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By J. M. Gomes

Bench-scale flotation tests were conducted on two western tactite ores to study the recovery of tungsten and zinc minerals. The investigation, which is part of the Bureau of Mines ongoing program to develop methods for beneficiating minerals and metals from domestic low-grade ores, demonstrated the feasibility of producing scheelite, sphalerite, and their bulk concentrates. Sphalerite concentrates containing 51 to 53 pet Zn and less than 0.11 pct W03 were selectively recovered prior to scheelite flotation. Zinc recovery ranged from 85 to 91 pct. Scheelite concentrates containing 17 to 25 pct W03 were then recovered from the ore; tungsten recoveries ranged from 88 to 94 pct. Bulk flotation concentrates containing 84 to 91 pct of the W03 and 87 to 95 pct of the zinc also were prepared. More than 98 pct of the W03 in a bulk concentrate containing 9 pct W03 was extracted by autoclave leaching with a soda solution. The zinc remained in the leached residue.

Jan 1, 1982

By E. G. Baglin

As part of an effort to decrease U.S. dependence on imports of critical and strategic metals, the Bureau of Mines investigated three leaching methods for extracting the base metals and recovering platinum-group metals (PGM) from matte prepared from Stillwater Complex flotation concentrates. Because of a limited supply of natural material, synthetic matte of composition similar to matte prepared from natural concentrates was used to devise the extraction sequences. The validity of the sequences was verified with matte prepared from Stillwater concentrates. In two-stage matte leaching, first-stage H2S04 leaching extracted 99 pct of the nickel and iron from the matte but negligible amounts of copper and PGM. Second-stage oxidative leaching with Fe2(S04)3 or FeC13 solubilized more than 98 pct of the copper and no precious metals. Sequential leaching, in which acid and oxidizing lixiviants were added sequentially to the matte without an intervening filtration step, extracted 99 pct of the Fe, Ni, and Cu. A roasting-leaching technique, in which the residue from first-stage leaching was roasted between 360° and 500° C before a second leaching with H2S04, solubilized 98 pct of the copper. The three leaching methods yielded high-grade PGM residues containing more than 98 pct of the PGM in the matte.

Jan 1, 1982

By A. E. Raddatz

The Bureau of Mines is investigating methods for recovering tungsten from domestic resources. A calcine-quench-leach (CQL) technique was developed for the extraction of tungsten from the Golconda, Nev., hot springs ores. The deposit contains disseminated tungsten that cannot be beneficiated by conventional techniques and must be treated by hydro-metallurgical methods. The CQL procedure consists of calcining the ore at 900° C for 3 hours, quenching in a solution containing 1.5 parts of Na2C03 and 1.5 parts of NaOH per part of WO3 in the ore and at a solution-to-ore ratio of 3 to 1, leaching at 200° C and at 250 psig for 3 hours, and filtering and washing the residue. A series of closed-circuit batch tests showed that 92 pct of the tungsten was extracted from a sample containing 2.32 wt-pct W03. The pregnant solution contained 11 g/l W03.

Jan 1, 1982

By Sterling J. Anderson

To define the technical competence and capabilities of a nonexplosive excavation concept, the Bureau of Mines conducted reduced-scale laboratory tests of a mechanical excavation tool called a rock splitter. Hydraulically actuated splitters, capable of generating both radial and axial loads on a predrilled hole, were designed and fabricated. Through paired variable testing and drifting simulation, reduced-scale splitter performance was evaluated in concrete. Testing proved that the rock splitter is capable of excavating within the highly confined drift set-ting and that it offers a distinct advantage over splitters that can generate radial loads only.

Jan 1, 1982

By T. M. Kohler, G. L. Finfinger, D. M. Hyman, A. T. Iannacchione

The Bureau of Mines measured methane emission rates from an advancing salt face ranging from 15 to 56 ft3/ton (0.5 to 1.8 m3/t). Small room size, use of a continuous miner, and a well-defined ventilation system made possible air velocity and methane concentration measurements, These measurements, representing data from 18 production days, were con- ducted in an area of abnormally low grade salt, Methane emissions occurred primarily during the advance of the salt face by continuous miner.

Jan 1, 1982

By L. W. Higley

It is estimated that well over 20 million lb of chromium and 8 million lb of nickel, plus other metal values, are diverted annually to furnace dusts, mill scale, and contaminated swarfs in the domestic stainless and other specialty steelmaking industry. Little inroad has been made toward the in-plant recycling of these wastes to reclaim the metal values. The Bureau of Mines has devised a process for recovering about 90 pct of the chromium and molybdenum and well over 90 pct of the nickel and iron from stainless steelmaking furnace dusts, swarf, and mill scale. Other metals such as manganese are also recovered. Initial laboratory results were confirmed and expanded to include a wide variation of stainless steelmaking waste mixtures. Later experiments have included specialty steelmaking wastes other than from stainless steelmaking. Significantly, the ease of technology transfer has been demonstrated by a number of industrial-sized (19-ton) commercial electric furnace heats, in which the pelletized wastes represented some 10 to 20 pct of the furnace charge, replacing part of the normal scrap charge. Results of these successful large-scale trials are presented. Some information is also presented on incorporation into the pellets of chromium-bearing particulate wastes originating from other than steelmaking production. Cost evaluation indicates the process is economically attractive.

Jan 1, 1982

By J. K. Richmond

This is a progress report summarizing more than 5 years of a long-range Bureau of Mines research program. The purpose of this program has been to investigate the fire and explosion properties of Green River oil shale in the Bureau's Experimental Mine, in laboratories, and in the field. The lean limits of explosibility of oil shale dust, by small-and large-scale tests, are reported as a function of grade, ignition source, and particle size. A limited number of laboratory tests on the autoignition of oil shale dust layers and the spontaneous combustion tendencies of oil shale are described. Moderate-scale rubble fire tests were conducted to determine flame spread rates as a function of ventilation flow. With the aid of a system to continuously monitor methane emissions in a deep oil shale mine, the characteristics of the methane flow are reported as a function of ventilation and blasting procedures, and are compared with gas yields from core samples. Tentative predictions as to the emission of the methane to be expected in deep oil shale mines, far from the outcrop, are offered. Brief reference is made to a parallel investigation into the fire and explosion hazards of oil shale mining and processing by a Bureau contractor; detailed results of the latter investigation are to be found in the contractor's reports.

Jan 1, 1982

By Yael Miron

ANFO blasting agents may undergo an exothermic reaction when they contact warm ore bodies that contain pyrite and its weathering products. The reaction is very fast at temperatures above 80° C. Urea, when present in sufficient amounts, inhibits this reaction at temperatures below 180° C. But urea-ammonium nitrate mixtures are very hygroscopic and, in certain climates, may be difficult to handle in the field. Reaction-inhibiting characteristics of three compounds were reported by the Bureau of Mines in 1979. Recently, the Bureau investigated the reaction-inhibiting qualities of five additional compounds. Mixtures of ANFO, pyrite, weathering product, and prospective inhibitors were slowly heated, under conditions simulating a hot borehole, to determine prospective inhibitor capability at temperatures up to ~175° C. Small-scale thermal tests of the same mixtures were used for verification and clarification of results. Two organic compounds, phthalimide and xanthine, similar in structure to urea, failed to inhibit the reaction. Zinc oxide and calcium carbonate were found inferior to urea, though zinc oxide raised the onset of reaction from 80° C to about 140° C. Only magnesium oxide was found to be similar to urea in its inhibitory ability at temperatures below 175° C. Based on results from analysis of quenched residues, the use of more than 5 wt-pct magnesium oxide is recommended.

Jan 1, 1982

By Siavoljub D. Maksimovic

The Bureau of Mines, through a cooperative agreement with Duquesne Light Co. of Pennsylvania, field tested a method of using pneumatic stowing of crushed limestone to construct seals in long-abandoned mine openings that were part of an active mine closed shortly before sealing. A total of 13 openings at 11 sites were backfilled. In pneumatic stowing, material is conveyed through a pipeline and into the mine opening under low air pressure. The stowing equipment consists of a power sup-ply, a blower, a feeder to inject material into the pipeline, and a nozzle for directing the placement. Material is ejected from the nozzle at high velocity, creating a high-compaction fill upon impact. The fill material used was well-graded limestone aggregate up to 1-1/2 inches in diameter, with sufficient fines. This fill was modified at five locations by the addition of portland cement, expansive cement, and/or bentonite. The pneumatic stowing method is safer and faster than conventional methods, is cost competitive, and eliminates or reduces the exposure of workers to possible hazards since the nozzle can be kept outside the mine opening. The equipment is mobile, but some modifications in the technique would improve performance. The technique was used at remote locations where other methods could not be used without disturbing the environment.

Jan 1, 1982

By Slavoljub D. Maksimovic

The Bureau of Mines, through a memorandum of agreement with the State of Ohio, tested a method of constructing seals in abandoned mine openings in Ohio by means of pneumatic stowing of crushed limestone and gravel with sand. A total of five openings and one shaft were back-filled. Pneumatic stowing uses compressed air to convey material through a pipeline and into the mine opening. The stowing equipment consists of a power supply, a blower, a feeder to inject the material into the pipeline through an airlock, and a nozzle for directing the placement. Material is ejected from the nozzle at high velocity, creating a high-compaction fill upon impact. Well-graded aggregate up to 2 inches in diameter and having sufficient fines is used as fill. The stowing method is safer and faster than conventional methods, is cost competitive, prevents trespass into abandoned mine openings, and eliminates or reduces the exposure of workers to possible hazards since the discharge nozzle can be kept at the mouth of the opening. The equipment is mobile, and, with some modification, the technique could be widely used for sealing abandoned and active mine openings, even in remote locations and during severe weather conditions.

Jan 1, 1982

By C. E. Jordan

The Bureau of Mines conducted tests on seven samples of Florida phosphate operations.slimes to develop a method to recover phosphate presently being discarded because of its small grain size. A system of hydrocyclones and hydroseparators was used to recover up to 96 pct of the plus 400-mesh material from the slimes. This plus 400-mesh material was subjected to fatty acid flotation, and concentrates containing up to 33.4 pct P205 were produced. As much as 88 pct of the phosphate (P205) was recovered from the plus 400-mesh material, and up to 29.6 pct was recovered from the total slimes.

Jan 1, 1982

By K. P. V. Lei

The Bureau of Mines as part of its research effort to minimize the generation of hydrometallurgical waste, investigated a sodium sulfide leaching-electrolysis procedure for treating hydrometallurgical residues for elemental sulfur and base-metals recovery. Research was conducted on a leaching residue from a lead concentrate. The following procedure was developed. 1. The elemental sulfur was dissolved as polysulfide with an Na2S solution. 2. The resultant metal sulfide bearing residue was oxidatively acid leached in a cationic membrane electrolysis cell; the metals were solu¬bilized at the anode, and a base was generated at the cathode. 3. The elemental sulfur was recovered from the polysulfide solution by neutralizing with the acid in the anolyte. Byproducts of the neutralization were H2S and a sodium salt solution. 4. Sodium sulfide was regenerated by reacting the H2S byproduct with the base in the catholyte. 5. Lead as PbCL2 was recovered from the anode residue by brine leaching, and the other metals were recovered from the sodium salt solution as metal sulfides. 6. The barren filtrate from the metal sulfide precipitation constituted the recycled electrolyte. Ninety-eight percent of the elemental sulfur, 98 pct of the lead, and up to 80 pct of other accessory metals were recovered from a residue obtained from the FeCl3-NaCl leaching of a lead concentrate.

Jan 1, 1982

By R. H. Lien

The Bureau of Mines has conducted research on a flue gas desulfurization (FGD) process as part of its goal of minimizing the undesirable environmental impacts associated with sulfur dioxide (S02)-bearing waste gases. This FGD process, referred to as the modified citrate process, involves absorption of S02 in a buffered citric acid solution. The absorbed S02 is subsequently stripped from the solution using steam, which regenerates the solution and produces a wet S02 product. This product can be further processed to make sulfuric acid or liquid S02. Economic evaluations showed the process to be expensive when the stripper was operated at or near ambient pressures because of the large amounts of steam required for solution regeneration. Research was directed at reducing steam consumption in the stripper. The effect of stripper pressure on steam consumption was investigated. A process research unit (PRU) was operated with the stripper pressurized in the range of 5 to 150 psig. Test results showed that steam consumption decreased with increased stripper pressure. For example, when operating the PRU stripper at 150 psig, 4.1 grams of steam per gram of S02 was required to remove 90 pct of the S02 from a 1.0-vol-pct-S02 gas. This compares to 7.1 grams of steam per gram of S02 required for 90-pct S02 recovery at 5 psig.

Jan 1, 1982

By Robert J. Timko, Edward D. Thimons

Sulfur hexafluoride (SF6) is an odorless, colorless, nontoxic gas that has found acceptance as a tracer gas in research on ventilation pat- terns, measurement of air leak rates, respirable dust reductions due to bagging hood modifications, and the study of airflows relating to gob boreholes. Following a short review of the SF6 sampling technique, this report describes recent Bureau of Mines projects in which SF6 was used successfully as a tracer gas, enabling researchers to acquire representative data quickly and inexpensively.

Jan 1, 1982

By Theodore L. Turner

This Bureau of Mines report describes calcination of kaolinitic clay in a direct-fired 2-1/2- by 24-ft rotary kiln at 750° and 775° C. Methods for preparing kaolin feed materials and characterization of calcined products are discussed. Approximately 99 pct of the alumina in a typical eastern Georgia kaolin was soluble in HC1 after calcination at either 750° or 775° C.

Jan 1, 1982

By J. I. Paige

The Bureau of Mines studied methods for recovering unreacted titanium minerals and petroleum coke from titanium chlorination plant wastes prior to neutralization treatment with lime. The objective was to recover valuable raw materials and to reduce the amount of waste materials that must be treated for disposal. Samples of solid wastes were physically beneficiated by gravity concentration (tabling) to recover titanium minerals containing 69.0 to 92.4 wt-pct Ti02 and by selective carbon flotation to recover petroleum coke containing 94.0 to 96.8 wt-pct C. Laboratory data indicate that the recovered titanium mineral would decrease the amount of solid waste to be disposed of from 32.8 to 53.9 wt-pct. The recovery of coke would further decrease the amount by additional 32.9 wt-pct. Preliminary tests conducted on recovering vanadium, chromium, and columbium from liquors obtained by leaching chlorination residues also have shown that (1) 97 pct of the vanadium was extracted from leach liquors in a two-stage solvent ex-traction procedure and (2) 58 pct of the columbium and 40 pct of the chromium were separated from the leach liquors by an ion exchange technique using a strong acid resin.

Jan 1, 1982

By John A. Breslin

The Bureau of Mines measured respirable dust in coal mines by means of multiple dust samplers worn by persons moving about the mines. The measurements were made primarily to evaluate the effectiveness of certain dust-control techniques; however, for this report, the data have been analyzed to determine the precision of the personal dust-sampling measurements. A total of 68 sets of measurements were available from multiple personal samplers. The measured dust masses were less than 1.0 mg because the sampling times were short. The coefficient of variation calculated from these data was 18.5 pct, compared with coefficients of variation ranging from about 10 to 30 pct, which were calculated from the most precise and extensive data available for fixed-point dust measurements made in coal mines. From this comparison, it is concluded that dust samplers worn by personnel are as precise as fixed-point samplers in measuring respirabe coal dust; the wearing of the samplers by someone moving about a mine does not contribute significantly to the variation in measurements made with these instruments.

Jan 1, 1983

By Annie G. Smelley

As part of its program to develop technology that will encourage maximum utilization of the Nation's mineral resources, the Bureau of Mines conducted research on debrining potash-clay waste slurries by means of flocculation with a high-molecular-weight polymer and subsequent solid-liquid separation on a rotating trommel screen. In laboratory batch tests, potash-clay waste slurries were consolidated from initial clay contents of 8 pct to final contents of 30 pct with a polymer dosage of 1.2 Ib/ton of dry clay waste. Small-scale continuous tests yielded debrined products containing 20 pct solids using a polymer dosage of 1 Ib/ton of dry clay solids.

Jan 1, 1983

By Roy C. Bartholomae

This Bureau of Mines report presents the results of a laboratory investigation of coal cutting mechanics and noise. These experiments were performed using linear cutting apparatus that operates over a broad cutting speed range. The influence of several coal cutting parameters on the noise, force, productivity, and specific energy associated with linear cuts was ascertained. Some basic theoretical aspects of coal cutting mechanics and noise generation are discussed, and the results of the laboratory experiments are used to formulate analytical models of the coal cutting forces and noise. The analytical model for coal cutting noise is then generalized to account for the more important effects of rotary cutting. Based on the generalized model, an estimate of the sound pressure level at an operator's position is made for a typical continuous mining machine. It is concluded that by employing linear rather than rotary cuts, using deeper depths of cut, slower cutting speeds, and more efficient cutting tools, it is possible to reduce the level of coal cutting noise, as well as provide benefits to other important areas of health and safety in underground mining.

Jan 1, 1983

By R. S. Olsen

The Bureau of Mines is engaged in research to recover aluminum from kaolinitic clay and other nonbauxitic domestic resources. As part of this work, calcined Georgia kaolin was prepared by a process that prevents slime formation and makes the leached residues fast settling and easy to filter. The leaching reaction for calcined kaolinitic clay in a 5 pct stoichiometric excess of boiling 23-to 26-pct HCI was found to be zero order. Rate constants based on the weight-fraction of aluminum in the clay were found to be between 0.095 and 0.15 min-1 depending on feed preparation and leaching parameters. The mathematical relationships between aluminum extraction and time for both batch and continuous, stirred-tank operations were derived and verified experimentally.

Jan 1, 1983