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By S. C. Termes

The Bureau of Mines conducted research on the flocculation of various minerals with insoluble cross-linked starch xanthate (ISX) to determine its potential as a beneficiation technique for low-grade, highly dissem-inated ores and for selective desliming. Covellite, chalcocite, pyrite, pyrrhotite, chalcopyrite, bornite, sphalerite, galena, and molybdenite fines flocculate with ISX. Floc formation, floc size, and settling rate are dependent on pH, with the pH dependence differing for each mineral. Quartz is not flocculated by ISX. Experiments to obtain selective flocculation of sulfides from quartz were attempted. Good selectivity was only obtained for the bornite-quartz system. postflocculation separations resulted in flocculated bornite in grades as high as 92 pet. Evidence is presented that the flocculation of many of the sulfide minerals with ISX may involve covalent bonding of the xanthate group to lattice metal site(s).

Jan 1, 1983

By S. C. Termes, P. E. Richardson, R. L. Wilfong

"The Bureau of Mines conducted research on the flocculation of various minerals with insoluble cross-linked starch xanthate (ISX) to determine its potential as a beneficiation technique for low-grade, highly disseminated ores and for selective desliming. Covellite, chalcocite, pyrite, pyrrhotite, chalcopyrite, bornite, sphalerite, galena, and molybdenite fines flocculate with ISX. Floc formation, floc size, and settling rate are dependent on pH, with the pH dependence differing for each mineral. Quartz is not flocculated by ISX. Experiments to obtain selective flocculation of sulfides from quartz were attempted. Good selectivity was only obtained for the bornite-quartz system. Post flocculation separations resulted in flocculated bornite in grades as high as 92 pct. Evidence is presented that the flocculation of many of the sulfide minerals with ISX may involve covalent bonding of the xanthate group to lattice metal site(s). INTRODUCTIONBecause of the increasing interest in selective flocculation as a beneficiation technique for low-grade, highly disseminated ores and for selective desliming, the Bureau of Mines has been investigating the flocculation behavior of several cross-linked starch derivatives containing chelating groups. This report dis cusses the flocculation of sulfide mineral fines by insoluble cross-linked starch xanthate (ISX).Polymeric materials such as ISX, which contain a chelating group of known re¬activity towards specific mineral surfaces, were first proposed by Slater, Clark, and Kitchener (1), 3 Kitchener (2), and Attia and Kitchener (3) as selective flocculants for mineral fines with particle aggregation possible through a bridging mechanism. ISX appeared to be attractive as a sulfide mineral flocculant because (1) alkyl xanthates are known to react selectively with sulfide minerals"

Jan 1, 1983

By Bruce D. Hanson

The Bureau of Mines conducted a series of ignition tests with two types of conical bits (plumb bob and pencil) used on continuous mining machines, to determine their ignition potential at various bit speeds, cut depths, and wear conditions. The tests were conducted using single bits mounted on a 34-in-diam drum in a Bureau ignition test facility. The bits impacted blocks of Berea sandstone in a 6.5 pet methane atmosphere at various bit speeds and cut depths. In a new condition, the plumb bob bits were considerably more incendive than the pencil bits, causing ignitions in 32 of 35 tests at 60 rpm, compared with ignitiolls in 2 of 22 tests for the pencil bits. The results from new bit testing also show that reduction of bit tip velocity to 180 fpm does not eliminate ignition potential. When subjected to progressive wear, bits of both types were more incendive when they were locked in place, unable to rotate, than when they were free to rotate.

Jan 1, 1983

By J. M. Riley

The Bureau of Mines investigated a promising new technology for recovering A1203 from alunite to support the Bureau's alumina miniplant project. Results are presented for a study of the technical feasibility of treating alunite crushing and grinding reject fines for recovery of A1203. Alunite pellets having sufficient strength and resistance to degradation were produced by combining fines and coarse alunite with a KOH binder. The best pellets were prepared, in a laboratory pelletizer, by adding 1 pct KOH as a 5-pct solution to a mixture of 40 pct alunite dust (98 pct minus 65 mesh) and 60 pct coarse alunite (minus 20 plus 65 mesh). Calcines suitable for K2SO4 and A1203 recovery were produced by reducing dehydrated alunite pellets with sulfur in a laboratory shaft furnace for 4 h at 600° C, followed by air oxidation of the reduced calcine for 1 h at 600° C. This report presents design calculations, schematic diagrams, and discussions of the essential features of a proposed process research unit (PRU)--a continuous, 6-lb/h alunite shaft furnace--for studying the process.

Jan 1, 1983

By M. Hayashi

The Bureau of Mines conducted laboratory studies on low-grade vanadiferous silicates from the Pumpkin Buttes and Nine Mile Lake deposits of Wyoming to examine techniques for extracting vanadium and uranium. Recovery from low-grade sources such as these could contribute to future vanadium production and reduce reliance on vanadium imports. The Pumpkin Buttes samples contained 0.03 to 0.04 pct V205 and 0.06 to 0.12 pct U308; the Nine Mile Lake samples contained 0.02 to 1.0 pct V205 and 0.06 to 0.19 pct U308" Leaching the Pumpkin Buttes samples for 18 h at 800 C with addition of 200 lb/ton H2S04 resulted in recoverey of 80 pct of the vanadium contained in the samples. The Nine Mile Lake samples were readily leached, yielding 78 to 94 pct of the vanadium after 3 h at 800 C with addition of 100 lb/ton H2S04, A solvent extraction procedure was used to selectively recover urani-um from Pumpkin Buttes and Nine Mile Lake leach solutions and to recover vanadium from the raffinates. In batch shakeout tests, Alamine 336 recovered over 95 pct of the uranium from leach solution adjusted to pH 1. Di-2-ethylhexyl phosphoric acid and Cyanex 272 recovered vanadium from the uranium raffinate after reduction and adjustment to pH 2; vanadium extractions of up to 96 pet and 92 pct, respectively, were achieved.

Jan 1, 1985

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 P. M. Brown

The Bureau of Mines is investigating a dewatering technique for coal-clay waste that uses a flocculant, polyethylene oxide (PEO). This flocculant forms strong stable flocs that can be dewatered on a static screen. A field test unit (FTU) using this technique was operated at approximately 400 gal/min, using a waste stream from the flotation circuit of a coal preparation plant. Consolidated coal-clay material con-taining 55 to 60 pct solids was produced when the flotation circuit slurries of 2.7 to 8 pct solids were treated with 0.1 to 0.3 Ib PEO per ton of solids. The FTU was also operated at 64.5 and 87.5 gal/min using a portion of the underflow slurry from the preparation plant's thickener. Consolidated coal-clay material containing 55 to 60 pct solids was produced when the thickener underflow slurries of 19 to 24 pct solids were treated with 0.08 to 0.2 Ib PEO per ton of solids. PED-treated materials continued to dewater when placed in a pit.

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