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By Timothy A. Clancy

In support of research on forming ceramics from mining and processing wastes, the Bureau of Mines tested various commercial refractories to evaluate their resistance to melts of these wastes. Sixteen refractories of various types were exposed in slag erosion tests to two siliceous waste melts with Si02/CaO ratios of 4.0 and 2.2, The extent and nature of slag attack were then determined for each refractory. The nature of slag attack was investigated through scanning electron micrographs and microprobe elemental distributions. The refractories that performed best in resisting attack by the melts were high-alumina types, and of the refractories tested, the most resistant was a 90-pct-Al203, 10-pct-Cr203 refractory.

Jan 1, 1983

By R. A. Busch, R. R. Backer, R. W. McKibbin

The Bureau of Mines conducted laboratory tests to determine the slur- ry transport and deposition properties of coal waste. A 188.5-ft pipe test loop was constructed with instruments to measure density, flow, and power and discharge, suction, and differential pressures. A 20-ton sample of Western coal waste was crushed and screened to 100 pct minus 1/2 in. Eight loop tests using this graded waste were run at slurry densities ranging from 1.15 (25 wt-pct solids) to 1.46 (60 wt-pct sol- ids). The resultant friction-pressure gradients ranged from 0.06 to 0.24 ft of water per foot of 4-in standard steel pipe. Particle-size degradation was significant. In a typical loop test lasting 25 min, the minus 200-mesh fraction increased from 19 pct to 34 pct. Deposi- tion tests showed that without the use of a flocculant, the slurries would not dewater when left to stand for 1 week. With flocculant, ad- ditional water was released; however, the settled slurries remained thixotropic. Further testing is necessary to determine their suitabil- ity for use as backfill material in active mines.

Jan 1, 1965

By Jack L. Henry, Davis E. Traut, L. R. Penner

The Bureau of Mines conducted solvent extraction batch tests to evaluate the usefulness of neodecanoic acid ( NDA) for extracting Co 3+ from ammoniacal leach liquors high in ammonium sulfate . This work is an outgrowth of previous Bureau research in which technology was devised for the recovery of cobalt , nickel , and byproduct copper from domestic laterites . The previously devised technology uses an oxidative ammoniacal sulfate leach to treat the laterite , and nickel and copper are then recovered from the leach solution by solvent extraction and electrowinning . This report deals with the subsequent solvent extraction of cobalt from the nickel - copper raffinate solution . The results showed that about 70 pct of the contained Co 3+ can be extracted batchwise at pH 8 using NDA ( a 10 - carbon - chain highly branched carboxylic acid ) . However , NDA had a solubility of approximately 0.6 to 0.8 g / L in aqueous raffinate following extraction , and this high solubility makes it impractical for use with alkaline solutions that are low in cobalt . In addition , the extracted cobalt species ( predominately cobaltic hexammine ) is not amenable to the electrolytic recovery of cobalt metal because of its extreme stability . This fundamental prob-

Jan 1, 1965

By B. W. Madsen

The Bureau of Mines conducted a large-scale (6.4 t), long-term (2,165 days) test to gain a better understanding of the leaching characteristics of chalcopyritic ores. An ore sample containing 0.77 pct Cu was leached in a fiberglass column by downward percolation of acidified ferric sulfate solutions. Three sets of leaching conditions were investigated: (1) ambient temperature leaching, (2) elevated temperature (50° to 60° C) leaching, and (3) elevated temperature leaching after inoculation with thermophilic bacteria. Leaching at ambient temperature resulted in a copper extraction rate of 0.44 pct per 100 days. Increasing the temperature to 50° to 60° C resulted in decreased activity of natural mesophilic bacteria, and the leaching rate decreased to 0.22 pct per 100 days. The pH was lowered from 2.0 to 1.6, and nutrient solutions that contained thermophilic bacteria were added. This procedure resulted in an increase in the ferric-to-ferrous iron ratio and an increase in the copper leaching rate. However, the increased leaching rate was not sustained, and 120 days after inoculation the bacterial activity declined, the ferrous iron content increased, and the copper leaching rate decreased.

Jan 1, 1983

By R. P. Walters, M. J. Lynch, D. R. Flinn

The Bureau of Mines evaluated tthhee feasibility of substituting platinum- coated metals for bulk platinum shapes as a means for conserving platinum . Platinum coatings were prepared using four different methods of electrodeposition , then tested and evaluated . In order for platinum coatings to be useful in process environments , they must be thick , adherent , stress - free , and pore - free . The Bureau evaluated direct - current , current reversal , cathode shielding , and pulsed- current plating techniques for producing a pore-free platinum electrodeposit from a molten cyanide bath . Aqueous corrosion tests of Fe - 10Cr substrates coated with approximately 25 μm of platinum showed that pulse plating yielded the most corrosion- resistant and , hence , the most pore -free coatings . The morphology of coating cross sections was in all cases columnar . The average grain size of pulse -plated deposits was independent of thickness , while all other plating techniques produced grains that increased in size as the coatings became thicker . It is believed that the constant grain size in the pulse - plated deposits resulted from better mass transport during the electrodeposition .

Jan 1, 1965

By T. L. Turner, Daniel T. Rogers

As part of a program to investigate technology for the extraction of studied HNO3 alumina from abundant domestic ores , the Bureau of Mines leaching of calcined Georgia kaolinitic clay . In this investigation , iron impurities were removed from the aluminum nitrate pregnant leach liquor by solvent extraction , and the purified liquor was evaporated to prepare a suitably concentrated crystallizer feed liquor . Aluminum nitrate nonahydrate was crystallized from the liquor to separate the aluminum from undesirable trace elements and excess water . Continuous crystallization at 40 ° C in a pilot plant vacuum evaporative unit was performed for 5 days to observe the effects of impurity buildup under minimum bleed- stream conditions . Liquor feed rate was 26 lb/h and AAll (( NNOO33 )) 33..99HH22O0 ((AANNNN)) crystal production rate was 17 lb/h . Fe 203 and Cr203 were not effectively separated from the crystals , and P205 , MgO , and K20 impurities must be removed by recrystallization . Other impurities did not excessively contaminate the crystals . Washing the crystals with water or aqueous HNO3 gave an equivalent increase in crystal purity levels by displacing mother liquor . Theoretical equations , applicable to any continuous evaporative crystallization of developed to produce material balances for engineering ANN , were applications .

Jan 1, 1965

By Dwight L. Sawyer, Roy T. Sorensen

The Bureau of Mines has investigated the recovery of alumina by hydrochloric acid leaching of calcined kaolinitic clay . Bench- scale studies indicated that horizontal belt filtration was a pprraaccttiiccaall method for separating the siliceous residue from aluminum chloride liquor generated in the leaching step . Miniplant -scale continuous testing was performed to evaluate the filter circuits and to compare filtration response of different calcined kaolin feed materials and of different agitatorbaffle designs in the leaching reactors . Soluble alumina recovery with a single filter ranged from 94 pct with minus 10 -mesh feed more than 96 pct with minus 35-mesh or misted feed . Process advantages were confirmed for the calcined misted kaolin feed material prepared by a Bureau-developed misting process . With two filters in series , an overall filtration rate of 100 lb solids /hr.ft - 2 of filter area was attained with a soluble alumina recovery of more than 99 pct . More than 99.5 pct alumina recovery was obtained with a thickener and a two - filter circuit for either the minus 35-mesh or the misted feed . Modifications in leaching reactor design made to decrease particle- toparticle attrition were successful and significantly increased filtration rates and decreased flocculant requirements .

Jan 1, 1965

By V. E. Edlund

As part of its efforts to devise new and improved methods for recovering lithium from unconventional resources , the Bureau of Mines investigated a lime -gypsum- roast , water- leach technique for processing lithiumenriched ( 0.01-0.68 pct Li ) clays . This report presents the results of a study of the technical feasibility of extracting lithium from raw material representative of clay beds associated with the McDermitt Caldera complex in Nevada and Oregon . prepared from water used Pellets suitable for bench-scale roasting studies were mixtures of minus 200 -mesh clay , limestone , and gypsum , with as the pelletizing agent . Roasting pelletized charges at 900 ° to 1,000° C temperatures for 1- to 4-h periods produced calcines that leached readily , yielding water - soluble lithium sulfate ( Li₂SO4 ) . A 5-3-3 ( weight ratio ) mix of clay , limestone , and gypsum produced calcines with the best leaching characteristics . More than 91 pct of the contained lithium was extracted from pelletized mix batches roasted in covered refractory boats . Lithium recovery decreased to about 87 pct when the mix was roasted under dynamic conditions in a gas - fired rotary furnace . A reaction mechanism was postulated which indicated that dilution and loss of SO2 and oxygen in the combustion exhaust adversely affected the leachability of the dynamically roasted calcine .

Jan 1, 1983

By G. B. Atkinson

The Bureau of Mines investigated a method for increasing the leaching rate of bulk superalloy scrap to facilitate recycling and recovery of critical metals such as Ni, Co, and Cr. Three superalloys were investi- gated, the cast-nickel-base superalloy IN-738, the wrought-nickel-base superalloy Rene-41, and the cast-cobalt-base superalloy Mar-M-509. Superalloys melted with 20, 30, 40, and 50 pct Al metal to form inter- metallic compounds were easily crushed to a convenient particle size and reacted rapidly with acid solutions which dissolved the metals. For example, leaching 1/2-in pieces of unalloyed IN-738 with excess 6N HC1 at 95° C for 2 h dissolved about 0.5 pct, while leaching 10 g of minus 20-mesh 30 pct Al-70 pct IN-738 with excess 6N HC1 at 95° C for 2 h dis- solved 96.2 pct.

Jan 1, 1983

By Richard S. Olsen

Prior work by the Bureau of Mines demonstrated a feed preparation method that eliminates the formation of slime during leaching of calcined kaolinitic clay and makes leached residues fast settling and easy to filter. Nitric acid leaching rates determined for calcined kaolinitic clay prepared by this method were found to correspond to a zero-order reaction model for both batch and continuous, stirred-tank leach-ing. A rate constant of 0.136 min-1 was determined. Separation of solid residues from the reacted slurry was examined, and filtration rates were determined. Permeabilities of the flocculated, leached residues were around 51 darcys, or 5.0 x 10-7 cm2 for laminar flow through 4-ft-deep beds.

Jan 1, 1983

By C. O. Ruud, R. E. Siemens, D. Chandra

The mineralogical constitution of a lateritic ore dictates the type of metallurgical process that can be used to extract valuable metals such as nickel and cobalt . To provide needed mineralogical information on the interrelationships of the metals contained in domestic laterites , the Bureau of Mines awarded a grant to Denver Research Institute to study the transition - type , low - grade laterites found in northern California and southern Oregon . For comparison , limonitic - type laterites from New Caledonia and the Philippines were also studied . X-ray diffraction , electron microscopy , electron beam analysis , and conventional petrography were used to determine the mineralogical associations of nickel and cobalt in the laterites . Results showed that for both laterite types studied most of the nickel and minor amounts of cobalt are associated with the mineral geothite ( FeO ( OH ) ) . Most of the cobalt and minor amounts of nickel are associated with a mixed manganese oxide (wad ) mineral .

Jan 1, 1983

By J. E. Schiller

The Bureau of Mines is investigating methods to treat waste water that contains cyanide. This report describes a new method that removes heavy metals and all forms of cyanide. In the first step, hydrogen peroxide and sodium thiosulfate are added at pH 7 to 9 in a 1:2 molar ratio to convert free and weakly complexed cyanide to nontoxic thiocyanate. Then steryldimethylbenzylammonium chloride is added to precipitate ferro-cyanide, and finally, ferric sulfate is added as a sweep floc and sequestrant for heavy metals. After the suspended solids settle, the water is polished by filtering. The water initially contained 1 to 5 mg/L Fe, 1 to 5 mg/L Cu, and 10 to 30 mg/L total cyanide; the level of each of these constituents was reduced to less than 0.02 mg/L.

Jan 1, 1983

By K. J. Ladwig

The Bureau of Mines conducted a field investigation of the water quality in inundated underground coal mines in the Northern Anthracite Field, eastern Pennsylvania. Water samples were collected at multiple depths from nine abandoned mine shafts in the Wyoming Basin, ranging from 68 to 650 m (223 to 2,132 ft) in depth and intersecting as many as seven mined seams in a single shaft. The shafts were also monitored for fluid resistivity, fluid temperature, Eh, and pH using downhole instrumentation. The monitoring program showed that the formerly highly acidic mine water is now slightly alkaline. Sulfate concentrations decreased as much as 74 pct in the flooded workings and 54 pct at a mine water discharge from values reported in 1964 and 1968, respectively. These data are consistent with the inhibition of pyrite oxidation and gradual flushing of oxidation products in flooded mine environments. The monitoring program also revealed significant vertical stratification in water quality in five of the nine shafts, each characterized by two easily recognizable zones. The transitions between zones were sharp, marked by rapid changes in Eh, pH, and ionic composition, the upper zones being less contaminated than the lower zones. The development of stratification appears to be a function of shallow localized flow conditions, arising primarily from the relative positions of mine openings and structural features of the coalbeds.

Jan 1, 1984

By Nicholas Kyriazi

The Bureau of Mines subjected three commercial compressed-oxygen self-contained self-rescuers to a series of laboratory treatments designed to simulate various environmental conditions in underground coal mines. The environmental treatments consisted of extremes of temperature and of shock and vibration. The tests were designed to predict the ability of the self-rescuers to withstand those environmental stresses without causing a decrease in wearer protection. A critical concern was internal damage to an apparatus that would cause it to malfunction or seriously degrade its performance without any obvious external signs. The Bureau has previously tested chemical oxygen self-contained self-rescuers in a similar research program. Although the three compressed-oxygen units are not as sturdy as the chemical oxygen self-rescuers tested previously, they performed reliably after treatments on treadmill tests with human subjects and on machine tests using a breathing and metabolic simulator. Serious damage was caused by both the heat treat-ment of 71° C (venting of the 02 bottle in most cases), and in the shock treatment (breaking open of the case and dislodging of the components). When physical damage is obvious, a complete refurbishing of the damaged self-rescuer is recommended.

Jan 1, 1983

By R. E. Siemens, Gary L. Hundley

The Bureau of Mines has devised and demonstrated a process for recovering Ni and Co from low-grade domestic laterites . The process consists of four mmaajjoorr steps : ( 1 ) reduction roast , ( 2 ) ammoniacal leach , ( 3 ) solvent extraction , and ( 4 ) electrowinning . Several solid - liquid separation steps are required that affect the economics of the overall process . In this study , two techniques for solid - liquid separation , centrifugation and thickening , were investigated . This report presents the results of ( 1 ) laboratory and pilot plant studies to determine parameters for sizing centrifuges and thickeners and ( 2 ) an economic study of the two techniques , based on the requirements of a commercial - size ( 5,000 - tpd ) laterite processing plant . Sizing and other equipment - related recommendations , based on data from the Bureau's studies , were obtained from commercial manufacturers . The costs of thickening and centrifugation , including all the unit operations affected , were determined by the Bureau's process evaluation group . The total operating costs for separation using the two techniques ( including depreciation on the capital cost of equipment ) were found to be quite close : $ 17.26 per ton of laterite for centrifugation and $ 18.15 per ton of laterite for thickening . For centrifugal separation , the greatest cost was found to be the initial capital cost for the separation equipment ; using thickeners , the greatest cost was for reagent recovery .

Jan 1, 1983

By E. C. Baker

The Bureau of Mines estimated the economic feasibility of investing in a directional hole methane drainage project in the Pittsburgh coalbed for 5 yr in advance of mining. This report estimates the capital investment and operating cost of recovering 325 MMft3 of methane gas per year and the selling price of approximately 317 MMft3 of gas per year. The labor, equipment, and supply requirements were determined from those of a previous directional hole drilled at the Emerald Mine, near Waynesburg, PA. The cost of equipment, materials, services, and labor are in third quarter 1982 dollars. They were obtained from vendors, contractors, and the U.S. Department of Labor. Findings indicate a total capital investment of $1,381,160. Annual operating cost amounted to $167,690. At a wellhead price of $2.05 per thousand cubic feet, the sale of approximately 317 MMft3 of gas per year results in a rate of return on investment of approximately 25 pet.

Jan 1, 1984

By Arthur V. Petty

The Bureau of Mines has investigated the effect of refractory oxide additions, introduced in soluble form, on the refractory properties of 42-, 58-, and 70-pct-A1203 brick. Brick having porosities ranging from 12 to 16 pct were impregnated with solutions containing chrome, chrome-iron, zirconium, calcium, magnesium, cobalt, nickel, tin, and manganese ions. Additions of some of these ions provided dramatic improvements to such properties as hot modulus of rupture, hot load, and particularly slag resistance. These improvements can be related to reduction of porosity, amorphous grain boundary phases, formation of more refractory bond phases, and reduction of the wettability of Al203-containing refractories by metallurgical slags. Fifty-eight-percent-AI203 brick, impregnated with chrome, showed hot modulus of rupture, hot load, and slag resistance two to five times better than those of untreated 70-pct-AI203 brick. This could result in reducing the Nation's dependence on imported refractory-grade bauxite generally required for high-A1203 brick, as domestic alumina resouces could be used to produce the improved refractories.

Jan 1, 1984

By L. P. Kleinmann

To control the formation of acid drainage at its source, the Bureau of Mines has investigated the role of iron-oxidizing bacteria in the oxidation of pyrite. In laboratory tests, it was determined that Thio-bacillus ferrooxidans could be controlled in coal refuse using anionic surfactants, with an associated decrease in acid production of about 75 pet. Based on these results, large-scale tests were conducted at an 8-acre active coal refuse area in northern West Virginia and an 11-acre inactive refuse pile in southern West Virginia. Acid production was decreased 60 to 95 pet for 4 to 5 months after application of 55 gal/ acre of 30-pct sodium lauryl sulfate solution. To date, effluent surfactant concentrations have been extremely low. Either a hydroseeder or a road-watering truck can be used to apply the surfactant. Since the surfactant solution must reach the pyritic material to be effective, sites that have been reclaimed are generally not amenable to these procedures. A simple laboratory test is described that provides an estimate of adsorption potential; this can be used to calculate a safe application rate.

Jan 1, 1983

By J. P. Bennett

Based on previous Bureau of Mines research indicating that improved high-temperature properties could be achieved for periclase refractories through chemical additions, the Bureau investigated the properties of full-size bricks produced from chemically modified periclase refractory grains and the suitability of making such chemical additions to Mg(OH)2 slurries prior to production of the periclase grains. In full-size brick testing, strength values, both hot and cold, for the optimized bricks were superior to those for a commercial 98-wt-pct-MgO refractory. The best results were obtained for a natural magnesite with an adjusted CaO:Si02 (C:S) ratio of 3.0 and a 1.0-wt-pct addition of Zr02 and for a seawater periclase with an adjusted C:S ratio of 2.5 and a 0.5-wt-pct addition of Mn02. For samples produced from chemically modified Mg(OH)2 slurries, additions of both Mn02 and Zr02 and an increase in C:S ratios produced significant increases in hot flexural strength, similar to those resulting from chemical additions made to periclase grains. The most effective modifications were additions of Mn02 to brine-derived periclases having a C:S ratio adjusted to 3.0. These results on chemically modified magnesia refractories indicate that such material could potentially substitute for magnesiachrome refractories containing imported chromite.

Jan 1, 1984

By D. J. MacDonald

The Bureau of Mines has conducted bench-scale investigations leading to the design of an integrated process for producing reactor-grade zir-conium oxide (Zr02) from zircon sand, which avoids the air pollution, water pollution, fire hazard, and odor problems associated with the hexone-thiocyanate process. The integrated process consists of three steps: production of crude zirconyl sulfate solution, solvent extraction, and production of Zr02 from strip liquor. This report describes the solvent extraction step. Multistage, countercurrent liquid-liquid extraction with a tertiary amine in kerosine was used to separate zirconium from a dilute H2S04 solution containing hafnium and other impurities. Process steps de-scribed include extraction from an aqueous feed solution to form a hafnium-contaminated, zirconium-bearing organic-phase solution, scrubbing to separate zirconium from coextracted hafnium, stripping to transfer hafnium-free zirconium into an aqueous strip liquor, chloride-loading to produce a chloride-bearing organic solution, scrubbing with the chloride-loaded organic solution to remove traces of uranium impur-ity from the zirconium-bearing strip liquor, and regeneration to pre-pare the organic solution for reuse. These steps were performed simul-taneously in steady-state, bench-scale experiments. Zirconium recovery of up to 93 pct was achieved. Results of an economic evaluation are included.

Jan 1, 1984