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A preliminary study was conducted by the Bureau of Mines to determine the effect of humidity on salt mine airborne dust levels. Results showed less dust where the humidity was elevated. Dust reductions appeared to be dependent on the equilibrium between humidity and salt.

Jan 1, 1980

The Bureau of Mines conducted large-scale laboratory copper ore leaching tests to enable improving copper recovery from large dump-leaching operations. This was done by comparing leaching progress when copper was recovered from recycled leach liquor either by cementation or by solvent extraction. Copper was leached from 7-ton ore samples at room temperature using pH 2 ferric sulfate solutions. With are samples containing 11 percent minus 0.5-inch fines, no marked advantage in using either of the copper recovery methods was evident after 416 days of leaching. With ore containing 32 percent minus 0.5-inch fines, solvent extraction of copper was advantageous in that 60 percent of the copper was extracted after 568 days, whereas only 48 percent of the copper was extracted when cementation was used. Less acid was consumed during leaching when solvent extraction, rather than cementation, was used for copper recovery. Iron, contributed by cementation with scrap iron, plugged the ore bed containing 32 percent fines.

Jan 1, 1981

By M. J. Sapko

A moderately scaled apparatus was developed by the Bureau of Mines to determine the fire resistance characteristics of mine conveyor belts and similar type materials. The design of the apparatus was based upon data obtained in full-scale fire tests and features a radiant panel to preheat the belt and a methane-oxygen ribbon burner to ignite the sample under ventilating condi¬tions in a rectangular duct. The test method overcomes the limitations of existing laboratory-scale methods and provides a measure of both ignitability and flammability in quantitative terms. Flame propagation depended upon such variables as air velocity, ignitor heat flux, and belt width and height in the test chamber. Data are presented for nine belt materials and fire resistance ratings are proposed in terms of the flame spread rate, heat release rate, and the critical ignitor heat flux. The ratings discriminate between the fire hazard posed by different fire-resistant belts and tend to be in reasonable agreement with those obtained in full-scale fire tests.

Jan 1, 1981

By L. A. Haas

The Bureau of Mines conducted bench-scale leaching tests with recycled spent copper electrolytes and copper-nickel mattes produced from the Minnesota Duluth Complex concentrates. This report describes the first stage of an overall two-stage leach operation. The objective of this research was to determine the matte-leach technology required to convert spent copper electrolyte into an enriched nickel liquor suitable for a nickel refinery and there-fore essentially free of copper, iron, and sulfuric acid. The experimental variables investigated were matte composition, particle size, spent electrolyte content, pulp concentration, oxygenation, temperature, and time. The time required to produce an enriched purified nickel liquor decreased with increasing pulp concentration, temperature, and oxygenation, but increased with increasing particle size and electrolyte copper and acid content. Nickel-rich (about 50 g/l) liquors at a pH of about 4 and containing less than 1 g/l of copper and iron were produced at 70° C by leaching minus 325-mesh low-iron (less than 5 pct) matte for 8 hours with spent electrolyte containing 22.4 g/l Cu, 28.9 g/l Ni, less than 0.1 g/l Fe, and 50 g/l H2S04 at a pulp concentration of 1 kg of matte per liter of spent electrolyteo Varying the nickel content of the spent electrolyte from 11 to 101 g/l appeared to have no appreciable influence on the matte leaching characteristics.

Jan 1, 1981

By C. F. Davidson

The Bureau of Mines studied the extraction of lithium from lithium-containing clays by chlorination with hydrogen chloride (HC1). In bench-scale laboratory investigations, HC1-H20 mixtures were used to selectively chlorinate lithium, but not calcium or magnesium, in lithium-containing clays. The addition of calcium carbonate to the clay was found to improve the lithium recovery. Reaction conditions found to affect the lithium recovery were ratio of clay to carbonate, reaction temperature, and HC1 concentration. The best conditions for selective chlorination of the lithium were 2:1 clay-carbonate, 750° C, and 20 wt-pct HC1. The experimental results and trends in lithium extraction are explained using thermodynamic relationships.

Jan 1, 1981

By S. D. Hill

To help insure the continued viability of the minerals and materials sector of the U.S. economy, the Bureau of Mines is conducting research and disseminating technology that will result in more efficient minerals extraction. As part of this effort, a process is being investigated that involves an aqueous chlorine-oxygen leaching procedure to treat complex sulfide concentrates to produce ZnCl2. Subsequent fused-salt electrolysis of the ZnCI2 produces high-purity zinc metal. Previous reports described preliminary, small-scale research on the chlorine-oxygen leaching system and fused-salt electrolysis of ZnCl2. This report discusses the details of design, construction, and longterm, continuous operation of both monopolar and bipolar fused-salt cells. The effects of temperature, electrode gap, current density, electrolyte composition, and electrode configuration on current efficiency and energy consumption were determined for a ZnCl2-KC1-NaCl electrolyte system. Zinc metal was produced at the rate of about 50 lb/day in a monopolar cell which was operated continuously for 60 days with current efficiencies from 85.8 to 98.6 pct and an average power consumption of 2.1 kwhr/lb. Bipolar cells with several different electrode configurations were operated for 90 days. A current efficiency of about 70 pct and power consumption of about 1.7 kwhr/lb of zinc were achieved using a three-electrode-pair, bipolar assembly with a chlorine gas lift pump to circulate electrolyte.

Jan 1, 1981

By Robert P. Vinson

This Bureau of Mines report presents the results of tracer gas studies conducted at three facilities where bagger hoods had been installed several years ago to remove airborne silica dust from the vicinity of the bagging operator. The studies indicated that for optimum benefits makeup air must be evenly dispersed, the hood enclosures and duct systems must be as airtight as possible, the average intake air velocity of each hood should be at least 200 fpm, and the hoods and duct systems must be properly maintained.

Jan 1, 1981

By L. W. Brandt

The Bureau of Mines, as part of its mission to effect pollution abatement, conducted research to study various means of dewatering Florida phosphatic clay wastes and reclaiming mined lands. The work was done in cooperation with 10 Florida phosphate companies. During this work, a novel technique to effectively dewater phosphatic clay wastes was developed. The solids contained in the clay waste slurry are slowly compressed by moving wire mesh screens through the system. In a typical application, the screens were moved downward, compressing solids ahead of the screens. The rate of movement of the screens is an important variable in the process. It is believed that the moving screens distort the gel structure of the phosphatic clay system and cause the release of water. Samples of 18 clay wastes, including a high-grade attapulgite from beneficiation plants of the Florida phosphate field, were studied using the method. Typical samples were concentrated from initial solids of 4.7 and 11.9 percent to 16.8 and 25.2 percent, respectively, in 3-1/2 days. The high-grade attapulgite sample was dewatered from 2.7 percent solids to 13 percent solids in the same period.

Jan 1, 1980

By V. R. Spironello

The Bureau of Mines is conducting studies of the slags related to ferrous technology to evaluate acceptable substitutes for the auxiliary flux, mineral fluorspar, in foundry operations. This work is directed toward the Bureau's goal of minimizing the Nation's dependence on scarce and critical minerals Comparative basic practice cupola (18-inch-ID) trials were made to evaluate a waste material called "used potlining," which contains significant levels of fluorine, sodium, and aluminum in various compounds. Used potlining is recovered from alumina reduction cells after its useful life, and was supplied by the Aluminum Co. of America (Alcoa) to the Bureau for evaluation. The material in the lump and pelletized form (with limestone) provided extremely fluid slags based on visual observation during cupola operation. No adverse effects were found on cupola performance, metal and slag chemistry, the environment, or mechanical properties of the castings produced. Fluorine recovery in the slag was equal to, or higher than, that of fluorspar; fluorine losses to the scrubber water and solids were lower. The acidity of the scrubber Hater was somewhat neutralized. No difference was observed in furnace-refractory attack, as determined by the level of magnesia in the slag and visual inspection. The recovery of sodium in the slag, presumably as the oxide, significantly increased slag fluidity, suggesting that less than equivalent fluorine may be required. There was no contamination of the gray iron by the aluminum from the used potlining. Used potlining was completely satisfactory as a substitute for fluorspar in cupola ironmelting.

Jan 1, 1981

By John C. LaScola

The Bureau of Mines investigated coal storage silos to determine how gassy coal must be for methane accumulations in a silo to become hazardous and where such accumulations are likely to occur. Methane concentrations were measured in the open space above the stored coal pile, in the pile, and in the reclaiming area. No methane layering was found in closed-top silos. Reclaiming areas were as gassy as the top part of the silos. Coal samples were collected from the conveyors entering the silos in order to assess the gassiness of the coal. No simple correlation was found between the gassiness of the coal stored and the measured methane concentrations. However, at mines where the average 24-hour gas emission from the conveyor belt samples was 14 ft3/ton or more, fans or open tops were used. It appears that a large fraction of the methane released during storage remains in the void space between the coal particles.

Jan 1, 1980

By E. R. Cole

This Bureau of Mines investigation was prompted by the need forr a stable anode for electrowinning metals, particularly zinc and copper, from acid solutions. The polarization behavior of Pb-Ag (1 pct Ag) anodes in H2SO4 and fluoride solutions was determined as the first step in the development of such an anode. A Luggin capillary, dc power supply, high-impedance voltmeter, and other equipment standard to an electrochemical laboratory were used in this study. It was determined that during polarization, a relatively hard, stable coating of Pb02 was formed on the surface of the lead-silver anode and the rate of formation of this coating was considerably enhanced by the presence of fluoride ions in solution. Subsequent investigations at the Bureau of Mines Rolla Research Center resulted in the development of a Pb02-coated titanium (Pb02-Ti) anode. Results of this effort were presented in Bureau of Mines Report of Investigations 8111. Additional data resulting from extensive testing of the Pb02-Ti anodes, as well as process improvements and innovations, are included in this report. The anodes were considered generally unsatisfactory for zinc electrowinning because of lower conductivity, higher oxygen overvoltages, and shorter in-cell life as compared with the Pb-Ag anodes now being used in industry. However, the PbO2-Ti anodes were used successfully to oxidize waste chromium solutions and to electrowin copper.

Jan 1, 1981

By A. E. Raddatz

In an attempt to develop technology to use domestic resources in place of imported bauxita, the Bureau of Mines investigated sulfurous acid leaching to extract alumina from kaolin. The process consists of leaching the calcined kaolin with a 30 wt-pct S02 solution at 60° C and 160 psig for 17 hours, fil¬tering the leach slurry, precipitating monobasic aluminum sulfite from the filtrate at 110° C and 60 psig, a& decomposing the sulfite in the spent liq¬uor at 150° C and 55 psig to produce crude alumina. Purification of the crude alumina was accomplished using a modified Bayer process. Results from closed-circuit tests employing the sulfurous acid process showed that overall extraction of alumina from kaolin was 67 pct. Production of 1 ton of alumina would require 3.6 tons of calcined kaolin, 0.7 ton of sul¬fur dioxide, and 8.4 tons of water. After purification by a modified Bayer process, the alumina product contained the following; impurities, expressed in weight-percent: Fa203, 0.009; S, 3.6; Si02, 0.07; Ti02, 0.002; K20, 0.017; and P205, 0.03.

Jan 1, 1981

By Philip C. Good

The Bureau of Mines investigated the feasibility of utilizing low-grade phosphatic shale as a feed for phosphoric acid production. Present practice in the phosphate mining operations of southeastern Idaho is to remove and either stockpile or waste low-grade phosphatic shales as the high-grade phosphate beds are selectively mined. Acid digestion studies were performed on uncalcined shale and on shale calcined to remove free carbon to determine phosphoric acid quality, yield, and amenability to filtration. The untreated shale, containing 21.4 pct P205, was digested with sulfuric acid in a single-tank reactor to yield phosporic acid and gypsum residue. Although 96 pct P205 recovery was attained in digesting uncalcined shale, only the calcined product gave satisfactory filtration rates. Calcined shale yielded phosphoric acid recovery of about 93 pct of the contained P205. It was higher in impurities than commercially prepared acid derived from high-grade western phosphate rock. An acid filtration rate of 745 lb P205/ft2/day was attained. This value is lower than the rate of 900 lb P205/ft that is generally considered to be acceptable in industrial production of phosphoric acid from high-grade phosphate rock.

Jan 1, 1981

By D. A. Stanley

The Bureau of Mines conducted laboratory-scale experiments to determine whether or not surface waters with a high organic content could be purified sufficiently to be used to replace the natural high-quality deep well water currently being used in the silica flotation step of phosphate rock beneficiation. Waters abundant in organic matter were collected from two central Florida streams, flocculated with a cationic polyethylenimine polymer, and processed in a sand filter. This treatment removed most of the organic materials from the water. Untreated surface water, treated surface water, and distilled water were used to compare the flotation response of the acid insolubles in an amine flotation circuit. Surface water treated with PEI-1000 was shown to be as effective as distilled water for the acid-insoluble-flotation step. Flocculation and filtration can therefore produce water suitable for amine flotation of quartz, which would permit substitution of surface water for deep well water.

Jan 1, 1981

By N. I. Jayaraman

High-pressure shrouded sprays were first tested on a bench to determine air-moving capability and dust collection efficiency. The bench-scale tests indicated that at 500 psi and above, the dust collection efficiency, when sampled downstream of a water eliminator, was about 99 pet for two types of nozzles. However, for the same water flow, the induced airflow was about three times greater in one type than in another. Since the only difference in the nozzles was the spray angle, this factor was important in air movement through a shrouded spray. Full-scale model mine tests were then conducted to determine the reduction in dust concentration behind the line curtain and at the operator position produced by high-pressure sprays in a shroud. The shroud was mounted on top of the boom of a model continuous miner, and high-pressure (greater than 500 psi) sprays were installed inside the shroud. The inlet of dusty air to the shroud was open toward the face and the outlet toward the exhaust line curtain. The high-pressure sprays were compared with conventional sprays mounted at the head of the continuous miner and directing water toward the face. The difference at the operator position (opposite side of brattice) was significant in that, under certain conditions, with conventional sprays an increase in respirable dust concentration of 471 pet was noticed compared with dry operation due to rollback from face. High-pressure shrouded sprays, on the other hand, decreased the dust concentrations at the operator position (opposite side of brattice) by 28.2 pct.

Jan 1, 1981

By D. R. Flinn

A newly developed chemical conditioning technique, which greatly simplifies the preparation of plating baths for the electrodeposition of titanium diboride (TiB2) coatings, is described in this report. The new plating technique was used to prepare samples of titanium diboride (TiB2) coatings on three types of substrate materials. These samples were then evaluated in both low- and high-speed wear-test programs to determine the wear resistance, microhardness, and adhesion of the coatings. In general, it was found that the wear resistance of the coatings is independent of substrate. Scanning electron micrographs have shown that the coating wear surfaces are very smooth, suggesting slow and continuous removal of the coating during the wear test (that is, adhesive wear). Adhesion between the coating and all substrates was excellent. Microhardness results show that the TiB2 coating is harder than alumina, with a hardness value exceeding 5,000 kg/mm2 measured in one test. The results of the wear tests show that TiB2 coatings have relatively poor wear resistance compared with alumina in low-speed unlubricated sliding environments, but exhibit wear properties comparable with alumina in high-speed unlubricated sliding environments.

Jan 1, 1981

By I. Liebman

The Bureau of Mines conducted experiments on coal dust explosion suppression. The investigation took place on a beltway in the double-entry of the Bureau's Experimental Mine. Using conditions that simulate those in a working mine, the investigation showed that a coal dust explosion can be readily initiated in a conveyor belt entry. Also, the explosion can spread into adjacent entries through opened crosscuts (stopping destroyed by explosion) to propagate for long distances even though the adjacent entries are rock dusted in compliance with regulations. Passive water barriers (water-filled tubs) were found to be effective in suppressing explosions on a beltway; however, barrier efficiency was reduced by opened crosscuts. The study indicated that the beltway barrier should be the distributed type consisting of continuous rows of water-filled tubs covering long distances along the entry. A plan is outlined for the installation of a water barrier system in a working coal mine for the protection of a beltway.

Jan 1, 1981

By S. R. Crane

One Bureau of Mines goal is to minimize the undesirable environmental impacts associated with industrial plants emitting waste gases containing S02. To help meet this goal, a regenerable flue gas desulfurization process was developed. This process, known as the citrate process, uses a buffered weak acid solution to absorb S02 from the waste gas. The absorbed S02 is reacted with H2S to precipitate elemental sulfur and regenerate the solution for recycle. The H2S feedstock for the process, if not otherwise available, may be produced by reacting two-thirds of the recovered elemental sulfur with natural gas and steam. Laboratory investigations and pilot plant operations were conducted by the Bureau to determine if H2S from the natural gas, sulfur, and steam reaction was suitable for the citrate process. The laboratory investigations, in which an H2S generator was integrated with other citrate process operations, provided a basis for design and operation of the pilot plant. The objective of the pilot plant was primarily to provide H2S for the citrate pro-cess pilot plant at the Bunker Hill Co. lead smelter in Kellogg, Idaho. The design capacity of the pilot plant was 0.4 to 1.25 tons of H2S per day. The operation demonstrated that (1) a 77-to 79-dry-volume-percent H2S product could be produced from pilot-plant product sulfur, natural gas, and steam; (2) the product R2S regenerated the SO2-loaded citrate solution; and (3) under certain conditions over 95 percent of the natural gas could be converted to H2S.

Jan 1, 1981

By W. N. Marchant

The Bureau of Mines performed chemical research to elaborate details of sulfur chemistry pertaining to the citrate flue gas desulfurization process in which sulfur dioxide (SO2), absorbed (as bisulfite ion) in a buffered sodium citrate solution, is reduced by hydrogen sulfide (H2S) according to the overall reaction 2H2S + HSO3 + H+ ? 3S + 3H20. The rate-limiting step in the process was shown to be the reduction by H2S of thiosulfate (S2031-) that is formed as an intermediate. Pseudo first-order kinetic measurements were made at room temperature to retard the reaction sufficiently that adequate analysis was possible. These measurements showed the rates of the following net processes to be -d [S02]/dt (pH 4.5) = (0.409±0.050)min-1 [S02]; d [S2032-]/dt (pH 4.5) = (0.199±0.017)min-1 [S02]; -d [S2032-]/dt (pH 4.0) = (0.0437±0.0265)min-1 [S2032-]~1; -dH2S/dt (pH 3.9) = (21.6±3.0) mmoles/min-atm [H2S]g1.4, where [H2S]g is the partial pressure of H2S in the gas phase, in atmospheres, and the rate describes the consumption of H2S, in millimoles per minute; d[S]/dt (pH 4.0) = (38.0±3.4)min-1 [H2S]1, where [H2S] is the concentration of H2S in solution. Hydrogen ion consumption during the slow phase of regeneration was shown to occur at (2.1±0.5) times he rate of thiosulfate consumption, which is interpreted as evidence for the following as the rate-limiting reaction: 2H2S + S2032- + 2H+ ? 4S + 3H20 A scheme consisting of five sequential general reactions is proposed to account for sulfur formation.

Jan 1, 1981

By E. D. Calvert

The Bureau of Mines, in its effort to promote greater utilization of domestically abundant materials, conducted reasearch on an alternate mold material that has commercial potential for titanium investment casting. Using variations of the conventional lost wax molding process, investment shell molds were formed entirely of fused, calcia-stabilized Zr02 and a Zr02-forming binder. Optimization of binder/slurry properties', stucco grain size and dis¬tribution, and curing practices resulted in a structurally sound investment shell that was distortion free and thermally stable. Small titanium castings, weighing up to 10 pounds, were prepared in unheated molds by both static and centrifugal casting techniques. Microstruc¬tural examination of the castings revealed that mold fill and surface quality were enhanced by centrifugal casting, although good results also were obtained from the statically poured molds. Microstructural and electron microprobe examinations showed that excessive, brittle case formation could be avoided by curing the dried shell molds in air for at least 2 hours at 1,400° C. Increasing curing temperature and time above these levels yielded added bene¬fits. Molds fired in vacuum at 1,500° C for 4 hours yielded castings essen¬tially free of case formation. The tensile properties of as-cast test specimens (no surface conditioning performed) id the chemical composition of representative metal samples showed that castings produced were comparable to Grades C-1 and C-2 unalloyed titanium This indicated that no sifnificant degradation of metal properties resulted from mold/metal interaction.

Jan 1, 1981