability to: • Increase the order of the design sequentially. • Perform the experiment in orthogonal blocks. Orthogonally blocked designs allow for model terms and block effects to be estimated independently and minimize the variation in the estimated coefficients. • Rotate the design. Rotatable designs provide the desirable property of constant prediction variance at all points that are equidistant from the design center, thus improving the quality of the prediction. • Detect model lack of fit. Given the requirements of the experiments, a Box-Behnken design was chosen. This particular design can be created as a blocked or unblocked design. The illustration below, Figure 31, shows the general layout of a three-factor Box-Behnken design. The points on the diagram represent the experimental runs that are performed and used for response analysis. Box-Behnken designs are often used when performing non-sequential experiments. That is, planning to perform the experiment only once. These designs allow efficient estimation of 68
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CHAPTER 4 4.1 Pilot-Scale CrossFlow Test Work 4.1.1 Overview The next stage in elutriation testing as an effective heavy mineral upgrade tool began with continuous open circuit testing on a larger pilot-scale CrossFlow. The unit used during this period of testing was installed in the field and arranged for continuous field operation. The unit constructed for this test work had a cross-sectional area of 2’ x 2’. This pilot unit was installed directly in line with the final wet mill concentrate at a Florida mineral sands operation. This particular unit was positioned in the exact feed location as the 4”x16” lab unit previously tested, immediately following the attrition scrub system and prior to dewatering and stacking. It was surmised that scale-up testing using a unit of this size and capacity would generate much more realistic data for any future full-scale installation plans. Although significant modifications were required to functionally install the pilot scale unit, the basic flowsheet remained the same. Figure 32 shows the basic overview of the flowsheet used for pilot-scale operation. Feed material was taken directly from the wet mill final concentrate line and fed to the CrossFlow’s tangential feed box. Two 4” hydrocyclones were used to dewater the feed slurry to the necessary 50-60% solids recommended by the manufacturer. Two additional 4” hydrocyclones and a 7.5 HP pump with a variable speed drive were required in order to transport and stack the underflow process stream. In addition to these ancillary equipment needs, additional steel work was required in order to sustain the weight of the larger unit. 72
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the pilot-scale unit. The hydrocyclones would be fed directly from the bypass feed line installed prior to the full-scale stacker cyclone. As previously stated, pressure and percent solids of this bypass line were incorrect for unit feed conditions for laboratory scale testing. However, installation of the larger feed hydrocyclone would allow for effective operation under these high pressures and low percent solids present. The installed hydrocyclone had been previously tested in-line to determine its operational ability. Minimal loss of fines in the overflow stream was experienced with underflow percent solids reporting in the range of 40–70%. The larger volume of elutriation water required for the pilot unit posed another installation problem. Required flowrates were initially estimated at 8–16 gpm, 2–4 gpm/ft2. The 110 volt chemical pump previously used during lab-scale testing would prove to be inadequate. Instead, a ¾” by 1”, 220 volt pump was installed. This particular pump was fixed speed and capable of supplying 35 gpm under the testing conditions. Initial shakedown testing of the pilot-scale facilities included the use of a RCM Industries fixed aperture flowmeter. However, the fluctuations in flow readings experienced with this model flowmeter were much greater than desired and made precise flowrate changes difficult. Instead, a Cole-Parmer 5000 series variable area flowmeter was installed. This particular meter was a direct reading unit constructed from solid acrylic and was capable of reading flowrates from 0.1 to 20.0 gpm. Product specifications for this model showed an accuracy of 2% full scale, well within the required field. This type of meter makes use of a single calibrated stainless steel float, whose size and weight determines the relative flowrate present within the chamber. The inner chamber containing the float is bored at precise specifications from acrylic to allow for accurate flowrate readings. This particular unit was 75
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well suited for field use due to its high pressure capacity, 100 psi, as well as its high temperature capacity, 150(cid:176) F. Underflow stacking of the high tonnages was also a new issue for the pilot-scale activities to address. Test stand facilities would need to be at least 20 ft in height in order to allow sufficient height for stacking. Instead, unit underflow was directed to a sump pump where it could be sent to stacking equipment. The underflow material, combined with added makeup water, would then be pumped directly to two stacker hydrocyclones. The hydrocyclones chosen for this task were 4” Lynatex models. The small apex diameter of this model would allow for higher underflow percent solids rates. In order to facilitate stacking, a percent solids greater than 65% would need to be created by the new hydrocyclones. Overflow from these units would be sent back to the underflow sump, and thus re-circulate the water. This system would also allow for re-circulation of any fine material that might become misplaced in the overflow streams. Re-circulating this material would increase its probability of reporting to the stacking underflow stream. The sump pump chosen for transport of the unit underflow was a Warman 1.5” by 1” centrifugal pump. The impeller chosen for installation under these particular conditions was constructed of natural rubber in order to reduce capital cost. A 7.5 HP motor capable of reaching speeds of 2000 rpms was also chosen. This equipment setup would allow for ample capacity of the various underflow rates predicted. A variable speed drive unit was installed such that pump rpms could be changed quickly. This arrangement would allow important changes in pump discharge flowrate and pressure, vital to hydrocyclone performance under varying conditions. 76
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The previous microprocessor based fuzzy logic controller operated during lab-scale testing was successfully adapted for use in the new system. However, some minor changes to the program logic were necessary to incorporate this equipment into the new setup. The most difficult aspect of this configuration was the setting of the response rate for the valve operation. As compared to the lab-scale unit, pressure changes in the pilot-scale unit were much slower and required careful programming of the process logic. If the valve response rate were too fast, steady state conditions would never predominate within the unit and successful separation would be quite difficult. In addition to the tangential feed system used by the CrossFlow, a deflection plate was added. This plate forced solids downward into the separation bed. This addition appears to reduce the amount of fine heavy mineral lost to the unit overflow. These particles, having been introduced farther down into the cell, must be forced through significant amounts of material prior to overflow rejection. This development is believed to offer higher levels of TiO recovery than the previous setup. Figure 34 shows the location of the deflection plate 2 within the cell. 77
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4.2 Pilot-Scale Model Test Work Results Test work using the pilot-scale setup was carried out based on the testing program previously described in Chapter 3. A total of 30 test runs were performed in order to extract sufficient information necessary to generate a statistical model for unit operation. Those aspects of the program which were controllable were changed between each test run, those variables not controllable were tracked and recorded. As previously stated, the key operational conditions under examination are feed rate, elutriation flow rate, and bed level. Although not specifically controllable, feed percent solids and feed grade were also tracked for model development. Table VIII shows the actual results experienced during this phase of testing. Sample 22 was removed due to error or mistakes in the sample laboratory analysis. Mass balancing of the test data was performed using the program developed in Chapter 3. Unfortunately, there were excessive tonnage fluctuations experienced for both the overflow and underflow unit streams. Several test runs required relative changes of 50% or more to the overflow and underflow stream tonnage, much too high for the balancing software to make accurate predictions. Reaction rate of the pneumatic underflow valve was attributed as the primary source of these fluctuations. The reaction rate of the valve system forced periodic “purges” in order to maintain bed level at the specified level. Instead of mass balancing, the following common recovery and rejection equations were used for this stage of test work: Concentrate(Feed - Tailings) Recovery = Feed(Concentrate- Tailings) Tailings(Concentrate- Feed) Re jection = Feed(Concentrate- Tailings) 80
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performance. The larger unit capacity and feed arrangement for the pilot unit are believed to have reduced these feed fluctuations quite drastically. Dramatic fluctuations in the feed material would have made test work extremely difficult since the pilot unit had a retention time of approximately 20 minutes, depending on feed rate. Table IX: Average Pilot-Scale Model Testing Results Feed Underflow Overflow Test Runs Ave. TiO Ave. HM Ave. TiO Ave. HM Ave. TiO Ave. HM 2 2 2 30 26.64 76.47 32.63 91.28 2.55 5.87 Ave. Recovery Ave. Rejection TiO HM Quartz 2 97.87 98.42 67.27 Quartz rejection was slightly lower than desired for the testing program. An average rejection of 67.27% was experienced for the entire test program. This phenomenon is explained by the high and low operational conditions used for testing. Certain test designs either had extremely low elutriation flowrates or low bed pressure levels, neither setting being optimal for quartz rejection. Model development from the test work should allow for significant improvement in rejection at similar TiO and Heavy Mineral recoveries. Figures 2 36 and 37 depict the various recoveries as a function of both quartz rejection levels and feed rate. Although limited reduction in TiO recovery occurs for higher feed rates, Heavy 2 Mineral recovery is left completely unaffected. Feed tonnages above 2 tph/ft2 are needed in order to assess the impacts on recovery and quartz rejection. 84
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Although the feed entering the system fluctuated quite drastically, unit underflow remained relatively constant for the entire testing program. Figure 38 shows descriptive statistics for the feed TiO grade. Typical wet mill performance during this phase of testing gave a 2 standard deviation for concentrate grade of 3.0%. Fluctuations in this plant performance are attributed to such things as tonnage shifts in dredging, mechanical sisues and operational errors. Figure 39 shows that the CrossFlow pilot unit was successful in reducing these fluctuations by approximately 44%. Unit TiO output grade averaged 32.63% with standard 2 deviation of 1.68%. This drastic reduction in fluctuation would significantly improve subsequent dry mill processing. Constant output grades would allow dry mill operators to configure plant performance around relatively tight ranges of feed grade, improving overall dry mill recovery and performance. Descriptive Statistics Variable: Feed TiO2 Anderson-Darling Normality Test A-Squared: 0.923 P-Value: 0.016 Mean 26.6432 StDev 3.0041 Variance 9.02447 Skewness -6.3E-01 Kurtosis -6.7E-01 N 28 20 22 24 26 28 30 Minimum 19.7600 1st Quartile 23.9700 Median 27.4000 3rd Quartile 29.4450 95% Confidence Interval for Mu Maximum 30.2900 95% Confidence Interval for Mu 25.4784 27.8081 24.5 25.5 26.5 27.5 28.5 29.5 95% Confidence Interval for Sigma 2.3751 4.0890 95% Confidence Interval for Median 95% Confidence Interval for Median 24.7507 29.1824 FIGURE 38: BASIC STATISTICS FOR UNIT FEED (%TIO 2) 86
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Data from the test program can be analyzed through several techniques. However, for the investigation multiple linear regression is used. This technique allows for model development using the following terms: • linear terms • linear terms and all squared terms • linear terms and all two-way interactions • linear terms, all squared terms, and all two-way interactions (the default) • a subset of linear terms, squared terms, and two-way interactions The model fit chosen will determine the nature of the effects, linear or curvilinear, that can be detected from the experimental data. 4.3.2 Linear Regression Analysis for TiO and HM 2 Based from data in Chapter 2, unit feed grade is known to contribute the vast majority of prediction for unit recovery. Simple linear and polynomial regression are used to determine the extent of feed grade on recovery. This procedure performs regression with linear and polynomial (second or third order) terms of a single predictor variable and plots a regression line through the data. Polynomial regression is one method for modeling curvature in the relationship between a response variable (Y) and a predictor variable (X) by extending the simple linear regression model to include X2 and X3 as predictors. The estimation methods used for this analysis is the least squares approach. The quadratic model developed in Figure 40 appears to provide a good fit to the data for TiO recovery. The R2 indicates that feed grade accounts for 68.9% of the variation in 2 TiO recovery. A visual inspection of the plot reveals that the data are randomly spread 2 88
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interactions present between X variables. MiniTAB provides a matrix plot option that quickly allows the interpretations of these interactions. Any interactions between terms can be seen by the plots through visible trends, either linear, logarithmic, or polynomial. Figure 42 shows the matrix plot developed from % Solids, TPH, GPM, Bed Level, and Feed TiO . 2 In general, there appears no strong interactions involving GPM, Bed Level, and Feed TiO . 2 However, TPH and % Solids does show a relatively strong interaction. This phenomenon is typical for a hydrocyclone feeding arrangement where an increase in tonnage corresponds to an associated increase in discharge percent solids. Using both TPH and % Solids in regression analysis is not advised given this occurrence. Further analysis is needed in order to assess which variable plays a more important role in model development. 69.6325 % Solids 53.8775 6.8875 TPH 4.1025 15 GPM 13 95 Bed Level 93 27.9875 Feed TiO2 23.3825 5 3.8 7 7 5 6 9.6 3 2 5 4.1 0 2 5 6.8 8 7 5 1 3 1 5 9 3 9 5 2 3.3 8 2 25 7.9 8 7 5 FIGURE 42: MATRIX PLOT ANALYSIS OF X INTERACTIONS FOR TIO 2 91
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In order to assess the use of either % Solids or TPH, regression analysis using the best subset tool was used. The best subsets output from MiniTAB can be seen in Table X. Each line of the output represents a different model comprised of different variables or predictors. The predictors used in each model are indicated by use of an X in the table. From this data, it can be clearly seen that Feed TiO accounts for as much as 62.4% of the predictive model. 2 GPM also plays an important role with a R-sq(adj) value of 25.0. Since % Solids and TPH cannot both be used for model development, this table allows for understanding as to which factor plays a larger role in model development. If the model where to be developed using % Solids, GPM, Bed Level, and Feed TiO , the model fit would be 83.2% R-sq(adj). If TPH is 2 added to the model and % Solids dropped, the fit remains 83.9%. For further modeling development, TPH will be used instead of % Solids. In the design of a full-scale unit, TPH plays a much larger role by determining the exact unit cross-sectional area needed for the intended feed tonnages. It is important to note that the TPH term used for analysis is not entirely independent and will consist of a TPH portion and an associated % Solids portion. 92
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Table X: Best Subsets Regression for TiO Recovery 2 93 % Solids TPH GPM Bed Level 2 Feed TiO Vars R-Sq R-Sq(adj) C-p S 1 64.0 62.4 30.1 0.74843 X 1 28.1 25.0 81.0 1.05740 X 2 84.7 83.3 2.8 0.49960 X X 2 66.3 63.3 28.8 0.73996 X X 3 85.8 83.8 3.2 0.49213 X X X 3 85.5 83.5 3.5 0.49656 X X X 4 86.6 83.9 4.0 0.48956 X X X X 4 86.0 83.2 4.8 0.49985 X X X X 5 86.6 83.1 6.0 0.50212 X X X X X Multiple regression analysis of TiO recovery began by using a quadratic model that 2 uses linear, square, and interaction terms. Each square or interaction term that displays a p- value greater than 0.05 is removed from the model. Although the linear term Feed TiO 2 exhibits a p-value greater than 0.05, it was left in the model based on its influence in the interaction term TPH x Feed TiO . It can be seen from Table XI that the R-sq(adj) value for 2 the regression model developed is 83.3%. Based on the coefficients and terms used, equation [3] represents the best-fit model for the given pilot-scale test work. This equation will most likely display curvature for some settings due to the inclusion of the square term TPH2 and the interaction term TPH x Feed TiO . 2
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Table XI: Estimated Regression Coefficients for TiO Recovery 2 Term Coef SE Coef T P Constant 98.883 11.578 8.541 0.000 TPH -0.079 0.0684 -1.161 0.260 GPM -0.362 0.0679 -5.336 0.000 Bed Level -0.104 0.0796 -1.310 0.206 Feed TiO 0.783 1.0196 0.768 0.452 2 Feed TiO 2 -0.009 0.0195 -0.461 0.650 2 S = 0.4995 R-Sq = 86.8% R-Sq(adj) = 83.3% TiO Recovery = 98.883 – 0.079(TPH) – 0.362(GPM) – 0.104(Bed Level) 2 + 0.783(Feed TiO ) - 0.009(Feed TiO )2 [3] 2 2 Regression analysis for the unit Output TiO began through the same process. Full 2 quadratic terms were first used for the model, then select terms were removed which possessed p-values less than 0.05. However, the use of several terms containing high p- values was necessary in order to create a model that showed an acceptable relative fit. Removal of these terms forced the overall fit, R-sq(adj), below the 84.2% value and also generated higher residual values. Leaving these terms in allows for a better fit of the model to the actual test data, however, will not accurately predict a model for a larger population of test work. This predictive equation displayed in Table XII can be used to predict the Output TiO for the specific testing data observed, however, will not accurately predict a continued 2 testing population. Equation [4] represents the predicted Output TiO based on TPH, GPM, 2 Bed Level, and Feed TiO . Running a 3rd replicate of the testing series would allow the 2 model to base its fit off more substantial information and improve the overall population prediction. 94
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these outputs given various inputs. Displayed are two overlaid contour plots on a single graph. The two factors, Feed TiO and GPM, are used as the two axes in the plots and the 2 third and fourth factors, TPH and Bed Level, have been held at levels 6.0 and 94 respectively. The white area inside each plot shows the range of Feed TiO and GPM where 2 the criteria for both response variables are satisfied. Responses used for this specific graph are a TiO recovery above 98% and an Output TiO above 33%. This plot, in combination 2 2 with the predictive models, can be used to find the best operating conditions for maximizing recovery and output grade. To achieve these process outputs, feed grade entering the unit can drop to as low as 27%. The ideal GPM for this situation is 14 GPM, as displayed by the graph. This elutriation flowrate allows for the upgrading of the lower feed TiO grades while 2 outputting the proper responses previously described. 97
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4.3.4 Multiple Regression Analysis for HM The first step in multiple regression analysis for heavy mineral recovery and output grade is to determine the various interactions present between X variables. The same process as for TiO is used, generation of a matrix plot through use of MiniTAB. This graph allows 2 quick interpretations of these interactions for the variables selected. Figure 45 shows the matrix plot developed from % Solids, TPH, GPM, Bed Level, and Feed HM. In general, there appears no strong interactions involving GPM, Bed Level, and Feed HM. However, TPH and % Solids again show a relatively strong interaction. Thus, using both TPH and % Solids in the regression analysis for heavy mineral is not advised given this occurrence. Further analysis is needed in order to assess which variable plays a more important role in model development, TPH or % Solids. 69.6325 % Solids 53.8775 6.8875 TPH 4.1025 15 GPM 13 95 Bed Level 93 80.575 Feed HM 65.965 99.09 HM Rec 97.35 53.8 7 75 6 9.63 2 5 4.1 0 25 6.8 87 5 1 3 1 5 9 3 9 5 6 5.9 65 8 0.57 5 9 7.3 5 9 9.0 9 FIGURE 45: MATRIX PLOT ANALYSIS OF X INTERACTIONS FOR HM 99
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In order to assess the use of either % Solids or TPH, regression analysis using the best subset tool was used. The best subsets output from MiniTAB can be seen in Table XIII. Each line of the output represents a different model comprised of different variables or predictors. The predictors used in each model are indicated by use of an X in the table. From this data, it can be clearly seen that Feed HM accounts for as much as 68.3% of the predictive model. GPM also plays an important role with a R-sq(adj) value of 15.6. Since % Solids and TPH cannot both be used for model development, this table allows for understanding as to which factor plays a larger role in model development. If the model where to be developed using TPH, GPM, Bed Level, and Feed HM, the model fit would be 87.3% R-sq(adj). If % Solids is added to the model and TPH dropped, the fit drops slightly to 86.6%. For further modeling development using heavy mineral analysis, TPH will be used instead of % Solids. However, initial observation using the best subsets regression information shows that GPM, Bed Level, and Feed HM account for a R-Sq(adj) value of 87.2. Based from this information, TPH does not appear to make a significant influence on the model, although further analysis is needed. 100
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Table XIII: Best Subsets Regression for HM Recovery 101 % Solids TPH GPM Bed Level Feed HM Vars R-Sq R-Sq(adj) C-p S 1 69.8 68.3 29.4 0.62575 X 1 19.6 15.6 108.3 1.02090 X 2 88.3 87.1 2.4 0.39982 X X 2 70.6 67.5 30.2 0.63376 X X 3 89.1 87.2 3.2 0.39720 X X X 3 88.9 87.0 3.5 0.40029 X X X 4 89.7 87.3 4.1 0.39574 X X X X 4 89.2 86.6 5.0 0.40684 X X X X 5 89.8 86.6 6.0 0.40630 X X X X X Multiple regression analysis of HM recovery began by using the same quadratic model as for TiO . This model uses linear, square, and interaction terms to develop a 2 predictive model of unit operation. Each square or interaction term that displays a p-value greater than 0.05 is removed from the model. Through this process, the TPH linear, square, and interaction terms were determined to play no significant role in the overall model. Also, during this analysis, test runs #7, 18, 23, and 28 were removed for their excessive residuals based from the developed model. The error in these points is either the development of laboratory analysis error or field test work error. Removal of these data points both increase overall model fit and reduces the average residual value for the test work. It can be seen from Table XIV that the R-sq(adj) value for the regression model developed is 95.1%. Based on the coefficients and terms used, equation [5] represents the best-fit model for the given pilot-scale test work. This equation will most likely display curvature for some settings due
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to the inclusion of the square term Feed HM and the interaction terms GPM x Feed HM and Bed Level x Feed HM. Table XIV: Estimated Regression Coefficients for HM Recovery Term Coef SE Coef T P Constant 249.717 53.4195 4.675 0.000 GPM -2.783 0.436 -6.384 0.000 Bed Level -1.464 0.5906 -2.479 0.024 Feed HM -1.436 0.6039 -2.377 0.029 Feed HM2 -0.003 0.0012 -2.228 0.040 GPM x Feed HM 0.031 0.0055 5.634 0.000 Bed Level x Feed HM 0.016 0.0073 2.247 0.038 S = 0.2367 R-Sq = 96.4% R-Sq(adj) = 95.1% HM Recovery = 249.717 – 2.783(GPM) – 1.464(Bed Level) – 1.436(Feed HM) – 0.003(Feed HM)2 + 0.031(GPM x Feed HM) + 0.016(Bed Level x Feed HM) [5] Regression analysis for the unit Output HM began through the same process. Full quadratic terms were first used for the model, then select terms were removed which possessed p-values less than 0.05. All terms remaining contain extremely low p-values which represents a relatively high influence from each factor on the developed model. Besides linear terms, the square term Feed HM and the interaction term TPH x Feed HM were left in the model analysis. Unlike the HM recovery regression analysis, TPH and its square and interaction terms play significant roles in unit output HM grade. In addition to those test runs removed in the HM recovery analysis, test runs #9 and 15 were also removed for their high residual values relative to the developed model. Table XV shows the regression analysis information given the specific test runs and terms used in its 102
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development. An R-sq(adj) value of 92.1% was achievable under the given circumstances. Equation [6] represents the predicted Output HM based on TPH, GPM, Bed Level, and Feed HM. Running a 3rd replicate of the testing series would allow the model to base its fit off more substantial information and improve the overall population prediction. Table XV: Estimated Regression Coefficients for Output HM Grade Term Coef SE Coef T P Constant -18.000 33.96 -0.530 0.604 TPH 24.060 5.1928 4.634 0.000 GPM 2.150 0.1922 11.165 0.000 Bed Level -0.580 0.1993 -2.922 0.011 Feed HM 1.360 0.3003 4.528 0.000 TPH2 -0.980 0.1562 -6.296 0.000 TPH x Feed HM -0.170 0.0482 -3.525 0.003 S = 1.283 R-Sq = 94.4% R-Sq(adj) = 92.1% HM Output = -18.000 + 24.060(TPH) + 2.150(GPM) – 0.580(Bed Level) + 1.360(Feed HM) – 0.980(TPH)2 – 0.170(TPH x Feed HM) [6] In order to understand the HM recovery equation developed, graphical analysis is needed. To examine more than two interactions a 3-D surface plot is used. Figure 46 shows one such contour plot where Feed HM and GPM are used as the X and Y variables, while HM recovery is used as the Z value. For this particular instance, Bed Level is held at 94 and TPH is not used. It can be seen that GPM displays a relatively linear relationship with HM recovery. If significantly lower and higher water rates are used, this model would most likely display curvature for HM recovery as a function of GPM. However, the flowrates used in the model test work are relatively close which makes linear regression the only 103
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Figure 47 is one such contour plot for these outputs given various inputs. Displayed are two overlaid contour plots on a single graph. The two factors, Feed HM and GPM, are used as the two axes in the plots and the third and fourth factors, TPH and Bed Level, has been held at levels 6.0 and 94 respectively. The white area inside each plot shows the range of Feed HM and GPM where the criteria for both response variables are satisfied. Responses used for this specific graph are a HM recovery above 98% and an Output HM above 90%. This plot, in combination with the predictive models, can be used to find the best operating conditions for maximizing recovery and HM output grade. To achieve these process outputs, feed grade entering the unit cannot drop below approximately 72% HM. The ideal GPM for this situation is 14 GPM, as displayed by the graph. This elutriation flowrate allows for the upgrading of the lower Feed HM grades while outputting the proper responses previously described. 105
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4.5 Economic Analysis As previously stated, installation of a CrossFlow unit has several economic advantages. The largest financial incentive is the reduction of haulage requirements to the dry mill facilities. This material also carries an additional tailings haulage necessary for zircon retrieval. The cost of haulage to the dry mill facility and zircon wet mill facilities are estimated at $1.75 and $2.50 per ton of concentrate, respectfully. Given a yearly plant production of 355,000 tons of concentrate, a reduction in haulage of 10% would result in annual variable cost savings of $150,875. This system also saves the cost of drying unnecessary material in the dry mill facilities. These costs are estimated at $1.50 per ton of feed material. A 10% reduction of material needing drying would thus result in annual variable cost savings of $53,250. This calculation does not take into account any maintenance costs associated with drying wet mill concentrate, only the cost of fuel consumption. Installation costs of the proposed system is estimated at $200,000. This cost includes construction of the CrossFlow unit, necessary support structures, electrical services, water services, and engineering fees. Assuming no added variable cost for the proposed system, capital cost of $200,000 and yearly savings of $204,125 the Internal Rate of Return (IRR) of this project is estimated at 75% with a Net Present Value (NPV) of $372,897. Total economic calculations, including taxes, depreciation, and depletion, can be seen in Table XVI. This economic exercise used a tax rate of 38% with the typical graduated depreciation rates over 5 years. 109
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CHAPTER 5 Conclusions Lab/pilot-scale testing was accomplished using a 4” x 16” CrossFlow unit in continuous field operation. The primary goal of this test work was to evaluate the feasibility of using elutriation technology for heavy mineral concentration. These tests were carried out for numerous feed grades and tonnages. Various operational parameters were also examined during these tests. As previously stated, the feed material used was from a mineral sands operation in northern Florida. The results achieved from this testing program are as follows: • Quartz rejections greater than 80% were possible under certain operational conditions. TiO recoveries at these rejection levels were above 95%. 2 • Elutriation flowrates were reduced to as low as 2 gpm/ft2 under certain conditions. This reduction allows for significant savings of fresh water required for unit operation. • Use of a deflection plate showed significant recovery/rejection improvement over the typical CrossFlow feed arrangement. • Feed tonnages as high as 1.5 tph were successful in achieving the testing goals. This allows for reduced unit size and cost. Pilot scale testing was accomplished using a 2’ x 2’ CrossFlow unit in continuous field operation. These tests were carried out for numerous feed grades, tonnages, elutriation flow rates and bed levels. The results achieved from this testing program are as follows: 111
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• Quartz rejections greater than 80% were possible under many different operational conditions. TiO recoveries at these rejection levels were 2 approximately 98%. • Elutriation flow rate was optimized to 14 gpm, 3.5 gpm/ft2, for several operational conditions. • Use of a deflection plate showed significant recovery/rejection improvement over the typical CrossFlow feed arrangement. • Feed tonnages as high as 1.5 tph were successful in achieving the testing goals. This allows for reduced unit size and cost. • Standard deviation for the wet mill concentrate TiO grade was reduced from 2 3.0% to 1.68% Along with experimental testing, both empirical and statistical models for unit operation were developed. Given a feed grade of 28% TiO and a feed rate of 70 tph for full-scale 2 operation, the statistical model was successful in determining the following: • A minimum elutriation flow rate of 245 gpm (3.5 gpm/ft2) would allow for successful quartz rejection. • A feed rate of 1.5 tph/ft2 could be used to achieve successful unit results. This tonnage requires the use of a 47 ft2 CrossFlow unit. A typical 7’ x 7’ square configuration would achieve the proper cross-sectional feed rate. • An overall quartz rejection of 80% with a TiO recovery of 98% is possible for 2 these particular unit operational conditions. 112
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CHAPTER 6 Recommendations for Future Work Improve Performance of Hindered-Bed Classifiers for Heavy Mineral Separations. 1. Laboratory testing focusing on optimal settings for the added baffle plate are needed in order to better understand this item’s impact on unit performance. It is recommended that this baffle plate be set at various heights and distances from the feed presentation system to accomplish this task. 2. Full-scale installation of a CrossFlow unit in order to achieve the benefits previously mentioned within this report. Elaborate testing would be needed for this application to achieve the highest possible success. This testing should be used in order to generate model information that could be used by operators for precise field operation. Improved Rejection of Fine TiO from Zircon Wet Mill Concentrate. 2 1. Conducting testing to investigate the possible benefits of using elutriation technology in order to clean zircon wet mill concentrate. This particular concentration is comprised mainly of zircon, ilmenite, leucoxene, rutile, kyanite, sillmanite, and staurolite. This separation would be quite difficult given the near density of minerals such as ilmenite, 3.7, to the zircon product, 4.7. 113
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10/4/2015 VT Fair Use Analysis Results Draft 09/01/2009 (Questions? Concerns? Contact Gail McMillan, Director of the Digital Library and Archives at Virginia Tech's University Libraries: [email protected]) (Please ensure that Javascript is enabled on your browser before using this tool.) Virginia Tech ETD Fair Use Analysis Results This is not a replacement for professional legal advice but an effort to assist you in making a sound decision. Name: Scott Koermer Description of item under review for fair use: T.P Meloy, D.A Whaley, M.C Williams, Flotation tree analysis — reexamined, International Journal of Mineral Processing, Volume 55, Issue 1, October 1998, Pages 21-­39, ISSN 0301-­ 7516, http://dx.doi.org/10.1016/S0301-­7516(98)00023-­4. Report generated on: 10-­04-­2015 at : 14:37:31 Based on the information you provided: Factor 1 Your consideration of the purpose and character of your use of the copyright work weighs: in favor of fair use Factor 2 Your consideration of the nature of the copyrighted work you used weighs: in favor of fair use Factor 3 Your consideration of the amount and substantiality of your use of the copyrighted work weighs: in favor of fair use Factor 4 Your consideration of the effect or potential effect on the market after your use of the copyrighted work weighs: in favor of fair use in Based on the information you provided, your use of the copyrighted work weighs: favor of fair use http://etd.vt.edu/fairuse/analyzer/results.php 1/2
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10/4/2015 VT Fair Use Analysis Results Draft 09/01/2009 (Questions? Concerns? Contact Gail McMillan, Director of the Digital Library and Archives at Virginia Tech's University Libraries: [email protected]) (Please ensure that Javascript is enabled on your browser before using this tool.) Virginia Tech ETD Fair Use Analysis Results This is not a replacement for professional legal advice but an effort to assist you in making a sound decision. Name: Scott Koermer Description of item under review for fair use: Zhang, S., Forssberg, B.A., Moss, W., 1999. “Separation Mechanisms and Criteria of a Rotating Eddy-­Current Separator Operation” Resources, Conservation and Recycling, Vol. 25, No. 3-­ 4, pp. 215-­232.0301-­7516, http://dx.doi.org/10.1016/S0301-­7516(98)00023-­4. Report generated on: 10-­04-­2015 at : 14:38:30 Based on the information you provided: Factor 1 Your consideration of the purpose and character of your use of the copyright work weighs: in favor of fair use Factor 2 Your consideration of the nature of the copyrighted work you used weighs: in favor of fair use Factor 3 Your consideration of the amount and substantiality of your use of the copyrighted work weighs: in favor of fair use Factor 4 Your consideration of the effect or potential effect on the market after your use of the copyrighted work weighs: in favor of fair use in Based on the information you provided, your use of the copyrighted work weighs: favor of fair use http://etd.vt.edu/fairuse/analyzer/results.php 1/2
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10/4/2015 VT Fair Use Analysis Results Draft 09/01/2009 (Questions? Concerns? Contact Gail McMillan, Director of the Digital Library and Archives at Virginia Tech's University Libraries: [email protected]) (Please ensure that Javascript is enabled on your browser before using this tool.) Virginia Tech ETD Fair Use Analysis Results This is not a replacement for professional legal advice but an effort to assist you in making a sound decision. Name: Scott Koermer Description of item under review for fair use: Wilson, R.J., T.J. Veasey, D.M. Squires, The application of mineral processing techniques for the recovery of metal from post-­consumer wastes, Minerals Engineering, Volume 7, Issue 8, August 1994, Pages 975-­984, ISSN 0892-­6875, http://dx.doi.org/10.1016/0892-­6875(94)90027-­2. Report generated on: 10-­04-­2015 at : 14:28:39 Based on the information you provided: Factor 1 Your consideration of the purpose and character of your use of the copyright work weighs: in favor of fair use Factor 2 Your consideration of the nature of the copyrighted work you used weighs: in favor of fair use Factor 3 Your consideration of the amount and substantiality of your use of the copyrighted work weighs: in favor of fair use Factor 4 Your consideration of the effect or potential effect on the market after your use of the copyrighted work weighs: in favor of fair use in Based on the information you provided, your use of the copyrighted work weighs: favor of fair use http://etd.vt.edu/fairuse/analyzer/results.php 1/2
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PUBLISHERS OF: Recycling Today magazine Recycling Today Global Edition magazine Construction & Demolition Recycling magazine Plastics Recycling magazine Renewable Energy from Waste magazine Equipment & Services Buyers’ Guides Recycling Markets Directories Mr. Scott Koermer Virginia Polytechnic Institute and State University Blacksburg, VA Scott, Thank you again for your contributed article “Gauging yield and recovery,” which was published in the September/October issue of Recycling Today Global Edition magazine. Please be assured that you have our company’s permission to use your drafted article, or the article in any other form, as part of a submitted thesis. Should you need to access the published version of the article, in can be found here: http://www.recyclingtodayglobal.com/article/rtge0915-shredded-scrap-separation-performance and starting on page 34 of the digital editon of the magazine, which can be found here: http://www.recyclingtodayglobal.com/fileuploads/digital-editions/rtge/digital/20150910/index.html . Please let me know if you need any additional proof of permission from Recycling Today Media Group or its parent company GIE Media, and best of luck in organizing a successful thesis! Respectfully Yours, Brian Taylor, Editor, Recycling Today Media Group 5811 Canal Road / Valley View, Ohio 44125 Phone: 800-456-0707 / Fax: 216-525-0515 www.RecyclingToday.com www.CDRecycler.com / www.SDBmagazine.com PROVIDING INDUSTRY RESOURCES SINCE 1963.
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IDENTIFICATION OF IMPROVED STRATIGIES FOR PROCESSING FINE COAL by Zulfiqar Ali ABSTRACT In modern coal preparation plants, solid-solid and solid-liquid separation processes used to treat fine coal are least efficient and most costly operations. For example, field studies indicate that the froth flotation process, which is normally used to treat minus (-0.2 mm) fine coal, often recovers less than 65 to 70% of the organic matter in this size range. Fine coal separation processes are also inherently less effective in removing pyrite than that of coarse coal separations. Moreover, while fines may represent 10% or less of the total run-of-mine feed, this size fraction often contains one-third or more of the total moisture in the delivered product. In order to address these issues, several multistage coal processing circuits were set up and experimentally tested to demonstrate the potential improvements in fine coal upgrading that may be realistically achievable using an “optimized” fine coal processing flowsheet. On the basis of results obtained from this research, engineering criteria was also developed that may be used to identify optimum circuit configurations for the processing different fine coal streams. In the current study, several fine coal cleaning alternatives were evaluated in laboratory, bench-scale and pilot-scale test programs. Fine coal processes compared in the first phase of this work included spirals, water-only cyclones, teeter-bed separators and froth flotation. The performance of each technology was compared based on separation efficiencies derived from combustible rejection versus ash rejection plots. The resulting data was used to identify size ranges most appropriate for the various alternative processes. As a follow-up to this effort, a
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second phase of pilot-scale and in-plant testing was conducted to identify new types of spiral circuit configurations that improve fine coal separations. The experimental data from this effort indicates that a four-stage spiral with second- and fourth-stage middlings recycle offered the best option for improved separation efficiency, clean coal yield and combustible recovery. The newly developed spiral circuitry was capable of increasing cumulative clean coal yield by 1.9 % at the same clean coal ash as compared to that of achieved using existing conventional compound spiral technology. Moreover, the experimental results also proved that slurry repluping after two turns is not effective in improving separation performance of spiral circuits. The third phase of work conducted in this study focused on the development of methods for improving the partitioning of pyrite within fine coal circuits. The investigation, which included both laboratory and pilot-scale test programs, indicated that density-based separations are generally effective in reducing sulfur due to the large density difference between pyrite and coal. On the other hand, the data also showed that sulfur rejections obtained in froth flotation are often poor due to the natural floatability of pyrite. Unfortunately, engineering analyses showed that pyrite removal from the flotation feed using density separators would be impractical due to the large volumetric flow of slurry that would need to be treated. On the other hand, further analyses indicated that the preferential partitioning of pyrite to the underflow streams of classifying cyclones and fine wire sieves could be exploited to concentrate pyrite into low- volume secondary streams that could be treated in a cost effective manner to remove pyrite prior to flotation. Therefore, on the basis of results obtained from this experimental study, a combined flotation-spiral circuitry was developed for enhanced ash and sulfur rejections from fine coal circuits. iii
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ACKNOWLEDGEMENTS It is my pleasure to acknowledge everyone who contributed directly or indirectly to complete this research work. First of all, my special thanks to my research advisor, Dr. Jerry Luttrell, who was always there for guidance, suggestions, help, support and encouragement during my research work at Virginia Tech. Jerry, it was an honor for me to work with you and there is no doubt in saying that this work would not have been possible without you. I am also truly indebted and thankful to my respected committee members, Dr. Greg Adel, Dr. Emily Sarver and Dr. Jaisen Kohmuench for their valuable comments, suggestions and advices. During my experimental work, Bob Bratton was there to help whenever I was stuck. Thank you Bob, for your invaluable help and suggestions to improve my research work. My thanks and appreciation was due to Jim Waddell and John Matherly for their invaluable help during experimental set up. Special thanks are due to Kathryn Dew, Carol Trutt and to Gwen Davis for their administrative assistance throughout my graduate studies. I would like to thank Alpha Natural Resources, Arch Coal, Inc. and their employees for assisting in my in-plant experimental testing programs. I am also obliged to the management and employees of Cardinal, Knight Hawk, Prairie Eagle and Creek palm preparation plants for providing much needed fine coal samples for my experiments. Appreciation is also extended to Eriez Manufacturing for their assistance during teeter-bed and HydroFloat™ testing. The financial support provided by the University of Engineering and Technology, Lahore, Pakistan and Taggarat Global LLC and Nano Drying Technologies LLC is greatly acknowledged. I would also like to thank many friends for their nice company throughout my stay in Blacksburg namely Jawad Raza, Imran Akhtar, Shamim Javid, Arshad Mehmood, Karim Akhtar, vi
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CHAPTER 1 - INTRODUCTION 1.1 Motivation Coal is one of the most abundantly available energy sources in the world and is found almost in every country. The top five largest proven reserves of coal are in the United States, Russia, China, Australia and India, respectively. Table 1.1 shows the distribution of proven coal reserves. Currently, there are over 860 billion tonnes of proven coal reserves. In 2010, world coal consumption grew by 7.6% and now coal accounts for 29.6% of world total energy, 40% of world electricity and 66% of world steel production (BP, 2011). The United States leads the world with a little over 237 billion short tons of recoverable coal reserves, i.e., approximately 27.6% of the total world coal reserves. It is estimated that at the current production rate of 984.6 million tonnes per year (USEIA, 2010), the U.S. reserves would last for 240 years. Coal is the largest single fuel used for electricity generation in the U.S. and accounts for 42% of electric power generation. Since 2000, about 90% of all the coal consumed in U.S. has been used for electric power generation as shown by Figure 1.1. Run-of-mine coal often contains inorganic impurities in the form of mineral matter. The mineral matter consists of noncombustible materials such as shale, slate and clay. These unwanted contaminants reduce the coal heating value, leave behind an undesirable ash residue, and increase the transporting cost of coal. These impurities can also alter the suitability of coal for the manufacture of metallurgical coke or generation of petrochemicals and synthetic fuels. 1
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100 90 80 70 60 50 40 30 20 10 0 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010 Excess surface moisture also reduces the heating value of coal, leads to severe handling and freezing problems and increases the overall transportation costs of coal to consumer sites (Kaytaz et al., 1994). Therefore, strict limitations on the heating value, ash and moisture contents of purchased coal are imposed in coal purchasing agreements. Coal processing is an important step to satisfy the run-of-mine coal quality specifications as per end-user demand. Coal processing also removes impurities such as sulfur and trace elements like mercury, thus cleaned coal is more environmentally friendly. In short, coal processing increases the heating value, lowers the transport cost, reduces the particulate emissions and improves the marketability of the run-of-mine coal. There are 286 coal processing plants in the United States, which cleaned approximately 67% (660 million short tons per year) of the total coal consumed in the United States (Coal Age, 2010). )%( noitpmusnoC laoC Year Electric Power Coke Plants Other Industrial Residental & Commercial Figure 1.1 Coal consumption by sectors from 2000 to 2010 (US EIA, 2011). 2
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Although not shown in Figure 1.2, coal processing usually starts with crushing, i.e., run-of-mine coal lumps that are too large to pass through the processing plant are crushed down to an appropriate size. The crushed coal is then separated into appropriate size fractions as coarse, small, fine and ultrafine. Screens are employed for sizing coarser particles, while combinations of sieves and classifying cyclones are used for sizing finer particles. Figure 1.3 shows coal particles sizing equipment for various size ranges. The objective of coal processing is to separate impurities from valuable carbonaceous material. In order to remove these impurities, modern coal processing plants incorporate a number of solid-solid separation methods such as dense medium vessels, water-only cyclones, teeter bed separators, coal spirals and froth flotation. Figure 1.3 shows the effectiveness of different types of conventional coal cleaning separators relative to the coal particles sizes. The final step of coal preparation is solid-liquid separation, or dewatering, which removes unwanted surface moisture and produces a relatively dry concentrate. Dewatering methods are broadly classified in to three main groups: sedimentation, filtration and thermal drying (Wills & Napier-Munn, 2006). Primarily screens are used to remove excess moisture from coarser (+5 mm) coal particles. Finer particles, which used to have higher moisture contents than that of coarser ones due to their greater surface area, are dewatered using centrifugal methods or filtration systems (Luttrell et al., 2007). Figure 1.3 shows several different types of mechanical dewatering methods for different ranges of particle sizes. 5
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Figure 1.3 Range of coal particle sizes that can be effectively treated by conventional coal processing methods (Luttrell, 2012). 1.2 Problem Statement The solid-solid and solid-liquid separation processes used to treat fine (-1 mm) coal are the least efficient and most costly operations used in modern coal processing facilities (Figure 1.4). Field studies indicate that the froth flotation process, which is normally used to recover coal finer than 0.1-0.2 mm, often recover less than 65 to 70% of the organic matter in this size range. Moreover, this surface based separation process is inherently less effective in removing pyrite than density based separation processes used to treat coarse coal. The lower particle size that can be effectively treated by water based density separators is severely limited by the low mass of small particles. Moreover, fines often represent 10 percent or less of the total run-of-mine feed. However, this size fraction may contain one third or more of the total moisture of the delivered 6
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well as various types of surface-based separators such as conventional or column flotation machines. In many cases, the separation processes are used in multistage circuits and are integrated with various types of classification operations either before or after the cleaning step. In addition to technical and economic reasons, operator preferences and vendor biases also appear to contribute to the large variations that are observed in how fine coal is cleaned and dewatered. As a result, a standard “optimum” flowsheet for fine coal processing, which can be flexible and adaptable to accommodate changes in feed coal characteristics, does not exist at this time. 1.3 Research Objectives The objective of this research is to develop an engineering criterion that can be used to identify optimum circuit configurations for the processing of fine coal streams. This dissertation describes several potential improvements in fine coal processing circuitry. Several multistage circuits, including laboratory, bench-scale, pilot scale-and in-plant test circuits, were set up and tested to demonstrate the potential improvements in fine coal recovery that may be realistically achievable using an “optimized” fine coal processing flowsheet. This research work also focused on the development, testing and evaluation of a modified compound spiral to treat fine coal feedstocks. A new combined flotation-spiral circuitry for desulfurization of high sulfur fine coal was also developed and experimentally tested. Finally, this research work also evaluated an innovative fine coal dewatering technique called Nano Drying Technology (NDT™). This innovative process is capable of physically removing moisture from fine coal at ambient temperature using molecular sieve technology. 8
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1.4 Contributions The key contributions of this research and development work are as follows: • Developed an improved fine coal processing circuitry based on feed size characteristics. • Developed an expanded stage compound spiral circuit (4-3-4-3 turn spiral circuit with second and fourth stage middlings recycle). • Developed a new and innovative enhanced fine coal sulfur rejection circuit using combined spiral-flotation circuitry. • Evaluated the effectiveness of a new low-temperature fine coal drying process. 1.5 Dissertation Organization This dissertation is composed of seven chapters. The first chapter “Chapter 1 - Introduction” provides an introduction to the research topic, a detailed problem statement and a listing of research objectives. The second chapter “Chapter 2 - Literature Review” is a brief report on current status of research on fine coal processing. Specifically, this chapter describes in detail the research and developments in coal spiral technology (i.e., history, construction, design variables and operating variables). A brief introduction of several other fine coal processing separators used in this research work is also included in the literature review. The next four chapters focus on the experimental testing and engineering evaluation of various new approaches for fine coal cleaning and dewatering. The first of these chapters “Chapter 3 - Performance Comparison of Fine Coal Cleaning Alternatives” discusses all the laboratory-scale and pilot-scale test results obtained from the detailed testing of common technologies used to clean fine coal (i.e., spirals, teeter bed separators, water-only cyclones and froth flotation). The resultant data suggest, for the particular coal investigated in this study, that the most effective processes for each size range were generally (i) froth flotation for feeds finer 9
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than about 0.3 mm, (ii) spirals for feeds sized to 1 x 0.3 mm, and (iii) teeter-bed systems (particularly the HydroFloat™ technology) for feeds larger than 1 mm. Water-only cyclones are not recommended as stand-alone units due to the potential for high coal losses when secondary back-up units are not available within the plant circuitry. The next chapter “Chapter 4 - Engineering Development of Expanded Stage Compound Spiral” provides results of field tests conducted with a prototype compound spiral that was modified to improve coal recovery and enhance the selectivity of fine coal processing. Detailed in-plant experimental tests results, along with separation performance data comparisons, are presented in this chapter for five different spiral circuit configurations. The performance comparison indicates that, amongst all the spiral circuits tested, a modified compound spiral with more cleaning stages and partial middlings recycle is the best option for improved separation efficiency, clean coal yield and combustible recovery. Preliminary calculations indicate that this new modified spiral circuit is capable of increasing the clean coal yield by 1.9%, while maintaining the same ash contents as achieved by existing compound spiral circuits. This spiral technology research was further expanded in the next chapter “Chapter 5 - Enhanced Sulfur Rejection Using Combined Spiral Flotation Circuits” to investigate new methods for improving fine coal desulfurization. Specifically, this chapter discusses the experimental set up, test results, and technical evaluation of an innovative combined spiral- flotation circuitry. This chapter also describes in detail the study conducted to evaluate the partitioning of pyrite within fine coal circuits. The sulfur and ash separation performances of different fine coal cleaning alternatives were also presented and compared. On the basis of this study, a spiral followed by a froth flotation cleaning process is recommended for the cleaning of high sulfur ultrafine (minus 0.25 mm) coal feeds. This chapter describes the rationale for the 10
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design of this new fine coal cleaning circuit and finally a generic flowsheet is also proposed for any coal preparation plant treating high sulfur ultrafine coal feeds. The next chapter “Chapter 6 - Engineering Development of Micro Sieve Drying Process” discusses the theoretical basis for an innovative fine coal drying process. Experimental results obtained from bench- and pilot-scale testing of this novel approach to fine coal dewatering are also presented and discussed in this chapter. The results obtained from the experimental work indicates that the NDT™ system can effectively dewater fine (1 mm x 0) coal from slightly more than 30% surface moisture to single-digit values. Test data obtained using a pilot-scale NDT™ plant further validated this capability using a continuous prototype facility. The data presented in this chapter also showed that the performance of the NDT™ system is not dictated or constrained by particle size, i.e., it works equally well on 1 mm x 0 coal as it does on 325 mesh x 0 coal. The seventh and final chapter of the dissertation “Chapter 7 – Summary and Conclusions” provides an overall summary of the findings, conclusions and recommendations resulting from this research and development study. 11
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CHAPTER 2 - REVIEW OF LITERATURE 2.1 Fine Coal Processing Coal loss during fine (-1 mm) coal processing is perhaps the greatest among all other size fractions. For example, froth flotation processes typically recover only 60-80% of the organic matter contained in fine coal feeds (Bethell, 1998). A study conducted by Cavallaro et al. (1991) indicates that the reserves of low-ash coal in the central Appalachian region could be nearly doubled by efficiently cleaning at a particle topsize of 1 mm (Figure 2.1). Moreover, surface- based separation processes, such as froth flotation, which are generally used to treat fine (0.15 x 0.044 mm) coal, are less effective in removing pyritic sulfur than density-based processes used to treat the coarser sizes of coal (Adel and Wang, 2005). Therefore, fine coal desulfurization is often poor in many coal processing facilities treating high sulfur run-of-mine coal seams. Field studies indicate that the yield and quality of clean coal products from fine coal circuitry may be significantly increased by improving the efficiency obtained for particle size separations at 150- and 45-μm. Unfortunately, screens used for sizing fine particles, and particularly those finer than 0.5 mm, tend to blind easily, wear quickly and suffer from low throughput and poor efficiency (Mohanty, 2003). Another problem associated with fine coal screening Figure 2.1 Effect of decreasing top size on coal availability (Cavallero et al., 1991). Used under fair use, 2012. 15
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is the inefficient removal of ultrafine mineral sediments, such as high-ash clay particles, from fine coal feeds (Mohanty et al., 2002). Moreover, fine (-1 mm) coal particles may represent as little as 10% of the total run-of-mine coal, but often contain one-third or more of the total moisture in the final coal product. Existing fine coal dewatering processes, such as filtration, centrifuges and thermal drying, are expensive and consume large amounts of energy (Osborne, 1988; Le Roux et al., 2005). The lack of an efficient, inexpensive and safe drying process is one of the primary reasons that about 2 billion tons of fine coal was discarded by the United States coal preparation plants into waste impoundments (Orr, 2002). 2.2 Spirals 2.2.1 Spiral Technology A spiral is composed of a helical channel of modified semicircular cross-section wound around central column. These are flowing film concentrators and have been found varied applications in coal and mineral processing industry. Generally, a feed pulp containing between 15 to 45% solids by weight and in the size range of 3 mm to 75 µm is introduced at the top end of spiral trough. The pulp then gradually flows spirally downwards and, during this motion, the particles tend to stratify into different streams depending upon their particle size and specific gravity. Separation is achieved by the combined action of stratification, film sizing and centrifugal/gravitational forces. Finally, adjustable splitters and/or cutters are used to divert the separated particles into clean, middlings and refuse streams (Davies et al., 1991; Wills and Napier-Munn, 2006). Figure 2.2 is a schematic cross-section of a coal spiral trough. In addition, coal spirals have been successfully used for the treatment of iron ore, chromite, heavy mineral sand deposits. 16
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Figure 2.2 Cross-section of flow through a spiral trough. Spirals are considered as one of the simplest, most effective and lowest cost fine (1 x 0.15 mm) coal processing technology (Kohmuench, 2000). Coal cleaning using spiral concentrators was started back in 1947 when Hudson Coal Company installed 48 spirals to clean fine anthracite coal in eastern Pennsylvania. During the 1950s, a number of researchers tried to use spirals to clean fine bituminous coal, but their attempts were not successful (Denin & Wilson, 1948). Finally, since first introducing design changes in the 1980s that made spirals larger (which improve throughput capacity) and lighter (due to fiberglass and urethane construction), spiral separators have become one of the most popular fine coal cleaning separators. Apart from their simplicity, coal spirals have many other advantages such as low capital and operating cost, simple to operate, no moving parts, no regent requirements, stable cut point with size, good clean coal recovery and high reject ash levels. On the flip side, spirals have low throughput capacity 17
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compared to other water-based separators such as water-only cyclones. Spirals also operate with a relatively high specific gravity cut point and can treat only a very limited feed size range (MacHunter et al., 2003; Luttrell et al., 2003). 2.2.2 Historical Development The concept of separation by spirals dates back to 1943 when Humphreys Mineral Industries introduced their first spiral for concentrating mineral ores. These early units were used to upgrade a wide variety of ores including gold, silver, tin, ilmenite, rutile, zircon, monazite, iron, barite, fluorspar, mica and phosphate (Davies et al., 1991; Leonard, 1991). For many years following the introduction of the first units, spirals tended to be used only for comparatively easy separations. However, subsequent research and development by different spiral manufacturers around the world led to much wider use of spirals in mineral processing applications and eventually to their adoption for the coal cleaning (Richard et al., 1985). The early spirals utilized relatively simple profiles and were designed with a single start and 4-6 turns. These units were constructed from semicircular sections that were bolted together. One of the disadvantages of early spiral separators is that they were constructed from cast iron and weighed about one tonne each. In Australia, sand miners used truck tire sections that were cut and reattached together to form a spiral instead of using excessively heavy spirals. In 1947, spirals made from asbestos reinforced concrete were introduced for rutile and zircon extraction. The decade of 1950 marked a major advance in spiral technology when Ernst Reichert used fiberglass as a construction material for spirals. The use of fiberglass made it possible to made light weight, non -corrosive continuous helices and allowed two or three helices to be mounted on one central column (Davies et al., 1991, Hunter et al., 1985). Another development in the subsequent spirals is the replacement of rotating disc cutters for concentrate removal with the 18
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concentrate cut from the pulp stream by finger-type splitters. All early designs used wash-water channels to overcome the sanding/beaching problem of inner trough section. In late 1970s and early 1980s, Australian researchers came up with modified spiral geometry that resulted in complete wash-waterless light-weight spirals (Richards & Palmer, 1997). The most recent breed of spiral is made of fiberglass spray-coated with polyurethane (Das et al., 2007). 2.2.3 Particle Separation Mechanism While spirals are conceptually very simple in terms of design, the particle separation mechanism that occurs along the flow path is relatively complex. Feed slurry introduced at the top of the spiral gradually flows downward under gravity through the spiral trough. Within the rotating flowing film, coal particles are subjected to gravitational, centrifugal and Bagnold forces (Bagnold, 1954; Kapur and Meloy, 1999). The combined action of these forces causes lighter particles to move towards the outer wall and the denser particles move to the central column. The particle separation mechanism on spirals has been a continuous source of confusion in the literature. Some researchers believe that there are two basic types of fluid flow along a spiral trough, which are (i) a primary axially downward flow and (ii) a secondary cross channel flow (Figure 2.3). The hydraulic phenomenon responsible for both of these flows has been explained by a number of researches (Holland-Batt, 1990, 1992, 1994, 1998; Richards and Palmer, 1997; Kapur and Meloy, 1998). According to Holland-Batt (1990), the interaction between the fluid flow and the particles results in separation of particles of different densities. On one hand, light particles are carried in the cross flow from the inner region of the trough towards the outer region and settle at the bottom of the channel. In this case, light particles are picked up and carried down by the primary flow, which eventually transport the particles out of the separator. On the other hand, dense particles in the outer region quickly fall to the bottom of 19
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the channel and are carried towards the inner region by the cross flow. These dense particles are too heavy to be picked up and carried back into the outer region. Hence, dense remain in the inner region and are carried by the primary flow down the separator (Holland-Batt, 1989). Richards and Palmer (1997) divided the cross section of the spiral trough into three zones as shown in Figure 2.3. The inner zone is occupied by a bed of slow moving heavy particles. In the outer region, or recovery zone, heavy particles must settle into lower layers in order to be transported towards the center of the spirals. The intermediate transition zone contains composite “middlings” particles and is located between the inner and outer zones (Richards and Palmer, 1997). Figure 2.3 Separation mechanism and primary and secondary flow pattern on a spiral trough (Richards & Palmer, 1997). Used under fair use, 2012. According to Luttrell et al. (2007), the above mentioned description of particle separation fails to recognize two counter-rotating flows that actually present across the spiral profile. These 20
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two rotating flows converge along a line of separation as shown by Figure 2.4. The clockwise flow in the lower rotation zone is responsible for moving lighter particles towards the outer wall of the spiral. Heavier particles contained in this flowing stream settle down and are carried inward towards to the inner side of the spiral trough. The clockwise rotation is responsible for providing a dense concentrate that is relatively free of light particles. In contrast, the counter clockwise flow in the upper rotating section stratifies particles along the outer wall according to density. Unfortunately, some denser particles in the upper flow zone settle against the wall and are trapped there by rising current of the counter clockwise flow. Studies indicate that these entrapped high density particles rarely cross from the upper to the lower flow zones and eventually report with the low density product regardless of density. To eliminate these entrapped particles, Luttrell et al. (2000) recommends recleaning of primary low-density product using a secondary stage of spirals. Figure 2.4 Separation regions across a spiral profile (Luttrell et al., 2007). Used under fair use, 2012. 21
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2.2.4 Particle Separation Forces The forces responsible for particle separation within a spiral trough have been studied by a number of researchers (Atasoy and Spottiswood, 1995; Kapur and Meloy, 1999; Atasoy, 1987; Holland-Batt and Holtham, 1992; Luttrell et al., 2000). Forces involved in the particle separation within the spiral trough include hindered settling, interstitial trickling, centrifugal, frictional, gravitational, drag and Bagnold forces (Bagnold, 1954; Kapur and Meloy, 1999). Among these, the Bagnold force is distinctive. Data that shows its existence during particle separation within a spiral trough was first shown by Holtham in 1992. He concluded that Bagnold forces arises due to increase in inter particle interaction at high pulp densities and at high shear rates. It was also found that Bagnold forces weaken at a solid percentage below about 50% (Holtham, 1992). The Bagnold force is a dispersive force that is directly proportional to the shear rate and square of the particle diameter. The Bagnold force varies along the depth of the flowing film and, depending on its magnitude, causes particles to move upward or downward in the flowing film. Studies show that Bagnold forces are in effect within the inner region of spiral, where particles are in bed-load motion and the percentage solids are more than 50% (Atasoy and Spottiswood, 1995). Kapur and Meloy (1999) concluded that amongst all the forces acting on a particle, no single force dominates the others and, hence, separations are based on differences in the rate of change of all these individual forces with respect to particle size, shape, density and radial position. 2.2.5 Spiral Design Parameters Spiral design is critical to effective separation performance and has been the subject of both experimental and computational studies over the last three decades (Kapor and Meloy, 1998; Holland-Batt, 1989; Holtham, 1990; Stokes, 2000). Primary spiral design parameters include spiral pitch, diameter, trough slope, length and profile. Secondary design parameters 22
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include wash-water configurations, feed box arrangements, splitters locations, repulper locations and construction materials. The design process consists of a number of interactive stages and usually starts with the scale-up, followed by volute shape determination, and finally with a sanding analysis (Davies et al., 1991; Holland-Batt,1990). Some of the key design variables are described in greater detail in the following sections. Pitch and Diameter: The ideal pitch of a spiral trough for a particular feed type is one that ensures particle fluidity. In general, the pitch is steeper for heavy high-density feed material and is shallower for light particles (Davies et al., 1991). The diameter of a spiral depends upon the capacity and the separation size. For a given separation size, the capacity of a spiral is a function of trough area and it decreases with the particle size (Hollan-Batt, 1985). Due to the low density and low unit value of coal, spirals used in coal applications have a lower pitch and a larger diameter than mineral spirals (Luttrell et al., 2007). Profile: Profile is a very important design parameter for spirals. In particular, the shape of the inner and flatter section of a spiral controls the migration of high density particles towards central column. The inner profile terminates and curves steeply upward at the outer side as a vertical water-retaining wall. The profile is generally designed to give a targeted relative density of separation, but in practice the profile often represents a compromise between fluidity and selectivity. Davies (1991) also considered the number and method of product stream divisions and overall pulp capacity as important parameters that influence the profile design. Optimizing studies of profile shape, with a focus of material handling aspects, were conducted by Holland- Batt (1995). This work discussed various profile shapes and concluded that trough shape has a profound effect on the nature of fluid flow phenomena and, hence, on the separation efficiency as well. This study concluded that, for a given pitch, one shape will produce excellent metallurgy 23
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but poor material handling behavior, while other shapes may excel at transporting solids but perform poorly in terms of separation (Holland-Batt, 1995). Flow length: In addition to pitch and profile, spiral length is a critical parameter that has been thoroughly investigated by a number of researchers (Davies, 1991; Kohmuench, 2000; Wildon and MacHunter; 1997; Atasoy and Spottiswood, 1995). Length, which reflects the total distance over which slurry travels as it passed down a spiral, is normally referenced by the number of complete 360o turns utilized by the spiral design. This parameter should not be confused with spiral height, which varies depending on the pitch employed. The aim of these studies was to optimize, and perhaps standardize, the required number of turns on a spiral for an efficient separation process for different ores. In early 1960’s, Australian coal spirals employed as few as two full turns, while modern spirals employ as many as seven turns or more to achieve the required separation. In general, a minimum of five to six turns are recommended to achieve maximum separation efficiency (Holland-Batt, 1995). Other research (Weldon and MacHunter, 1997) has suggested that four turns are optimum for most spiral applications and that acceptable separations can be achieved using even shorter two or three turn spirals, depending on the density distribution of the feed particles (Figure 2.5). According to Atasoy and Spottiswood (1995), the optimum length of a coal spiral is a function of feed size. Shorter spirals are more effective for separation of coarse particles, while longer spirals are better for fine particles. 24
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(DGR = Clean Ash/Feed Ash) Figure 2.5 Plot for optimum number of spiral turns (showing 4, 5 and 6 turn coal spirals) (Wildon & MacHunter, 1997). Used under fair use, 2012. Repulping: The installation of repulpers along the spiral length generally improves the separation efficiency of mineral spirals. The repulpers reinitiate the separation process by capturing, mixing and reintroducing the high velocity slurry stream with the relatively sluggish middling stream. The idea of repulping was introduced based on work originally done by Holland-Batt in 1995. According to this study, spiral fluid flow reaches steady-state after only two turns, while mineral recovery slowly continues for up to four or more turns. As a result, repulpers are generally installed after three or four turns when high density products are removed through central column. Several spiral manufacturers have introduced designs that have successfully incorporated repulping (MacHunter et al., 2003). The effectiveness of repulping in coal applications has drawn mixed opinions. In his PhD dissertation, Kohmuench (2000) argued that although repulping in coal spirals reduces gravity cut point but is found to be less effective in improving separation efficiency because the relatively low specific gravity of coal particles 25
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requires more turns to be effectively separated. Holland-Batt (1995) also stated that repulping can destroy a partial separation occurring with finer material and thus can decrease the separation efficiency. Similarly, Atasoy and Spottiswood (1995) noted that if a mineral spiral treating 4.0 SG solids requires only one turn for an effective separation, then it can be expected that a coal spiral will need approximately five or six turns to achieve a good separation. Construction Materials: The earliest spiral was manufactured from cast iron. This practice remained unchanged until the 1950’s when fiberglass was introduced as a construction material for the spiral structure by Ernst Reichert. Until the late 1970’s, rubber was used as a lining material for spiral trough and for feed and product boxes. Rubber lining was generally effective, but expensive and difficult to apply to complex shapes. In 1980’s, sprayed polyurethane was introduced as a lining material. Finally, in 1988, the first mono-polymer spiral was commercially introduced, which is available in either ceramic or polyurethane. The major advantages of the mono polymer spiral construction include improved wettability and fluidity and superior resistance to reagents and to acid and spark attacks. Today, reverse casting is now well established for the construction of spirals, which made it possible to accurately fabricate feed and product boxes, splitters, repulpers and other components of the distribution and laundering system in heavy duty sections (MacHunter et al., 2003). Feed Box: The spiral feed box is used to introduce the slurry to the spiral trough in a direction parallel to the walls of the trough. Ideally, the feed box should be hydraulically designed to provide equilibrium of the flow pattern as early as possible without splashing or surging. It is also generally accepted that the design of the feed box should facilitate the distribution of solids evenly throughout the slurry (Holland-Batt, 1995). More recently, however, some researchers have proposed that selective segregation and distribution of larger particles 26
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towards the inside of the trough may be desirable to reduce unwanted entrapment of dense particles in the high velocity flow region (Luttrell, 2012). Product Splitters: In order to make appropriate low-density, middling and high-density products, spirals are fitted with two adjustable splitters at the discharge end of the spiral. There are several different types of splitters such as small finger splitters, banana splitters and slide splitters. Splitters located at the end of the last turn are normally of the pivoting-blade type. These splitters are placed either on the trough surface or, in some cases, may be embedded in or positioned exterior to the trough surface. The splitters may be positioned in parallel or offset slightly to permit total elimination of either the middlings or concentrated products. Multiple start spirals are linked through a common shaft to control the same splitter positioning. Some mineral spirals are also equipped with one or more auxiliary splitters to remove separated solids (Holland-Batt, 1995). For spiral applications in the coal industry, two splitters are used to separate coal, middlings and refuse products. Generally, the outer splitter nearer the wall is capable of making a density cut between 1.55 and 2.0 SG, while the inner splitter nearer the support pole can make a density cut 1.8 and 2.4 SG (Mikhail et al., 1988). In order to maintain efficiency, a constant density cut amongst the entire spiral bank should be targeted, which requires the position of the splitters to be the same for all the spiral units (Luttrell, 2007). Typically, the outer splitter should be placed to provide an acceptable clean coal product quality, which typically requires a position of approximately 3 inches from outside wall. Likewise, the inner splitter should be placed to provide a reject product that is acceptable for discard, which normally requires a splitter position of approximately 10.5 inches from outside wall. The middlings product resulting from these positions can be diverted to the clean product, refuse stream or recycled back to feed. Some 27
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spirals have an additional primary refuse splitter, called a cutter, located after three or four turns. The purpose of the cutter is to remove high density refuse as soon as possible so as to improve separation efficiency and increase refuse loading capacity. Ancillary Components: In order to collect products from main and auxiliary splitters, some form of product receivers are also associated with the spiral assembly. Their designs vary depending upon the manufacturer and model of spiral. The main characteristics of product receivers include satisfactory performance in terms of wear resistance, avoidance of splashing of products and suitable material handling characteristics (Holland-Batt, 1995). Spirals are usually installed in multiple banks and the necessary ancillaries required for these banks include a frame to support the spiral bank, main distributors to split feed pulp equally amongst each start and launders to transport the concentrate, middling and tailing flows. Spiral banks are fed via an overhead feed distributor which ideally distributes the feed slurry equally and homogenously to every spiral unit in the bank. 2.2.6 Conventional and Compound Spirals There are a number of spiral manufacturer around the world. Some manufacturers incorporate proprietary features into their conventional single-stage spirals and claim that design improves the separation performance. Studies conducted by Honaker and Wang (1991) evaluated the separation performance of four conventional single-stage spirals made by different manufacturers. This investigation concluded that there is a little difference in the separation performance among all these spiral designs (Figure 2.6). Therefore, it is not surprising that most manufacturers have instead focused much of their R&D efforts on the development of compound spiral designs. Compound spirals incorporate two stages of spiral processing in a single spiral assembly. Typically, compound spirals consist of three or four turns of primary spirals 28
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2.2.7 Spiral Operating Variables The separating performance of spirals is greatly influenced by a number of operating variables that are under the control of the plant operators. In coal preparation plants, spiral circuits are not often run at their maximum separation efficiency because of poor feed sizing, incorrect splitter settings, inappropriate solid and volumetric flow rates and uneven feed distribution (Luttrell et al., 2000). Therefore, to avoid these issues, a brief discussion of how these operating variables influence spiral performance is provided in the following sections. Particle Size: There have been conflicting opinions about the optimum particle size range for coal spiral circuitry. For coal applications, some early researchers were of the view that the appropriate coal feed size for spirals is 3 x 0.1 mm (Kapur and Meloy, 1999; Davis et al., 1991), while others suggest that a feed size as broad as 3 x 0.05 mm can be effectively treated by this technology (Holland-Batt, 1992). Another point of view (Luttrell et al., 2007) is that coal particles coarser than 1 mm or finer than 0.2 mm are not cleaned as effectively in spirals and should instead be upgraded by dense medium processes (for plus 1 mm) and froth flotation (for minus 0.2 mm). Slurry Flow Rate: For an efficient separation, spirals should be provided with an adequate and stable slurry flow rate. The optimum slurry flow rate varies according to the spiral diameter. Typically, for most of the industrial units, the optimum flow rate is between 30-40 gallons per minute (GPM) per start for a particle size range of 1 x 0.15 mm (Luttrell et al., 2007). A volumetric flow rate on higher side is maintained for a coarser feeds, while a lower slurry flow rate is required for a finer feeds (Honaker et al., 2006). At a constant tonnage of dry solids, a lower flow rate may result in sanding or beaching problems along the spiral trough. A higher flow can also cause high density particles to report with the water, which reduces the quality of 30
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the low density product by lowering the separation efficiency and increasing the density cut point (Kohmuench, 2000). Atasoy and Spottiswood (1995) studied the effect of residence time on the separation performance of spirals. They concluded that the residence time has a mixed effect on the separation efficiency of the particles of different densities and size classes. For example, residence time does not play a significant role in the separation of low-density coarse (3.35 x 1.7 mm) coal particles. In contrast, increased residence time has an unfavorable effect on higher density (SG > 1.45) particles of the same size class because they tend to move towards the clean coal stream with time. Solids Feed Rate: Recent research (Luttrell et al., 2003; 2007) indicates that the density cut point (SG ) and Ecart Probable (Ep) increases sharply with an increase in the dry solids feed 50 rate to a spiral. As shown in Figure 2.7(a), a decrease in the solids feed rate improves the product quality (lowers the clean coal ash content), but decreases the recovery of product solids (reduces the recovery of combustible organic matter). An increase in dry solids feed rate to more than 3 tonnes per hour per spiral start seriously impacts the separation efficiency (Holland-Batt, 1994; Li et al., 1993). Contrary to this, some spiral manufacturers claim that their spiral designs can handle a feed rate as high as 4.5 tonne per hour per start without impacting the separation efficiency (Luttrell, 2012). 31
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Figure 2.7 Effect of dry feed rate on spiral performance (a) on gravity cut-point, (b) on separation efficiency (Luttrell et al., 2003). Used under fair use, 2012. Feed Solids Content: At constant feed percent solids, an increase in the feed rate increases the volumetric flow of slurry down the spiral. This increases the centrifugal force exerted on the particles, forcing more material to report to the low density product that, in turn, results in a higher density cut point (Mikhail et al., 1988). As shown in Figure 2.6(b), a similar relationship between dry feed rate and cutpoint was also reported by Luttrell (2003). If the dry tonnage is fixed, then an increase in the feed solids content decreases the slurry flow rate and lowers the specific gravity cut point. For coal applications, this action decreases combustible recovery and improves clean coal ash (Luttrell et al., 2003). Mikhail (1988) is of the point of view that feed rate may actually have a greater effect on separation cut point than even splitter position. 32