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By Robert M. Doerr

In a process being investigated by the Bureau of Mines for recovering alumina from domestic nonbauxitic resources, calcined kaolinitic clay is leached with hydrochloric acid. Iron impurity in the clay is coleached and is removed in a solvent extraction step prior to crystallization of aluminum chloride hexahydrate, which is subsequently thermally decomposed to alumina. The FeCI3-HCl stripping liquor from the solvent extraction step is unsuitable for discharging to the environment; furthermore, economics requires recovery of the contained chloride values. In the present research, it was shown that the stripping liquor can be reacted with calcined clay to yield AlC13 in solution, plus precipitated iron oxides, residual silica, and unreacted excess clay as mixed solids. For the recovery of the AICl3 solution, the slurry could be separated or returned to the clay-HCI process stream at the solids washing step that follows primary HCI leaching of the clay. For the range 20° to 99° C, the time (t) (103 sec) required to react the waste liquor with excess clay, for essentially complete iron precipitation, depends on the absolute temperature (T) chosen, according to the expression t = e[(9.000/T) -23.5J. (1) Alumina was tried as a reagent alternative to clay but was not very effective, even under pressure and at high temperatures.

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 Nancy S. Raymon

The Bureau of Mines investigated the effect of controlled additions of selected metal oxides, as well as the adjustment of the calcia-to-silica ratio on the high-temperature strength of refractory-grade periclase. Increases in the hot flexural strength of some periclase materials in the range of threefold to fourfold were obtained with additions of Zr02 and by adjustment of the CaO:Si02 ratio to the 2.5 to 3.0 level. Results show that for each periclase refractory raw material, there exists a combination of level of Zr02 addition and an adjustment to the CaO:Si02 ratio that optimizes the hot flexural strength of each of these materials. Data also indicate that the improved hot strengths can be attributed to the high-temperature secondary phases formed between the different levels of periclase impurities and the additives, resulting in improved intergranular high-temperature bond strength.

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 Connie S. Musulin

The Bureau of Mines conducted an experiment at Exxon Mineral Co.'s Buffalo Shaft Operation to determine the time required for radon concentrations to return to a base average after fan shutdowns. Shutdown times ranging from 5 min to 16 hr were evaluated. An equation was derived to calculate a ratio that determines the time required for the radon concentration to return to the average level that existed in the mine prior to shutdown. For fan shutdowns of 15 min or more, underground personnel should be evacuated to areas with natural downcast ventilation. For shutdowns of less than 1 hr, personnel should not return to the working area until the elapsed time is four times the shutdown, or until the working area is resampled and found safe. If the mine is not in production during weekends, the downcast fans can be turned off .from midnight Friday until 4 p.m. Sunday, and the radon daughter concentration should be below 1 WL throughout the mine by the start of the shift Monday. This fan shutdown would conserve energy and save the mining company an estimated $21,000 each year.

Jan 1, 1982

By L. W. Brandt

As part of its objective to expand the body of mineral information as a basis for new technology, the Bureau of Mines conducted research on the fundamental behavior exhibited by phosphate clay waste in settling ponds. A semiempirical equation used to describe the compaction of ceramic powders in a single-acting die was applied to aqueous phosphatic clay waste and attapulgite slurries. This equation, [*V = a1 e ?k1/P + a2e ? k2/P] was found to describe the compaction of an attapulgite gel and a phosphate slime gel by a moving screen. [*V] is the ratio of the compaction achieved at a given pressure, P, to the compaction achieved at a pres-sure sufficient to remove all space between particles. The constant al represents the fraction of compaction achieved at low pressure by rearrangement of floes to higher packing density, and a2 represents the fraction of compaction achieved at higher pressure resulting from removal of voids within floes. K1 and K2 are constants determined from the experimental data. Both the low-pressure and high-pressure compaction mechanisms were observed in the compaction of the clays. These two compaction mechanisms offer an explanation for the observation that impounded slimes initially dewater rapidly and then dewater at a much slower rate.

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 D. C. Fleck

The Bureau of Mines, in a cooperative research program with four lead companies, has investigated ferric chloride leaching of galena to prepare lead chloride for molten-salt electrowinning to produce lead metal. The hydrometallurgical-electrolytic process is an alternative to the sintering-smelting-refining process currently used to produce lead metal and avoids the environmental problems associated with a conventional smelter. During investigations on the electrowinning aspects of the work, it was noted that certain cations, moisture, and sulfate in the electrolyte affect lead metal purity, cell voltage, current efficiency, and viscosity of the electrolyte. Results of bench-scale tests are re-ported on the effects of CaCI2, CuCI2, FeCI2, MgCI2, NaCI, ZnCI2, PbS04, and moisture on electrolysis. As impurities increased in the electrolyte, current efficiency decreased. CaCI2, CuCI2, and FeC12 decreased current efficiency by 12 to 47 pct. ZnCl2 gave a small voltage increase, while CaCI2 addition equivalent to 4.9 pct Ca caused a 50-pet increase in voltage. The lead metal was contaminated in direct proportion to the CuCI2 buildup in the electrolyte, Anode corrosion was observed with MgCI2 and MgC12?6H20. Viscosity increased appreciably with the buildup of NaCI, CaCI2, and sulfate. Electrolyte foaming occurred with ZnC12, MgC12?6H20, MgC12, FeC12?2H20, and FeCI2. Moisture inhibited the coalescence of the lead metal.

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

By M. J. Ferrante

The Bureau of Mines determined the enthalpies of Ni3S2 relative to 298.15 K to provide new thermodynamic data for advancement of mineral science and technology. Enthalpies were measured with a copper-block calorimeter from 298.15 to 1,197 K. A solid-solid transition was found at 834±1 K, with an isothermal heat absorption of 13.32 kcal/mol. The temperature of this solid-solid transition was accurately measured by differential scanning calorimetry. Because Ni3S2 does not melt congruently, the heat of fusion of 4.70 kcal/mol was obtained by extrapolation of enthalpy measurements from the solid and liquid phases to approximately 1,064 K. Tabulated values are given for the relative standard enthalpy, heat capacity, entropy, and Gibbs energy function between 298.15 and 1,800 K. Enthalpies are also given in equation form and combined with data from the literature to derive values of standard enthalpies of formation and Gibbs energies of formation. Similar calculations were made for the reaction of crystalline and liquid nickel with gaseous diatomic sulfur for Ni3S-2(c, l).

Jan 1, 1982