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By D. E. Shanks

As part of its goal to help maintain an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines, U.S. Department of the Interior, is investigating a fused-salt electrolytic procedure for producing zinc metal. A previous report described preliminary, small-scale work on the fused-salt electrolysis of ZnC12. The present report covers a more detailed investigation of the properties of ZnC12-alkali metal chloride electrolyte systems in relation to the production of zinc metal and also discusses electrolysis in largescale, internally heated cells. The effect of composition on bath stability, current efficiency, cell voltage, and liquidus temperature was determined for the ZnCla-NaC1-KC1, ZnC12-NaC1-LiC1, and ZnC12-KC1-LiC1 electrolyte systems. An electrolyte com-posed of 38 mole-pct ZnC12, 31 mole-pct NaC1, and 31 mole-pct KC1 gave the best overall results. Sludge (ZnO) formation in the ZnC12-NaC1-KC1, ZnC12-KC1-LiC1, and ZnC12-KC1 systems was investigated during prolonged electrolysis. The ZnC12-KC1-NaC1 electrolyte showed the least sludge formation. A 1,500-amp cell was operated using the ZnC12-NaC1-KC1 electrolyte at 500° C. Zinc metal was produced at the rate of 4.0 lb/hr with a current efficiency of 95 pct.

Jan 1, 1979

By E. R. Cole

The Bureau of Mines developed a procedure that enables substitution of zinc cathodes for the aluminum cathodes normally used in commercial zinc electro-winning. Using zinc cathodes eliminates the necessity for stripping and makes it possible to electrowin zinc from solutions derived from material containing excessive amounts of soluble fluorides; for example, zinc concentrates obtained as a byproduct of fluorspar mining in Kentucky and Illinois. To demonstrate the viability of using zinc cathodes, fluoride-containing zinc concentrate was roasted, leached, and purified according to current commercial practice. Electrolysis was carried out in 0.8-, 1-, 5, and 10-liter cells at 35° to 40° C with a cathode-current density of 8 amp/dm2 in a solution containing 65 g/l Zn++ and 200 g/l H2S04 using PbO2 anodes. Zinc deposits were produced on zinc cathodes with good morphology and excellent current efficiency (90 to 94 pct) in solutions containing enough fluoride (~0.5 g/l, F+) to cause sticking of zinc to aluminum cathodes. The approach described has failed previously because of severe solution-level corrosion of the zinc cathodes. The present investigation found that the use of a simple mechanical barrier to prevent oxygen migration from the anode was sufficient to prevent solution-level corrosion of the zinc cathode starting sheet.

Jan 1, 1979

By James R. FitzSimmons

This report describes an instrument developed by the Bureau of Mines as an improved device for examining roof rock in bolt holes. The unit consists of a commercially available fiberoptic unit adapted for use as a flexible stratascope. Field testing in both metal and coal mines has shown the instrument can be easily transported and used by a single operator. The size and flexibility of the instrument eliminate the need for specially drilled holes.

Jan 1, 1979

By William C. McBee

Specialized sulfur concretes were developed by the Federal Bureau of Mines as a result of research for the beneficial utilization of sulfur in construction materials. Materials were developed for use in acid and salt corrosive environments where portland cement concrete has been found to deteriorate. Because the mineral aggregates also come into contact with the corrosive media, concretes were developed utilizing both limestone and quartz aggregates. The sulfur binder used with both aggregates was modified by reaction with 5 pct dicyclopentadiene to improve product durability. Sulfur quartz aggregate concrete was found to have moderately high strength characteristics (6,000 psi compressive) and was extremely resistant to chemical attack by both acid and salt solutions. Sulfur limestone aggregate concrete exhibited very high strength characteristics (9,000 psi compressive) and was extremely resistant to chemical attack of salt solutions. Both types of concretes maintained their strength and integrity after long-term testing in acid and salt solutions and exhibited considerable resistance to damage by the action of freezing and thawing. Potential uses include leach tanks, electrolytic cells, thickeners, bridge decking, industrial flooring, pipe, and tile.

Jan 1, 1979

By A. E. Raddatz

The Federal Bureau of Mines, as part of its goal to minimize undesirable environmental impacts associated with mineral processing, has investigated a soda-smelting technique for processing ilmenite into pig iron and a titanium slag that is suitable for a feed to a sulfate-process titania pigment plant. By this procedure, the generation of ferrous sulfate waste and its associated disposal problem is obviated. Molten titania slag was quenched, water leached, and filtered to yield a sodium titanate intermediate product containing about 70 wt-pct Ti02, 1 wt-pct Fe, and 20 wt-pct Na20. This intermediate product, high-soda titanate (HST), was mixed with H2S04, calcined, quenched, and water leached to produce a low-soda titanate (LST) product that contained only 2 wt-pct Na20. Both the HST and LST were evaluated as feed materials for preparing titania by the sulfate process. About 95 pct of the Ti02 was extracted from HST and LST by digestion in concentrated or 50-wt-pct-H2S204 solutions. About 95 pct of the solubilized Ti02 was subsequently recovered from the titanyl sulfate solutions by hydrolysis. Barren solutions from hydrolysis, containing about 26-wt-pct H2S04, were upgraded by vacuum-thermal evaporation or electrodialysis. The regenerated acid solutions were used to digest additional HST and LST.

Jan 1, 1979

By J. B. Stephenson

The Bureau of Mines, under an interagency agreement with the Department of Energy (DOE), investigated the feasibility of hardfacing the critical surfaces of valves and similar devices by chemical vapor deposition. The purpose of this research was to increase the wear resistance of these components for use in the abrasive and erosive environment of coal gasification units. Tungsten and molybdenum coatings were produced on nickel-plated carbon steels and stain-less steels by hydrogen reduction of the metal hexafluoride at 325° to 600° C. Titanium nitride coatings were produced on low-carbon steels by the reaction of titanium tetrachloride, hydrogen, and nitrogen at 1,000° C. Titanium carbonitride coatings were produced on low-carbon steels by the reaction of nitrogen, hydrogen, and methane at 900° C. Tungsten, molybdenum and titanium nitride coatings were formed on 6-, 10-, and l2-inch (0.15-, 0.25-, and 0.30-meter) ball valve seats for evaluation in the low-Btu coal gasification pilot plant at the Morgantown Energy Research Center, Morgantown, W. Va.

Jan 1, 1979

By Annie G. Smelley

The Bureau of Mines, U.S. Department of the Interior, as part of its mission to effect pollution abatement, conducted research to devise means for disposing of phosphatic clay wastes and reclaiming mined land. Part of the investigation was performed in a cooperative research project with 10 phosphate companies in Florida. The colloidal properties of the phosphatic clay suspensions, called slimes, make them difficult to dewater and dispose of without impoundment storage aboveground. Various reagents to flocculate and dewater these plant wastes were evaluated, and a polyethylene oxide polymer was found to function in a specialized flocculation dewatering technique. The flocculation dewatering method was investigated in bench-scale batch tests and applied in continuous dewatering tests using standard mineral-processing equipment. In continuous tests at feed rates of up to 58 liters per minute, wastes at 4 percent solids were dewatered to about 20 percent solids. About 0.8 kilogram of polymer was used for each metric ton of dry waste clay solids; processing time was about 4 minutes. Requirements for the treatment system are (1) proper mixing of the clay-waste feed and flocculant, (2) rapid removal of water as it is released, and (3) physical manipulation to promote cohesion of solids.

Jan 1, 1979

Toward the goal of maximizing minerals and metals recovery from domestic resources, the Bureau of Mines, U.S. Department of the Interior, has conducted in situ corrosion studies at the Salton Sea Known Geothermal Resources Area (KGRA) in the Imperial Valley, Calif., to evaluate and characterize materials of construction for geothermal resources recovery plants. General-, pitting, and crevice-corrosion characteristics of 13 commercially available alloys were investigated for periods of 15 and 30 days in seven process environments expected to be found in typical geothermal resources plants. Stainless steel alloy 29.4, Inconel 625, and the Hastelloys G, S, and C-276 were the most resistant to general corrosion, did not pit, and exhibited little susceptibility to crevice corrosion. Stainless steel alloys 430, E-Brite 26-1, and 6X had low general corrosion rates, but pitted and were susceptible to crevice corrosion. Stainless steel alloy 316 L had a low corrosion rate, but corroded intergranularly, pitted, and was susceptible to crevice corrosion and to stress-corrosion cracking. Titanium-1.5 nickel and TiCode-12 had low corrosion rates, did not pit, and were not susceptible to crevice corrosion. Carbon and 4130 steels had high corrosion rates, pitted, and had high susceptibilities to crevice corrosion. The major scale-forming mineral on the corrosion samples in most of the process environments studied was galena mixed with lesser amounts of other minerals.

Jan 1, 1979

By Max L. Glenn

As part of its goal to minimize requirements for mineral commodities through conservation and substitution, the Bureau of Mines conducted research to develop molybdenum as a potential substitute for superalloys containing the strategic and critical materials, nickel, chromium, and cobalt. Since molybdenum requires protection from oxidation at high temperatures, several complex oxides of the spinel and perovskite structure were investigated to determine which possessed the greatest potential for use as oxidation-barrier coatings. Two spinels (MgCr204 and MgA1204) and five perovskites (BaHfO3, YCrO3, NdCrO3, BaZrO3, and LaCrO3) were selected for testing. Various high-temperature prop¬erties that are important for oxidation-resistant coatings were examined, including diffusion rates of oxygen and molybdenum, recession (vaporization) rates, hardness, erosion resistance, sinterability, reactivity with molybdenum, and ease of application. From the evaluation of high-temperature properties, two spinels (MgCr204 and MgA1204) stand above the other oxides as possible coatings for molybdenum. However, laboratory coatings of MgCr204 at 1,360° C (2,480° F) are equivalent or inferior to currently available MoSi2 coatings; laboratory coatings of MgA1204 may be comparable under limited conditions to currently available MoSi2 coatings at the same temperature.

Jan 1, 1979

By L. E. Schultze

As part of the Bureau of Mines research program on recovering alumina from domestic resources, methods for extracting iron from aluminum sulfate solutions (obtained by leaching kaolinitic clay with dilute sulfuric ,acid) were investigated. In countercurrent extraction experiments at a l-gal/hr flow rate of aluminum sulfate leach liquor, the iron concentration 'was decreased from 1.4 g/l to 0.01 g/l after four stages of using a primary amine extractant. The iron-loaded amine solution was regenerated in five stages using 3[N] sulfuric acid or in four stages using 6[N] sulfuric acid. The aluminum sulfate solution obtained was suitable for the preparation of alumina meeting cell-grade standards of less than 0.01 pct iron.

Jan 1, 1979

By Robert F. Chaiken

The Bureau of Mines is using model ducts lined with coal to study the nature of coal mine fires, their rate of propagation, their influence on ventilation airflows, and their response to sealing and other fire suppression measures. For scale-modeling purposes these studies are being carried out in various size ducts; eventually they will include a full-size mine entry in the Bruceton multiple-entry Experimental Mine. To date, work has been carried out in an insulated 9.l-m-long duct with a 5-cm thickness of coal leaving a 23-by 23-cm square opening for air ventilation. Fire propagation processes in this duct were mainly transient in nature owing to the relatively small length-to-diameter ratio. This report describes the experimental equipment employed and the results obtained to date.

Jan 1, 1979

By John C. Edwards

The Bureau of Mines has developed a time-dependent mathematical model of radiative heating of bulkheads in mines. The model includes both reradiation from the duct (cylindrical) walls and direct radiation from the fire zone. Thermal loss into the wall of the duct and into the bulkhead is included. Both brick and wood bulkheads are considered. It is found that the heating rate of the system scales as the duct length-to-diameter ratio and the flame temperature. In particular, the time required for the irradiated surface of the bulkhead to reach a specified temperature decreases with increasing flame temperature for a fixed length-to-diameter ratio and increases with increasing length-to-diameter ratio for a specified flame temperature. It is also deter-mined that the time, T, for the bulkhead surface temperature to reach a specific value, Tb, for a fixed length-to-diameter ratio less than 4 and for a flame temperature of 1,200 K is approximately linearly dependent on Tb for 500 K < Tb < 700 K, and is nearly exponentially dependent on the length-to-diameter ratio for Tb = 600 and 700 K.

Jan 1, 1979

By B. J. Scheiner

As part of the goal to maximize minerals and metals recovery from primary domestic resources, design factors associated with minimizing current leakage in bipolar cell configurations were studied by the Bureau of Mines as a means of improving the efficiency of bipolar e1ectrooxidation cells. Initial studies that were conducted in a small bipolar cell operating at 140 to 145 volts and 15.4 amp indicated how design factors could be employed to minimize cur-rent leakage around adjacent electrodes during cell operation. Based on these results, a 40-electrode, 108-kva prototype of an industrial-sized cell was constructed and tested for extracting metal values from offgrade molybdenite concentrates. The feasibility of recovering molybdenum and rhenium from the oxidized pulp also was determined. Feed to the process sequence consisted of flotation concentrates containing 16 to 35 pet Mo as molybdenite and 6 to 15 pct Cu. E1ectrooxidation in the prototype cell resulted in 84 to 97 pct Mo and Re extraction with a corresponding energy consumption of 9 to 13 kwhr/1b Mo extracted.

Jan 1, 1979

By Gerald L. Finfinger

The Bureau of Mines conducted an experimental degasification project in Island Creek Coal Co.&apos;s Virginia Pocahontas No. S mine. Methane from the overlying Pocahontas No. 4 coalbed was entering mine workings in the Pocahontas No. 3 coalbed through fractures in the roof rock. Small-diameter (l-S/B-inch) holes were drilled into the overlying coalbed to reduce the gas pressure and intercept methane flows, which were piped to the surface through an underground 6-inch-diam steel pipeline. The total methane flow rate from the vertical holes averaged 150,000 ft3/day for the first month. Methane flows into the mine were reduced by 47 pet, thereby demonstrating the effectiveness of this form of degasification in reducing ventilation requirements and providing a safer working environment.

Jan 1, 1979

By John Durkin

A computer model has been generated to evaluate speech intelligibility of individuals wearing conventional and electronic hearing protectors. For speakers talking at normal levels in noise levels of 65 db(Lp) or less, it was found that conventional hearing protectors significantly reduced speech intelligibility. Under the same conditions, electronic protectors provided scores equal to those for the unprotected individuals while providing protection from high noise levels. Therefore, electronic hearing protection is valuable in areas where high noise level is intermittent.

Jan 1, 1979

By Martin Hertzberg

A comprehensive study of the flammability behavior of air-dispersed coal dust was made using an 8-liter Bureau of Mines system which included the following: (1) An optical probe to continuously monitor the dust concentration; (2) measurements of ignition energy requirements; (3) the use of several narrow size distributions ranging from 3 to 65 µm in average diameter; (4) measurements of the extent of flame propagation based on pressure attained at constant volume, residual O2 content after combustion, and flame and dust surface temperatures. The measured lean limit for near-horizontal propagation of Pittsburgh coal dust was about 135 mg/l (milligrams per liter), virtually independent of particle size. Required ignition energies were hundreds of joules and measured limit flame temperatures were 1,450 to 1,600° K. Data on inerting? requirements with KHC03, rock dust, and NaC1 gave approximately the same results as full-scale explosion tests. The good agreement suggests that the cause of earlier discrepancies between small-scale laboratory data and full-scale mine experiments may not have been the difference in size, but were rather a problem of proper care in isolating and controlling the significant experimental variables and in consistently defining the extent of flame propagation at the limits.

Jan 1, 1979

By S. Ralph Austin

This Bureau of Mines investigation determined the effects of so-called annealing at high temperatures on radon-222 emanation from domestic uranium ores. Concurrently, a method was developed for closely estimating the emanation coefficients of hot samples from measurements of their gamma activity after cooling. Emanation coefficients of 102 samples from 14 domestic areas of past, present, and possible future uranium production were investigated using modifications of the closed-can, gamma-only assay method at and after cooling from 100° to 1,000° C. True annealing probably does not occur below 500° C. In limited investigations at 500° C and above, effects of annealing are masked by the effects of other parameters. Emanation is commonly less at one or more of the steps investigated in the 100° to 500° C range than before heating. This decrease is tentatively attributed to water loss at temperatures dependent upon the minerals present. The average sample emanates least at 300° C; emanation increases with higher temperatures to at least 900° C. Emanation decreases sharply on cooling, but it is partially restored by prolonged exposure to the atmosphere at room temperature. Higher than average emanation of coffinite ores at 500° C and above may be related to destruction of the coffinite crystal structure.

Jan 1, 1979

By T. L. Marchewka

As part of its program to conserve the Nation&apos;s natural resources by developing improved performance materials, the Bureau of Mines, U.S. Department of the Interior, in cooperation with the U.S. Department of Energy, has conducted an investigation of materials of construction able to withstand the high temperature and hostile environments encountered in coal gasification units. Refractory pipe liners are required when extremely hot gases or abrasive solids are transported between processing units in the gasification plants. One promising technique for producing refractory pipe (or refractory pipe liners) is centrifugal casting. For this study, the effect of processing variables such as workability, additives, reinforcement and spinning time, and centrifugal force were evaluated using four commercial refractory concretes. In addition, data on characteristics such as strength, density, abrasion, and spalling resistance of 5-inch-diam refractory pipe were developed. Techniques for forming large-diameter (19-inch) refractory pipe also were evaluated. The test results indicated that all four refractory concretes could be made into strong, homogeneous pipe, but that optimum casting parameters had to be determined for each specific composition. The investigation revealed that the major controlling factor in the production of the centrifugally cast pipe was the workability of the refractory concrete.

Jan 1, 1979

By David M. Hopstock

To help assure an adequate supply of minerals to meet the Nation&apos;s economic and strategic needs, the Bureau of Mines is conducting bench-and pilot-scale research using wet high-intensity magnetic (WHIM) separation to recover iron from oxidized taconites of the. Lake Superior region. The advantages and disadvantages of WHIM separation in relation to other separation methods, the most recent innovations in WHIM flowsheet design, and the role of mathematical models in process optimization are discussed.

Jan 1, 1979

By J. M. Singer

Thermal, mechanical, and physical properties of virgin and heat-treated Pittsburgh seam coal were determined as part of a comprehensive study of combustion of monolithic coal block. The information was sought to help characterize pyrolysis and combustion processes in underground coal mine fires but should also prove useful in the study of in situ and surface coal gasifiers. Measured properties include thermal conductivity, specific heat, thermal expansion, density, compressive and tensile strength, porosity, and permeability. The transport property data were obtained (when feasible) in two mutually perpendicular directions of the anisotropic virgin coal material, and coal samples carbonized for 5 hours at temperatures of 350° C, 475° C, 500° C, 650° C, and 850° C. Other coals (Pocahontas No. 3, Sewell, and Illinois No. 6 seams) were investigated for porosity and relative permeability. Interdependence among all properties was evident from the results; however, only a few correlations could be developed owing to inhomogeneity of coal material and specimen variation, which had the effect of reducing the accuracy of measurement and increasing data scatter.

Jan 1, 1979