Method of producing of metal iridium powder from (trifluorophosphine) iridium hydride tetrakis
FIELD: process engineering.
SUBSTANCE: invention relates to method of producing iridium from (trifluorophosphine) iridium hydride tetrakis and may be used for production of high-purity metal iridium powder. Proposed method comprises ammonolysis of volatile complex compound of (trifluorophosphine) iridium hydride tetrakis Hlr(PF3)4 with conversion into nonvolatile iridium metallamine by water solution of ammonium. Then, iridium metallamine is dissolved in concentrated hydrogen nitrate and solution is evaporated. Evaporation over, residue is decomposed to sponge-structure metal iridium. Now, the latter is triturated, reduced in hydrogen flow and purified to high-purity iridium.
EFFECT: high-purity iridium powder.
The invention relates to a method for iridium from tetrakis(triptorelin)of iridium hydride and may be used to produce powder metal iridium.
The objective of the invention is to obtain iridium metal powder of high purity.
A method of obtaining pure iridium, where as the original substances using the concentrate of platinum group metals, in which iridium is in the form of metallic iridium. The method consists in the oxidation of iridium by fusing it with potassium nitrate, dissolved in Aqua Regia, then deposition in the form of hexachloroiridate ammonium. The residue purified by re-crystallization, mainly for the separation of platinum. After separation in a fairly pure state Sol calcined. Thus obtained metal iridium contains some amount of oxide, which restores when heated in a current of hydrogen. 
The difference of the proposed method of obtaining powder of iridium is that the original substance is tetrakis(triptorelin)iridium hydride.
The proposed method is the ammonolysis reaction of tetrakis(triptorelin)of iridium hydride followed by a chemical treatment, comprising the following steps:
1. The ammonolysis and evaporation of the solution;
2. Oxidation of the obtained emmakate nitrogen KIS the Auteuil and evaporation of the resulting solution;
3. Thermal decomposition;
4. The refinement.
The method is as follows.
The ammonolysis is carried out in a closed volume, capacity, lined with Teflon. In the capacity of the pre-fill water solution of ammonia in a molar ratio HIr(PF3)4:NH3=1:(19,4÷25). Tetrakis(triptorelin)iridium hydride from the tank supply precondensed in the capacity of ammonolysis, then defrost and stand capacity to fully interact tetrakis(triptorelin)of iridium hydride with an aqueous solution of ammonia. The resulting solution was evaporated in Teflon cookware at a temperature of 100÷200°C to plastic yellow-orange mass.
Obtained after evaporation of ammicht iridium in the form of a yellow-orange plastic mass is dissolved in concentrated nitric acid in a molar ratio HIr(PF3)4:HNO3=1:(40÷50). The solution is evaporated until dry in a dark blue residue.
Dark blue residue chopped, placed in a quartz boat and disposed in a vacuum at a constant pumping at a temperature of 700÷1000°C. thus Obtained metallic iridium sponge-like structure to a flat surface and hold dopostavleno in a stream of hydrogen at a temperature of 600°C.
Refining is carried out by a method based on obtaining soluble compounds of iridium, hexachloroiridate sodium, followed the by the dissolution and precipitation in the form of hexachloroiridate ammonium. Then hexachloroiridate ammonium restore in hydrogen to metallic iridium. 
Example 1. Using this method redesigned to 21.74 g of tetrakis(triptorelin)of iridium hydride. Received iridium metal powder with a yield of at least 99.9% of theoretical. Obtained by this method iridium low chemical purity predominantly contaminated with silicon, the material of construction of boats and classified according to GOST 13867-68 "products of the chemical. Denote purity" as iridium technical.
After refining the yield of the target product was 7,046 g, or 91,64% of theoretical. Iridium obtained by this method, the purity correspond brand I,9 GOST 13099-2006 "Iridium. Brand".
1. Handbook of rare metals. Ed. Vaitlusega. - M.: Mir, 1965.
2. Gbauer, Glemser, Globe and other inorganic synthesis Manual: 6 so V.5: TRANS. with it. Ed. Gbauer. - M.: Mir, 1982.
A method of producing powder metal iridium from tetrakis(triptorelin)of iridium hydride, including the ammonolysis of volatile complex compound tetrakis(triptorelin)of iridium hydride HIr(PF3)4with conversion in the non-volatile ammicht iridium aqueous solution of ammonia, dissolving emmakate iridium in concentrated nitric acid, evaporation of the solution, decomposition of the remainder of the metal is wow iridium sponge-like structure, his rubbing, dopostavleno in the stream of hydrogen and cleaned to high purity iridium.
SUBSTANCE: procedure consists in heating chemically active gas containing gaseous hydrogen. Further, the procedure consists in bringing oxide of refractory metal to contact with said heated gas in form of particles of pentaoxide of tantalum for reduction of tantalum pentaoxide in form of particles. Also, weight ratio of gaseous atomic hydrogen and tantalum pentaoxide in form of particles is over 1.5:1 at temperature from 1900 °K to 2900 °K with formation of primary metal of tantalum. Another version of the procedure consists in heating chemically active gas containing gaseous hydrogen. Oxide of refractory metal is brought into contact with said heated gas in form of particles of niobium oxide chosen from a group containing of niobium dioxide, niobium pentaoxide and their combination for reduction of said niobium oxide in form of particles. Weight ratio of gaseous hydrogen and niobium oxide in from of particles is at least 9:1 at temperature from 2100°K to 2700°K with formation of primary metal of niobium.
EFFECT: raised efficiency of production of primary metal of tantalum or niobium due to performing process in one stage.
24 cl, 4 tbl, 14 dwg
SUBSTANCE: invention refers to procedure for metal production. The procedure consists in reduction of metal oxides with hydrogen at presence of calcium hydride in heated closed reactor. Also stoichiometric amounts of reduced metal oxide and calcium hydride are spaced in the reactor at 15-20 cm one from another. The reactor is filled with hydrogen to pressure 0.1-0.3 at and metal oxide is heated at temperature 200-1000 °C, while calcium hydride at 80-120°C to complete reduction of oxide.
EFFECT: production of required amount of metals at minimal consumption of hydrogen.
3 ex, 1 dwg
SUBSTANCE: method includes homogeneous reduction of its volatile compounds by hydrogen in reactor made of refractory material at feeding with transportation by argon of volatile compound of reduced metal and hydrogen feeding into reduction zone. Reduction is implemented in reactor, consisting of evaporation zone and reduction zone, by means of feeding after evaporation from of volatile compound of metal into reduction zone. At usage in the capacity of compounds of halogenide metals or metal oxides into reduction zone it is fed correspondingly halogen-hydrogen or water vapors, at ratio of feed rates of hydrogen and argon 1:2 with receiving of metal in the form of metal foil, precipitated on heated walls of reactor. Device includes reactor, implemented of refractory material - fused quartz, treated material in the form of compound if the received metal, heater and feed system of gas. Reactor is implemented with quartz diaphragm for separation into evaporation zone and reduction zone, heated up to temperature 850-950°C separately by means of heaters.
EFFECT: increasing of metals grade at reduction of halogenides and oxides of metals.
2 cl, 1 dwg, 1 tbl, 3 ex
FIELD: process engineering.
SUBSTANCE: invention relates to metallurgy. Proposed method comprises zone chlorination of nickel metal in gaseous chlorine flow at 940 to 970°C to produce nickel chloride powder. Then, one-stage sublimation of nickel chlorides powder in atmosphere of humid argon at 940 to 970°C is carried out to produce nickel chloride vapors and diffusion recovery of nickel chloride vapors in dehydrated hydrogen at 950 to 980°C to produced compact recovered nickel. Now, said foil and crystals are pressed and vacuum zone re-crystallization is effected to produce ingots. The latter are remelted in cooled flat crystalliser in vacuum to produce flat ingot to be remelted on both sides for complete depth, at least, two times. Invention covers also device to produce nickel chloride powder for dispersed targets and device for sublimation and homogeneous recovery of nickel chloride.
EFFECT: sharp increase in nickel purity.
3 cl, 2 dwg, 1 tbl, 1 ex
FIELD: process engineering.
SUBSTANCE: invention relates to metallurgy. Proposed method comprises zone chlorination of nickel metal in gaseous chlorine flow at 940 to 970°C to produce nickel chloride powder. Then, one-stage sublimation of nickel chlorides powder in atmosphere of humid argon at 940 to 970°C is carried out to produce nickel chloride vapors. After sublimation, homogeneous recovery of nickel chloride vapors is performed in dehydrated hydrogen flow at 950 to 980°C and hydrogen-to-argon-flow rate ratio of 1:2-1:3 to produce foil and recovered nickel crystals. Now, said foil and crystals are pressed and vacuum zone re-crystallization is effected to produce ingots. The latter are remelted in cooled flat crystalliser in vacuum to produce flat ingot to be remelted on both sides for complete depth, at least, two times. Invention covers also device to produce nickel chloride powder for dispersed targets and device for sublimation and homogeneous recovery of nickel chloride.
EFFECT: sharp increase in nickel purity.
4 cl, 2 dwg, 1 tbl, 1 ex
SUBSTANCE: processed material in form of cobalt powder is put into reactor made out of refractory material and heated to temperature 700-750°C; further de-hydrated hydrogen is run through reactor at rate of supply 300 ml/min during 60 min for heterogenic reduction of cobalt chloride to powder of metallic cobalt. Reduced powder of metallic cobalt is heated to temperature 600-650°C in the same reactor; flow of chlorine is run through the reactor at rate of supply 100 ml/min during 30 min for partial chlorination of metal cobalt with preferential formation of chlorides of volatile impurities. Powder of metallic cobalt undergone partial chlorination is pressed into a rod and is subject to electronic vacuum zone re-crystallisation for production of crystals of high pure cobalt. Produced crystals are subject to electronic re-melting in the crystalliser cooled from both sides to whole depth not less, than two times till obtaining a flat ingot with structure of high quality.
EFFECT: great increase of purity of cobalt designed for fine film metallisation by magnetron sputtering of targets as cobalt purity substantially determines electro-physical parametres of applied thin layers.
1 dwg, 1 tbl, 1 ex
SUBSTANCE: invention refers to metallurgy and can be used for fabricating of metallurgical briquettes which are effective substitutes of coke in blast and cupola iron production. The mixture is prepared which includes 94-98 mas.% of filling compound - a carbon containing material, and the rest is a binding material such as an activated aluminium- boron- phosphate concentrate. Then forming of mixture is performed in an accessory under pressure and vibration. Activation of the aluminium- boron- phosphate concentrate is performed before immediate preparation of mixture by means of the binding material treatment with nano second electromagnetic impulses of 0.5-0.8 MW power.
EFFECT: invention upgrades quality of metallurgical briquettes due to their increased strength characteristics at a minimal quantity of a binding material and at a considerable reduction of time for briquette fabrication owing to briquettes self hardening and avoiding thermal treatment.
2 tbl, 2 ex
SUBSTANCE: proposed method includes reduction of silver chloride at heating and holding at heat in flow of gaseous hydrogen, bubbling of gas escaping from reaction chamber through water and obtaining aqueous solution HCl. Reduction is performed from silver chloride formed at refining of noble metals and ground to size of ≤100 mcm and located in reaction chamber at thickness of layer of ≤20 mm at temperature of 450°C±5°C by gaseous hydrogen heated to holding temperature.
EFFECT: increased degree of extraction of silver from silver chlorides.
1 tbl, 1 ex
FIELD: spraying targets and methods of manufacture of such targets.
SUBSTANCE: proposed method includes making the blanket of metal to be sprayed which contains tantalum, niobium or their alloy, performing cold cross rolling of blank and cold treatment of rolled blank for obtaining shaped blank. Proposed target is made by above method; it contains at least one rectifying metal. Target is designed for magnetron with hollow cathode and is characterized by the following parameters: (a) size of grain acc. to ASTM 5 or finer; (b) combined texture (111)-(100); (c) homogeneous size of grains varying within ±2 acc. to ASTM or their combination. Assembly of spraying target includes target proper and upper part made from non-sprayable material and secured to side walls of target and/or outer envelope made from non-sprayable material and secured to target. Proposed method of extraction of rectifying metal from used target assembly includes hydrogenation of rectifying metal.
EFFECT: smooth destruction of target and smooth precipitation of material on substrate.
57 cl, 5 dwg, 2 tbl, 1 ex
FIELD: non-iron industry.
SUBSTANCE: invention relates to method for reducing of manganese oxide from ore to manganese carbide. Solid metal oxide is brought into contact with gaseous reducing and cementation agent (e.g., hydrogen-hydrocarbon mixture), and optionally, with inert gas at temperature of 1000-12500C.
EFFECT: environmentally friendly method; decreased energy consumption.
21 cl, 22 dwg, 1 tbl
SUBSTANCE: procedure for purification of zinc sulphate solution from impurities consists in hydrolytic purification with preliminary iron oxidisation in two stages: first with diluted solution of hydrogen peroxide at temperature 20-55°C and consumption 0.95-1.1 of stoichiometric required amount, then with manganese dioxide contained in electrolytic slime of zinc production.
EFFECT: complete or partial avoiding expenditures for costly oxidant - manganese ore and reduced contents of foreign impurities in zinc sulphate solution.
SUBSTANCE: invention relates to metallurgy of noble metals, in particular, to method of processing nitration hydroxides in refinery of platinum metals containing chalcogenides, tin, arsenium and platinum group metals, gold and silver. Proposed method comprises leaching of hydroxides and extracting basic metal compounds from the solution. Hydroxide leaching is carried out for 1-2 h by alkali solution with concentration of 140-180 g/l with l:S ratio varying from 3:1 to 4:1, temperature 80-90°C, and introducing hydrazine hydrate into pulp to reach OVP of minus 400-600 mV relative to reference silver-chloride electrode. Then, alkaline solution is separated from insoluble residue that concentrates platinum metals. Now, extraction of basic metals is carried out in processing alkaline solution by sulfuric acid to pH=4-5 to produce hydroxide precipitate of tin, arsenium, selenium and tellurium, and by filtration, or processing of alkaline solution by sulfuric acid to pH 0.5-1.0 along with adding iron powder to OVP varying from 0 to minus 100 mV, and filtration of obtained cementates obtained on the basis of selenium and tellurium, and processing the solution by alkali to pH = 4-5 with deposition of tin and arsenium hydroxides. Invention allows extracting up to 85% of Se and Te into target products, 90% of Sn and As into secondary hydroxides at minimum transition (less than 1%) into PMH.
EFFECT: over 99% of platinum metals left in refinery cycle, reduced processing cycle.
SUBSTANCE: procedure consists in concentrating refractory ore with successive concentrate fine crumbling to release gold with extracting solution and in mixing fine crumbled concentrate with wastes or by-products of concentrating to facilitate filtering said concentrate mixed with said wastes of concentrating. Here is also disclosed the installation for implementation of the said procedure.
EFFECT: increased rate of processing of refractory mineral ore avoiding harmful effect to environment.
14 cl, 4 dwg, 1 ex
SUBSTANCE: electrosorption carbon material is the cathode and is carbon fibric on which there is a layer a conducting polymer - poly-3,4-ethylenedioxythiophene or polyaniline which can chemically reduce ions of noble metals Ag, Au and Pd to metal state. Before passing the aqueous solution to the electrosorption carbon material, a negative potential between -0.5 and -0.3 V is applied relative a silver chloride electrode. Reduction takes place upon contact of the electrosorption carbon material with the aqueous solution in flow mode while feeding the solution at a rate of 10-20 ml per minute per square centimetre of the electrosorption carbon material. Concentration of the extracted metal in the solution is measured and the reduction process is repeated many times.
EFFECT: invention increases efficiency of extracting noble metals, shortens duration of the process of their separation and simplifies and lowers the cost of the extraction process.
4 cl, 3 ex, 1 dwg
SUBSTANCE: invention relates to chemical engineering of inorganic substances and can be used in cases when there is need to produce a nickel concentrate. The method of processing oxidised nickel ore involves mixing the ore with ammonium chloride, heating the obtained mixture and water leaching to obtain a solution. The ammonium chloride is mixed with the material in ratio of 100-150 mol % of the stoichiometric quantity. The mixture is then heated to temperature 200-315°C and kept at that temperature until release of ammonia, water and hydrogen chloride stops. After water leaching, ammonia water is used to precipitate iron and aluminium at pH 6, nickel and cobalt at pH 8-8.5 and manganese, magnesium and calcium at pH above 8.5.
EFFECT: design of industrial processing oxidised nickel ore to obtain a nicke-cobalt concentrate.
1 dwg, 2 ex
FIELD: technological processes.
SUBSTANCE: invention is related to production of highly pure tungsten for spattering targets. Method includes cleaning of ammonium paratungstate from admixtures by ammonia sulfide and further treatment of solution anion-exchange resin AM-p. Then thermal decomposition of ammonium paratungstate is executed at the temperature of 600-800°C to produce tungsten trioxide, as well as cleaning of tungsten trioxide by zone sublimation at the temperature of 900-950°C in continuous flow of oxygen. After sublimation, heterogeneous recovery of tungsten trioxide is carried out by hydrogen at the temperature of 700-750°C to produce tungsten powder, as well as tungsten powder pressing to produce bar. Then electronic vacuum zone recrystallisation of bar is carried out to produce crystals of highly pure tungsten, as well as electronic vacuum melting in flat crystalliser with melting of flat bar from each side to the whole depth at least twice. Device is also suggested for zonal sublimation of tungsten trioxide.
EFFECT: sharp increase in purity of tungsten intended for thin-film metallisation by magnetron spattering of targets.
2 cl, 2 dwg, 1 ex
FIELD: technological processes.
SUBSTANCE: invention is related to production of highly pure molybdenum for spattering targets. Method includes cleaning of ammonium paramolybdate in the form of solution from admixtures with ion exchange in neutral and alkalescent mediums on hydrated tin oxide and on weakly-basic anion-exchange resin AN-106. Then thermal decomposition of ammonium paramolybdate is executed at the temperature of 600-800°C to produce molybdenum oxide, as well as cleaning of molybdenum oxide by zone sublimation at the temperature of 750-800°C in continuous flow of oxygen. After cleaning, heterogeneous recovery of molybdenum oxide is carried out by hydrogen at the temperature of 700-750°C to produce molybdenum powder, as well as its pressing to produce bar. Then electronic vacuum zone recrystallisation of pressed bars is carried out to produce crystals of highly pure molybdenum, as well as electronic vacuum melting in flat crystalliser with melting of flat bars of highly pure molybdenum from each side to the whole depth at least twice. Device is also suggested for cleaning of molybdenum oxide by zonal sublimation.
EFFECT: sharp increase in purity of molybdenum intended for thin-film metallisation by magnetron spattering of targets, since purity of molybdenum to a large degree defines electrophysical parametres of applied thin layers.
2 cl, 2 dwg, 1 tbl, 1 ex
SUBSTANCE: invention relates to a method of reclaiming cyanide from aqueous solutions, particularly recycled water which contains thiocyanates CNS-. The method involves electrochemical oxidation of thiocyanates. Before electrochemical oxidation, recycled water, which contains from 2 to 20 g/l thiocyanates, is acidified to pH=2-3. Electrochemical oxidation is carried out at current density of not less than 750 A/m2 for 2 to 3 hours while simultaneously letting in air into the solution. The formed hydrogen cyanide is trapped in an absorption vessel with its output ranging from 70 to 80%.
EFFECT: reduced content of thiocyanates in recycled water with simultaneous reclamation of cyanide.
3 dwg, 1 ex
SUBSTANCE: invention relates to non-ferrous metallurgy and can be used at method of cleaning against chlorine of zinc-sulfate solutions, received at sulfuric acid leaching of secondary zinc raw material, containing chlorine. Method includes sedimentation of chlorine-ion in the form of copper-chlorine cake by addition of copper-bearing solution and copper cake, containing metallic copper. In the capacity of copper-bearing solution it is used solution, formed at sulfuric acid leaching of solid residue, received after solution of copper-chlorine cake in solution of sodium hydroxide. Additionally copper-chlorine cake is solved in the solution of sodium hydroxide at concentration 50-75 g/l.
EFFECT: reduction of consumption of flowing copper cake to cleaning of zinc-sulfate solutions against chlorine and reduction of costs for this process.
2 cl, 1 tbl
SUBSTANCE: method consists in diluting material with water and in treating pulp with nitric acid. Further, not dissolved material is separated, washed and chlorinated in hydrochloric acid and pulp is filtrated. Upon filtration hydrochloric acid solution is neutralised; sediment of impurities of non-ferrous metals is separated from solution containing noble metals. Also upon diluting pulp is treated with nitric acid to redox potential of 800-900 mV. Sodium chloride is introduced into obtained hydrochloric acid solution first, then formed silver salt is separated, solution is treated with sodium sulphate and lead salt is filtered off. Further, redox potential of solution is reduced to 300-450 mV by introducing light alloy containing copper for reduction of palladium and its precipitation. Then sediment is separated, and solution is neutralised with alkali; formed sediment containing copper is filtered.
EFFECT: upgraded degree of separation of non-ferrous and noble metals and extracting of silver, copper, and lead into selective product with low contents of platinum metals.
SUBSTANCE: procedure for processing sulphide mineral products using bacteria for extraction of metals consists in vat leaching crumbled sulphide mineral products in not less, than two serially connected vats and in mixing with solution of sulphuric acid at value of pH below 1.8, contents of solid phase 10-60%, concentration of ions of trivalent iron over 3 g/l, and temperature 50-99°C. Pulp is withdrawn from the last vat, is divided into solid and liquid phases and solid phase is returned to leaching into the first vat. Bacterial oxidation of iron in a liquid phase is performed in a separate reactor at value of pH 1.4-2.2, and temperature to 90°C with aeration and with addition of elements for bacteria feeding. Upon iron oxidation liquid phase is returned to the leaching vats. Metals are extracted from leaching phases.
EFFECT: increased extraction of metals and rate of process.
11 cl, 1 dwg, 2 ex