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By P. L. Sibrell

The U.S. Bureau of Mines has tested cyanide leaching for recovery of palladium (Pd) from spent petroleum processing catalysts. Three different catalyst samples were supplied by a spent-catalyst processor. These catalysts consisted of a zeolite base and contained 0.4 to 0.7 pct Pd. During alkaline cyanide leaching, the catalysts exhibited ion-exchange properties due to their zeolite matrices. Hydrogen ions were released from the zeolite in exchange for sodium ions in solution, resulting in a significant decrease in solution pH. This could present a safety hazard because of the potential for release of toxic hydrogen cyanide gas. A pretreatment step where the catalysts were contacted with a 1.0M sodium hydroxide solution was found to prevent the pH shift from occurring. Following the sodium hydroxide pretreatment, two stages of leaching at 160 °C with solution containing 1 pct sodium cyanide and 0.1[M] sodium hydroxide gave at least 75 and up to 95 pct Pd recovery. The Pd was quantitatively recovered from the leach solution by thermal decomposition in an autoclave at 250°C for 1 h. The Pd content of the precipitate was over 50 pct. Thermal decomposition also decreased the total cyanide content of the barren solution to less than 0.2 mg/L. The catalyst leach residues passed the Federal Toxicity Characteristic Leaching Procedure and the California Waste Extraction Test, indicating that landfill disposal of the leach residues would be acceptable.

Jan 1, 2010

By N. B. Greninger

The U.S. Bureau of Mines conducted explosion tests on various full-scale cementitious bulkheads used in abandoned mine areas to evaluate the ability of the bulkheads to withstand gas explosion over-pressures of 20 psig. Tests were performed on 120-ft2 solid-concrete-block seals of varying thicknesses and designs. Of the seven solid-concrete-block seals tested, only the standard-type seal, having a 16-in thickness, keyed at the floor and ribs, all joints mortared, wedged at the roof, and a center pilaster, maintained its integrity when subjected to a 20-psig pressure wave. After being subjected to repeated explosions, the standard seal only showed a small hairline crack and had an air leakage of 87 ft3/min at a pressure differential of 1 in H2O. Tests were performed on cementitious foam seals of varying thicknesses and compressive strengths. Explosion tests have shown that 200-psi strength, 4-and 8-ft-thick seals can withstand a 20-psig pressure wave. At a pressure differential of 1 in H20, no air leakage was detected through the 200-psi, 8-ft-thick foam seal.

Jan 1, 2010

By Arden D. Fugate

This work was conducted to determine a feasible process for converting siliceous fluoride offgases to a commercially usable product. The offgases were generated by pyrohydrolytic defluorination of low-grade fluorspar in a gas-fired rotary kiln, and fluorine was collected as a hydrofluoric-fluosilicic acid. A silicon-free fluoride solution for further processing was then produced by neutralizing the acidic scrubber solution with anhydrous ammonia, silicon being separated as orthosilicic acid. Ninety to ninety-nine percent of the fluorine originally present remained in solution as ammonium fluoride. Silicon was also separated from synthetic fluosilicic acids, having F-to-Si weight ratios ranging from 3.50 to 14.3. The solutions below a ratio of 4.06, the F-to-Si ratio of H2SiF6, containing dissolved silicon were desiliconized as completely as those containing less than the stoichiometric quantity of silicon. An electrolytic-grade cryolite was recovered from the ammonium fluoride solution by reacting with either sodium aluminate or alumina trihydrate and sodium hydroxide. A product containing 97 to 100 percent of the fluorine, represented by Na3A1F6, was recovered, and 94 to 99 percent of the theoretical yield was realized.

Jan 1, 1963

By M. E. Tyrrell, C. W. Houck

Mixtures of zirconium diboride and refractory metals of group VI were resistance sintered to high - density compacts using modified electric welding equipment . To evaluate the use of chromium , molybdenum , or tungsten as binders for zirconium diboride the sintered compacts were examined in polished sections and tested for crushing strength , hardness , microhardness , oxidation rate , and resistance to mechanical shock . Chromium yielded the highest compressive strength , the greatest resistance to mechanical shock and oxidation , and a satisfactory Rockwell hardness . Molybdenum did not yield a satisfactory cermet . Tungsten yielded compacts having high microhardness but very low mechanical strength .

Jan 1, 1964

By H. E. Powell

A solvent extraction procedure was developed on a laboratory scale for recovering trisodium phosphate, zinc, and iron from waste phosphate sludge as separate products. The sludge was dissolved in hydrochloric acid, and iron was extracted as ferric chloride by isopropyl ether. Zinc was extracted by di-2-ethylhexyl phosphoric acid in kerosine. The efficiencies of the one-and two-stage extractions ranged from 98 to nearly 100 percent. Trisodium phosphate was recovered by crystallization from the raffinate. The value of two marketable products is considerably more than than the costs of the major reagent. The process was developed to permit recycling of values in this waste and to consequently reduce stream pollution from this source.

Jan 1, 1972

By Jack R. Woodyard

Bonding angles, promotion energies, and relative atomic sizes can be estimated through the solution of a set of algebraic equations generated from simple atomic models, and quantum mechanical parameters such as bond strength can be estimated from simple, hydrogenic form-wave functions. The precepts of The Engel-Brewer Theory are melded with the "Crystal Approximation Model" to produce atomic-structure models making these predictions, The two-valence-electron case is presented in this report. For the candidate atoms Be, Mg, Ca, Sr, and Ba the calculated promotion energies agreed within a few percent of their experimental values. These atomic parameters determine the possible crystal structure of the candidate atoms when alloyed. This is part of the effort at the U.S. Bureau of Mines to develop methods for alloy design in response to requirements for new high-performance alloys that conserve critical or rare materials.

Jan 1, 2010

By H. D. Jacobs

The Federal Bureau of Mines, as part of a program to insure future raw material needs for the iron and steel industry, undertook research to beneficiate the oxidized taconites from the western Mesabi range in Minnesota. The data presented were obtained by applying the Bureau-developed selective-flocculation/cationic-flotation process to the second of three oxidized taconite samples. These three samples are representative of an estimated 10 billion tons of ore analyzing 30 to 40 pct iron. The experimental work was performed in a 900-lb/hr pilot plant. Treating the ore sample (36.1 pct Fe) with the Bureau's process produced commercially acceptable concentrates averaging 63.5 pct Fe and 4.3 pct SiO2, with an average iron recovery of 84.6 pct.

Jan 1, 1980

During the period 1979 thru 1982. Multi Mineral Corporation conducted a mining research program at the United StAtes Department of the Interior's Bureau vi Mines Oil Shale Mining Environmental Research Facility in the Central Piceance Creek Basin, Rio Blanco County, Colorado. The program consisted of mining, environmental and geotechnical research data and. the results are described in this report.

Jan 1, 1983

By R. S. McClain

Continuous-circuit flotation and batch-scale precipitation tests were made by the Bureau of Nines to determine rejection of carbon and recovery of fluorine and aluminum compounds from aluminum reduction plant residues, About 40 to 60 pounds each of aluminum fluoride and cryolite are lost for each ton of aluminum produced. Gasoline and turpentine were satisfactory for floating carbon from both fresh water and saturated solution systems. Soluble fluorine and aluminum compounds were recovered by precipitation with sodium aluminate and carbon dioxide. Over 99 percent of the carbon was removed by flotation. Fluorine and aluminum recoveries up to 77 and 63 percent, respectively, were obtained in a combined precipitate and nonfloat product, In the fresh water system the combined product was mostly cryolite with some gibbsite. In the saturated solution system the product was mostly sodium fluoride, some cryolite, and minor amounts of gibbsite.

Jan 1, 1963

By Paul M. Tyler

Hafnium appears to be among the more abundant of the newly discovered elements . Though quite widely distributed in nature , its compounds chemically so resembled those of zirconium , its sister element , that it escaped detection until 1923 , when Coster and Hevesy announced the discovery of the element , to which they gave the name of " hafnium " , from Hafniae , the Latin name for Copenhagen , where their research work was performed . Hafnium has so far been found only as a minor constituent of zirconium minerals . Zirconium as an element was discovered more than 140 years ago , but only a few unimportant uses were found for the metal or its compounds until some 18 years ago ; it is still classed among the rarer commercial metals . It is not surprising , therefore , that hafnium has not yet found a definite place for itself in industry . Nevertheless it has commanded a considerable interest among scientists ; and in 1930 some 70 grams of perfectly pure oxide of hafnium were prepared in Europe . A commercial future for hafnium is already glimpsed in the radio industry , and its high melting point and electronic emissivity have already led to the taking out of patents for its use in radio tubes and incandescent electric lamp filaments and for the cathode surfaces of devices such as X- ray tubes and rectifiers .

Apr 1, 1931

By M. M. Fine

In an experimental study by the Bureau of Mines, in cooperation with National Lead Co., the roast-flotation process was found to be an effective means of upgrading certain cobalt-nickel stockpiles. The research was undertaken to determine whether the process could yield an enriched feed, with a minimum cobalt content of 6.0 percent, for the company refinery. The stockpiles (products of the company Fredericktown, Mo., milling operations) were essentially complex sulfides of cobalt, nickel, copper, lead, and iron, 1 sample of which contained 2.84 percent Co and 3.57 percent Ni. After a controlled oxidizing roast at 400° C., laboratory flotation with conventional sulfhydric reagents yielded an enriched concentrate analyzing 9.22 percent Co and 11.43 percent Ni, with recoveries of 84.9 and 85.8 percent, respectively. These are typical laboratory data; other data indicated higher grades were possible but at reduced recoveries. A brief, continuous campaign verified the applicability of the process to the raw material in question but was not continued long enough to establish optimum conditions. As a consequence, the results of the large-scale tests did not equal those obtained in the laboratory but definitely confirm the beneficiation possible from the roast-flotation process.

Jan 1, 1958

By A. G. Loomis

Although secondary-recovery methods have not been applied widely in California, it is apparent that increasing attention and effort must be given to this phase of recovery if the State is to maintain its high rank as a petroleum producer. Steadily increasing demands for petroleum products and decreasing rates of discovery of new oil fields, with rapid depletion of existing reserves, emphasize the prospect of an adverse situation of supply and demand in the not-far-distant future. If the trend of discoveries becomes more favorable or if more complete economic recovery of the oil in place can be obtained by secondary recovery, this situation can be averted. Not only are these reserves of economic importance to the petroleum industry for meeting increasing market demands; but economic reclamation of such reserves is an important conservation measure, which will prolong the productive life of many fields. Accordingly, progressive operators in California are alert to the possibilities of secondary recovery and have done much to implement such operations wherever feasible. Most current operations are of the pressure-maintenance type, in which the reservoir pressure is maintained or partly maintained by injecting natural gas to in-crease oil recovery. The possibilities of recovering additional oil from stripper fields by gas drive and water flooding (including water disposal) also are being tested in experimental field projects. Table 1 summarizes current gas-and water-injection projects in California.

Jan 1, 1952

By Jr. Frank Parrish

This report describes the performance of 17 selected water-injection projects producing from Pennsylvanian-and Permian-age reservoirs. Illustrations depict reservoir structure and thickness, and production and injection history. A selected bibliography of publications pertaining to area oil recovery and geology is included. Tabulations of field and reservoir data reveal marked differences in the projects. Increased oil recovery resulted from injecting water in most cases; however, seven projects recovered less oil than the operators anticipated. Oil recovery by water injection ranged from 0.2 to 262 bbl per acre ft, or 0.1 to 22.5 pct of the initial stock-tank oil in place. Major reasons suggested for poor performance include: (1) Adverse directional horizontal permeability, (2) channeling of injected water through fractures or zones of high permeability, and (3) lack of containment of injected water. One 330-foot-deep project is among the first successful shallow water-floods in north Texas. Another project is the first successful Canyon sand-stone waterflood reported in the area. Previous gas injection in two Cisco sandstone projects did not prevent the reservoirs from responding favorably to waterflooding.

Jan 1, 1965

By K. A. Johnson, H. F. Yancey

"INTRODUCTION Coals vary so widely in their burning characteristics that all coals prepared for domestic stoker use cannot be burned efficiently on every type of stoker. The overfeed stoker, a large number of which are in use in the Pacific Northwest, operates satisfactorily when burning low- to high-ash, noncaking bituminous or subbituminous coals, whereas on the clinkering-type, underfeed, bituminous stoker both caking and noncaking bituminous and subbituminous coals are burned, generally with ash contents below 12 percent and ash-softening temperatures between 1,800º and about 2,600º F. Because fly ash continues to be one of the most troublesome factors in domestic underfeed stokers, noncaking coals especially must be chosen carefully with respect to size composition, particularly as regards the exclusion of excessive fines. Their formation as a result of degradation in storage handling or because of crushing in .the stoker worm will increase the fly-ash nuisence.Bituminous and subbituminous coals with higher ash-softening temperatures and, often, higher ash contents have not been able to enter the domestic stoker-coal market in the Pacific northwest because clinkers are not formed readily during clinker-type underfeed-stoker burning, especially in mild weather, and because of the labor and attendant inconvenience required in handling larger volumes of ash. The work described in this report was undertaken to enable mines producing coals of the kind described to enter the stoker-coal markets. The anthracite stoker selected was one that conveys the refuse from the ash pit of the furnace and deposits it into one of two covered, dust-tight disposal cans."

Dec 1, 1945

By Ernest W. Johnson

In most underground iron mines in the Lake Superior district the active workings are at considerable depth. When additional openings into such. nines are needed, operating officials are eager to discover more efficient methods of constructing them. In recent years, openings into two mines in the district were made by the borehole method,-which employs chilled-iron shot as the cutting medium. Others were made by the churn-drill method, in which pilot hole is churn-drilled and subsequently reamed to a desired but relatively small diameter. Both methods are comparatively new and unique, at least in some phases and in their application.

Jan 1, 1946

By Jack W. Carlson

Considering the magnitude of today's public concern with critical mineral and fuel materials, regarding both their midterm and long term availability, the Nation is fortunate to have in place and operating the coordinated data systems of the Geological Survey and the Bureau of Mines. Under the supervision and policy direction of the Assistant Secretary--Energy and Minerals, these Department of the Interior agencies have long been responsible for important mineral activities in the Federal Government. Aside from their highly respected mineral industry publications such as the monthly Mineral Industry Surveys, annual Commodity Data Summaries and topical Professional Papers and Reports of Investigation, the Bureau of Mines and Geological Survey data bases and expertise have been readily available for use in emergency situations. Policymakers and decisionmakers in government have placed major reliance upon this ready mineral data and analytical capability in World War II, the Korean War, the recent price control era, and the Arab oil embargo.

Jan 1, 1975

By Walter Kawa

Bureau of Mines research on the hydrogenation of coal has been concerned with developing processes that could be used to supplement the Nation's petroleum and natural gas resources. Motor fuel was produced in a subsidized coal hydrogenation industry in Europe prior to 1945, but the process used is still not economical and other methods of producing liquid and gaseous fuels from coal are being investigated. As an aid to the planning of coal hydrogenation research, a literature survey was made of processes or methods of hydrogenating coal that differ from the subsidized or conventional process. This report contains a bibliography of unconventional methods of hydrogenating coal and a brief discussion of the economics of the conventional method. A general discussion of unconventional methods is included, and the advantages and disadvantages are pointed out where possible. The survey supplements a previous Bureau of Mines survey3 and a comprehensive review published in 1930.4

Jan 1, 1964

By J. D. Davis

THE carbonizing properties of one medium- and and five low-volatile coals from West Virginia and one high-volatile A and two medium-volatile coals from Pennsylvania were determined by 800° and 900° C. BM-AGA carbonization tests and expansion tests in the sole-heated oven. Plastic properties of the coals and the yields and quality of their cokes and other carbonization products were determined. The low-volatile coals comprised a mine and a coke-plant sample of Pocahontas No. 6-bed coal from the. Black Eagle No. 1 mine, Wyoming County, W. Va.; a mine sample of Pocahontas No. 6 bed from the Louisville mine, Mercer County, W. Va. ; Davy Sewell bed was sampled at the Twin Branch mine, McDowell County, W. Va.; and Fire Creek bed was sampled at the Dunedin No. 1 mine, Raleigh County, W. Va. The medium-volatile coals were from the Fire Creek bed, Laurel Creek mine, Greenbrier County, W. Va.; Lower Kittanning bed, Springfield No. 4 mine, Cambria County, Pa.; and Upper Kittanning bed, Springfield No. 6 mine, Clearfield County, Pa. The high-volatile A coal represented the Upper and Lower Freeport beds, Kent Nos. 1 and 2 mines, Indiana County, Pa. In addition to the coals listed, high-volatile A coal from the Pittsburgh bed, Warden mine, Allegheny County, Pa., a standard blending coal, was used in blends in this investigation.

Jan 1, 1950

By Philip C. Good

Preliminary studies showed that direct hydrolysis of H2SiF6 to SiO2 and HF at elevated temperatures was subject to many mechanical difficulties, and that corrosion of construction materials was a serious problem. Elimination of SiO2 from the HF product was generally poor. An alternative procedure, hydrolysis of lime-neutralized H2SiF6 by steam at 950° to 1,100° C, yielded a product very low in SiO2. Condensates containing up to 300 g/1 HF were prepared.

Jan 1, 1968

By E. E. Donath, L. L. Hirst, L. C. Skinner

Two processes are available for the production of synthetic fuels from coal high-pressure hydrogenation and the carbon monoxide-hydrogen synthe- sis. This paper presents some ideas and new developments in coal hydrogen- ation that have been incorporated in an estimate for the production of 30,000 barrels per day of liquid fuels, mainly gasoline. A few comparisons of the processes will be helpful before discussion of the details of pro- posed improvements in the hydrogenation process. The principle of the high-pressure hydrogenation process ie the addi- tion of hydrogen at pressurea in the range of 3,000 to 10,000 p.s.i. to coal at elevated temperature and with the help of catalysts. On the other hand, the principle in the Fischer-Tropsch synthesis is the complete break-down of coal into a mixture of carbon monoxide and hydrogen, followed by the catalytic combination of these two gasse into hydrocarbons or suitable catalysts. For the synthesis, moderately elevated pressures of about 350 p.8.1. will bo used in the immediate future, although it can be carried on at atmosphoric pressure with certain catalysts. The products of these two processes using coal as raw material are almost as differont as hydrocarbons can be. The products of the high-pres- sure hydrogenation of coal reflect the original constitution of the coal. They are, therefore, rich in ring compounds, both aromatic and naphthenic, but, due to the action of highly comprcesed hydrogen and catalyst, are satu- rated and very stable. These constituents give the gasoline a high octane number and excellent rich-mixture performance, combined with good gum and storage stability. Therefore, this gasoline is suitable for aviation gaso- line or base stock. The Diesel fuel can be hydrogenated to a centane number of 45 or higher, which is entirely satisfactory for operating normal Diesel

Dec 1, 1948