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By Benjamin W. Haynes

The Bureau of Mines conducted research to devise technology for increasing the Nation's mineral supply by recovering valuable constituents from currently discarded waste materials. Municipal solid waste (MSW), presently a major disposal problem, represents a significant source of metals, glass, and a combustible fraction that can be used to supplement coal in generating heat and electricity. As part of the total metallurgical system to treat MSW, this study evaluates the combustible fraction of MSW to characterize the various combustible components and to identify the principal sources of elements that eventually may be objectionable from corrosive or environmental considerations. Several possible sources for cadmium, chromium, cobalt, copper, lead, nickel, and zinc have been tentatively identified. These sources are pigments, inks, paper stock, and additives to plastics. A correlation between industry consumption values and measured concentrations in MSW was found for several elements.

Jan 1, 1978

By Richard G. Sandberg

Sphalerite concentrates prepared during processing of Missouri lead ores contain small percentages of cobalt and nickel which adversely affect zinc electrolysis. The Bureau of Mines has evaluated solvent extraction and precipitation techniques to remove and recover cobalt and nickel from zinc sulfate solution prior to zinc electrolysis. Prepared zinc sulfate solutions containing about 190 gpl of zinc and 50 ppm of both cobalt and nickel were treated using various combinations of complexing reagents, solvent, pH, concentration, time, and temperature. The following complexing reagents gave the best results: a-nitroso-ß-naphthol, ß-nitroso-a-naphthol, 1,2 cyclohexane dione dioxime (nioxime), di-2-pyridyl ketone oxime, and dimethylglyoxime. These reagents in suitable solvents lowered the cobalt and nickel levels to <0.1 ppm. Stripping the complexed reagents from the solvents was not possible except for nioxime. Direct addition of the appropriate reagent to the prepared zinc sulfate solution resulted in the precipitation of cobalt and nickel. Several possible flowsheets are presented for the removal and recovery of cobalt and nickel. Good zinc deposits were successfully electrowon from zinc sulfate solutions purified by solvent extraction and precipitation.

Jan 1, 1978

By R. K. Clifford

Chalcopyrite (CuFeSz) concentrates produced on the Lead Belt of Missouri typically contain 28 pct Cu and from 0.5 to 1.5 pct each of nickel and cobalt. Most of the nickel and cobalt are present as the mineral siegenite, (Ni,Co)3S4, almost none of which is recovered presently. The Bureau of Mines, U.S. Department of the Interior, has been conducting research on the chalcopyrite to produce a marketable fraction enriched in cobalt and nickel. Ferric chloride leaching of various chalcopyrite (copper) concentrates has yielded residues containing from 10.2 to 16.2 pct Ni and 8.3 to 11.4 pct Co with recoveries of approximately 79 pct. In another approach, laboratory froth-flotation tests have been conducted to investigate the effects of regrinding, roasting, baking, and steaming prior to flotation, with a variety of reagents. The best laboratory results were obtained after regrinding the copper concentrate to 94 pct minus 400 mesh and floating the chalcopyrite at natural pH (6.5) with 0.48 pound of sodium diethyldithiophosphate and 0.01 pound of sodium cyanide per ton of concentrate. This procedure yielded a tailings assaying 20.4 pct Cu, 5.2 pct Ni, and 3.45 pct Co. The tailings contained 67.2 pct of the nickel and cobalt and 15.9 pct of the copper originally in the copper concentrate; the remainder of the values reported to the flotation concentrate, which analyzed 29.6 pct Cu. To verify the laboratory flotation results, a 60 kg/hr process demonstration unit (PDU) was constructed in the Cominco American Magmont mill, Bixby, Mo.

Jan 1, 1978

By H. H. Dewing

The Bureau of Mines conducted a laboratory-scale investigation of a technique that produces zinc sulfate and elemental sulfur from sphalerite concentrates by reaction with sulfuric acid at 175° to 200° C and ambient pressure. The objective of the investigation was to develop a hydrometallurgical method of producing zinc from sulfide concentrates that does not generate sulfur dioxide pollutants. Reaction with 80-to 85-pct sulfuric acid produced 4 moles of sulfur for every 3 moles of sphalerite reacted, with minimal production of sulfur gases under optimum conditions. More than 98 pct of the zinc was recovered as zinc sulfate after 3 hours at 175° C. The reaction mixture was leached with simulated spent zinc electrolyte containing 13-pct sulfuric acid to recover zinc sulfate from the insoluble, high-sulfur residue. Neutral zinc sulfate, which is required for electrolysis, was separated from the sulfuric acid solution by crystallization as ZnS04?7H20 at -10° C. Up to 80 pct of the water in the recycled electrolysis solution was removed by the crystallization process; evaporation was used to further concentrate the sulfuric acid for reuse in leaching sphalerite. Advantages of the proposed method over conven-tional roasting and leaching include virtual elimination of sulfur dioxide, production of a solid sulfur byproduct, and higher zinc recoveries due to elimination of zinc ferrite losses.

Jan 1, 1978

By J. H. Perry, Joseph Cervik, G. N. Aul

The Bureau of Mines is conducting research to determine the effectiveness of long holes in degasifying an area of the Upper Split of the Lower Sunnyside coalbed at Kaiser Steel CO.&apos;s Sunnyside No. 1 mine. These holes were drilled from the two outside entries of a section that was closed to mining because of excessive methane emissions. Two holes drilled to 430 and 450 feet produced initial gas flows of 160,000 and 127,000 cfd, respectively. Sixteen days after the completion of the second hole, the total gas production declined to just over 144,000 cfd. In 9 months of degasification, over 35 MMcf of commercial-quality gas has been removed from the coalbed. The combined gas flows declined to 106,000 cfd in the 9-month period. The two holes have reduced face emissions by about 40 pct.

Jan 1, 1978

By J. H. Perry

The Bureau of Mines is conducting research to determine the effectiveness of long holes in degasifying an area of the Upper Split of the Lower Sunnyside coalbed at Kaiser Steel Co.&apos;s Sunnyside No.1 mine. These holes were drilled from the two outside entries of a section that was closed to mining because of excessive methane emissions. Two holes drilled to 430 and 450 feet produced initial gas flows of 160,000 and 127,000 cfd, respectively. Sixteen days after the completion of the second hole, the total gas production declined to just over 144,000 cfd. In 9 months of degasification, over 35 MMcf of commercial-quality gas has been removed from the coalbed. The combined gas flows declined to 106,000 cfd in the 9-month period. The two holes have reduced face emissions by about 40 pet.

Jan 1, 1978

By J. E. Matta

The Bureau of Mines has developed a tracer gas method for measuring leak-age through permanent mine stoppings. In this method, a temporary brattice is erected in the same entry as the leaking permanent stopping. Leakage was evaluated from concentration measurements of a tracer gas introduced into the space between the stopping and brattice. Stopping leakages ranging from 15 cfm to 265 cfm were simulated in an underground coal mine. Leakage values determined by the new method were within 10 pct of the known values.

Jan 1, 1978

By A. F. Colombo

In an effort to maintain an adequate supply of iron to meet national economic and strategic needs, the Bureau of Mines, U.S. Department of the Interior, is conducting research on methods for beneficiating the oxidized taconite resources located on the western Mesabi range in Minnesota, thus expanding domestic iron ore reserves. The selective flocculation and cationic flotation process was investigated in a pilot plant using an ore feed rate of 410 kg/hr (900 1b/hr) and 88 percent recycled water. Lime and a cationic flocculant were used to clarify the waste slurries treated in the water reclamation circuit. An oxidized taconite assaying approximately 36 percent Fe yielded concentrates averaging 63.5 percent Fe and 4.3 percent SiO2 and having an average iron recovery of 84.4 percent. The estimated reagent cost per tonne of concentrate was approximately $1.10. In an attempt to recover more of the iron lost in the flotation tailing, wet high-intensity magnetic (WHIM) separation was incorporated in the pilot plant circuit. The flotation concentrate grades obtained from beneficiation circuits with and without WHIM scavenging were similar, but when WHIM separation was used the overall iron recovery was increased by 2 to 9.5 percent, depending on the iron assay of the flotation tailing.

Jan 1, 1978

By J. C. White

A research study was conducted to devise a method for producing phosphoric acid directly from unbeneficiated Florida phosphate matrix. This research was performed as part of the Bureau of Mines, U.S. Department of the Interior, goals of improving minerals and metals recovery from domestic resources and of minimizing the environmental impact associated with mineral recovery operations. This report describes research in which unbeneficiated, dry, south-central Florida phosphate matrix was digested with sulfuric acid in a continuous-circuit, five-tank reactor to yield phosphoric acid and gypsum residue. Feed capacity of the reactor was 100 pounds (45 kg) of dry matrix per 24-hour day. When digestion was carried out at 185° F (85° C), acid filtration rates of up to 420 pounds of P20S per square foot per day were attained. Combined iron and aluminum impurities in the product filter acid were about 60 percent greater than values reported in commercially produced acid derived from concentrate. phosphate recovery was 87 to 90 percent of the phosphate contained in the as-mined matrix.

Jan 1, 1978

By J. H. Heginbotham

As part of the total metallurgical system to recover metals from secondary resources, the Bureau of Mines conducted froth flotation research, using cationic reagents to recover glass from urban refuse. Batch flotation tests showed that high-quality cullet can be obtained from glass-rich aggregates derived from municipal incinerator residues and unburned refuse. This was confirmed by pilot plant operations treating 350 pounds of flotation feed per hour. Aggregates containing 85 to 90 percent glass were wet-ground to minus 20 mesh, deslimed in two stages, and fed to flotation cells. The glass was selectively floated using an amine collector, usually in an amount under 0.2 pound per ton of solids in the feed. The glass concentrates from the rougher cells were cleaned by refloating two or three times. Over 90 percent of the glass in the deslimed feed was recovered in the cleaned concentrates.

Jan 1, 1978

By D. E. Traut

The effect of various ion concentrations on uranium absorption from a sodium carbonate solution by a strong-base, anion resin was investigated by the Bureau of Mines in support of its objective to help assure an adequate uranium supply for future needs. The studies were conducted to improve the recovery of uranium from in situ leach solutions by ion exchange. The effects of carbonate, bicarbonate, chloride, and sulfate ions were examined. Relatively low (less than 5 g/l) concentrations of chloride, sulfate, and bicarbonate were found to be detrimental to the absorption of uranium. High (greater than 10 g/l) carbonate concentrations also adversely affected the uranium absorption. In addition, the effect of initial resin form was investigated in tests of the chloride, carbonate, and bicarbonate forms; resin form was shown to have no effect on the absorption of uranium.

Jan 1, 1979

By R. P. Beyer

Low-temperature heat capacities and standard enthalpy of formation of copper difluoride (CuF2) were determined by the Bureau of Mines. The low-temperature heat capacities were determined from 11 to 302 K by adiabatic calorimetry. The enthalpy of formation was determined by HC1 solution calorimetry. The standard values of entropy (S°) and enthalpy of formation (?Hf°) at 298.15 K are l8.65±0.03 cal/deg mole and -129.02±0.29 kcal/mole, respectively.

Jan 1, 1978

By E. F. Ferrell

The Bureau of Mines, U.S. Department of the Interior, studied the use of manganese sea nodules for catalytic oxidation in air of 1 pct carbon monoxide, 1 pct propane, and 1 pct methane. Catalysts were prepared from both Pacific Ocean and Atlantic Ocean nodules and compared with a platinum catalyst using a fixed-bed, steady-state microreactor with gas chromatographic analysis. Combustion temperatures with manganese nodules were 50° to 100° C lower than those with the platinum catalyst. Ion-exchange addition of rare-earth promotors to the nodule catalyst decreased combustion temperatures an additional 5° to 45° C.

Jan 1, 1978

By T. G. Carnahan

The Bureau of Mines investigated a flotation-nitric acid leach procedure as part of the goal to maximize minerals and metals recovered from primary and secondary domestic resources. Studies were conducted on an ore that contained carbon-bearing and sulfide mineralization that rendered a portion of the ore refractory (resistant) to conventional leaching technology. The procedure investigated for treating the ore consisted of the following: (1) separation by flotation of the carbonaceous and sulfidic components from the ore, (2) leaching the flotation concentrate with nitric acid at 100° to 110° C, (3) leaching the flotation tailings with sulfuric acid, and (4) processing the combined leached slurries in a conventional manner to recover yellow cake. In step 2, HN03 is converted to gaseous products from which it is regenerated by reacting these products with air and water for further leaching. An overall uranium extraction of 96 pct was achieved by this procedure.

Jan 1, 1979

By David R. Flinn

This Bureau of Mines report describes methods to electrodeposit erosion-resistant titanium diboride coatings from molten alkali metal borate baths at 900° C. These coatings have been shown to be highly resistant to material loss during impingement with high-velocity alumina and silicon carbide powders, and they show promise as protective coatings to reduce metal loss in erosive chemical environments, such as coal gasification systems. The most erosion-resistant coatings were prepared on nickel, Inconel, and molybdenum from an electrolyte containing LiBO2, NaBO2, Na2Ti03, and TiO2. The best coatings were deposited at current densities of [~]20 ma/cm2, using titanium or titanium diboride anodes. Erosion-resistant coatings were shown to exhibit (1) a high degree of crystallographic orientation along the (100) or (110) planes, (2) a chromium impurity level of less than 3 pct, and (3) a uniform, smooth, consolidated surface appearance when viewed under a microscope or by scanning electron microscopy. Optical spectroscopic studies of the molten electrolyte suggest that the lower valent (+3) titanium ion predominates in the baths.

Jan 1, 1979

By Edward F. Divers

This Bureau of Mines report describes the results of a laboratory evaluation of a mechanical dust collector (scrubber) suitable for underground coal mine applications. The scrubber was developed by the Mining Research and Development Establishment (MRDE), Burton-On-Trent, England, and tested at the Federal Bureau of Mines Pittsburgh Mining and Safety Research Center (PMSRC) as part of a technical exchange program. The 2,000-to 8,000-cfm scrubber consists of an electrically driven vane-axial fan, water sprays, a 2-inch-thick, loosely knit stainless steel wire filter panel, and a water droplet eliminator. The dust-laden airstream travels axially through the water sprays, filter panel, fan, and eliminator. Slurry water drains into a sump where a belt-driven pump recycles it back to the sprays. Fractional breakdown tests showed a maximum dust collection efficiency of 96 pct of respirable-size (less than 7 µm) coal dust at 2,000 cfm. Efficiency decreased with increasing airflow; for example, to 91 pct at 6,000 cfm. Following these tests the original wire panel was replaced with a similar but smaller panel developed at PMSRC; a marked improvement in dust collection occurred at all flow rates tested.

Jan 1, 1979

By J. E. Pahlman

One of the goals of the Bureau of Mines is to develop metallurgical pro-cesses that conserve energy and/or that take advantage of abundant domestic energy sources. Western lignites and subbituminous coals can be used for firing pellet induration and metallization furnaces. However, the refractory linings of these furnaces must be able to withstand attack from corrosive alkali metal oxides present in the ash of many of the low-rank fossil fuels. The Bureau of Mines conducted dynamic and static slag tests on high-alumina and alumina-silica refractories to determine their resistance to lignite ash slags. The investigations showed that increased alkali content in the lignite ash caused increased corrosion and erosion of the tested refractories. The degree of corrosion decreased with increasing alumina content, with the 99-percent-alumina refractories having the highest resistance. In general, the matrix phase was attacked preferentially to the alumina grains. Also, porosity reduction and tar impregnation enhanced the corrosion and erosion resistance. The 90-to 99-percent-alumina refractories are recommended for use as furnace linings in alkali slag environments.

Jan 1, 1979

By J. S. Hansen

In support of its objective to conserve mineral resources by minimizing premature failure of materials, the Bureau of Mines conducted a cooperative study with the U.S. Department of Energy on the erosion and abrasion resistance of hard materials for valves in coal conversion systems. This report describes a newly developed erosion-testing apparatus and presents data on the erosion resistance of over 200 materials. Erosion resistance of most metals was comparatively low. In contrast, ceramics and cermets such as B4C, WC, SiC, Si3N4, and TiB2, when fabricated to minimize porosity, displayed greater than five times the erosion resistance of metals. Coatings such as boron diffused into Mo and WC, chemical-vapor-deposited TiCN, and electrodeposited TiB2 were highly erosion resistant if applied in thicknesses ranging from 60 to 75 µm. Erosion resistance of cemented carbides was inversely related to metal binder content.

Jan 1, 1979

By Raymond F. Farrell

A goal of the U.S. Department of the Interior, Bureau of Mines, is the advancement of minerals technology through the development of improved metals and minerals processing. In support of this goal, the Albany Metallurgy Research Center has developed atomic absorption spectrographic methods for the rapid analysis of A1203, CaO, Fe203, MgO, MnO, and Si02 in steelmaking slags. The application of these methods is discussed using an inexpensive pressure dissolution system. The overall coefficient of variation is 5 pct. The accuracy is the same as the reproducibility.

Jan 1, 1979

By A. Visnapuu

The Bureau of Mines, as a part of its goal to minimize occupational hazards associated with mining and mineral processing operations, has developed and field tested a compact exhaust air muffler for mechanized, jumbo-mounted pneumatic rock drills. The muffler is constructed of 1/8-inch sheet steel and has nominal dimensions of 1-3/4 by 9 by 13 inches. A directed air passage, flexible neoprene baffles, and an expandable slit-type outlet are incorporated to reduce drill exhaust air noise and eliminate muffler icing. Field tests in actual mining operations showed a l5-dbA reduction in exhaust noise and an 8-to 12-dbA reduction in overall drilling noise with no icing problems or decrease in drill performance. Data are presented on muffler construction, laboratory, and field test results.

Jan 1, 1979