The method of obtaining titanium powder
(57) Abstract:Usage: in nonferrous metallurgy, to obtain titanium powders based on it. The inventive spend for magnesium recovery of titanium tetrachloride, and then pre-treatment of the reaction mass by vacuum separation to the content of magnesium chloride 5-12%, the reaction mass is then removed from the apparatus, is crushed to a particle size 0-12 mm and subjected to further purification by leaching or vacuum separation. Moreover, when the purification vacuum separation after grinding the reaction mass is pre-dried in vacuum at stepwise increasing temperature from 20 to 250oWith, then spend the vacuum separation, the apparatus is cooled and produce regrinding the sintered powders to the desired size. table 1. The invention relates to the field of nonferrous metallurgy, in particular, to a method for producing titanium powders.There are several ways to obtain titanium powders (1 Powder metallurgy of titanium. Ed. 2nd, Ustinov C. S. olasov Y. G. Drozdenko C. A. and other M metallurgy, 1881, S. 10-22): metallothermic recovery of titanium from its compounds; mechanical and chemical-mechanical grinding GUI method of dispersion liquid of titanium by spraying a jet of liquid metal neutral gas, either by rotation in an inert atmosphere melted in an electric arc titanium rod came out of the research phase.The main disadvantages of the method are:
the complexity of structural design;
the resulting granules have a hardened surface, which necessitates only their hot pressing with the use of expensive equipment (2 Titan. Abundant C. A., Petrunko A. N. Galitsky N.In. and other M metallurgy, 1983, S. 492-493).A known method of mechanical grinding of titanium sponge is applicable only for his low grades, i.e., for titanium, krupenko high content of impurities, because the pure metal is very soft, viscous, plastic. Obtained in this method, the powders are of low quality. To facilitate the operation of grinding is recommended kruptovoti sponge titanium by hydrogen saturation with subsequent dehydrogenation (3 Production and use of powders of titanium. Olasov Y., Ustinov C. S. Drozdenko Century A. Ukrniinti, Kiev, 1971, S. 4-16). The obtained powders due to the high specific surface enriched gas impurities. It is also proposed operation of grinding to make with the addition of inert fillers, such as ice (4 is swesty two directions electrolytic method of producing titanium powders: 1) the recovery of titanium from its compounds (TiCl4, Tio2and others) using an insoluble anode is at the stage of research; 2) recovery of titanium from the melt his chlorides using soluble anode of waste metal titanium brought to the stage of pilot projects. The disadvantages of this method are the high energy intensity and low productivity of about 80 kg/day (3 Production and use of powders of titanium. Olasov Y., Ustinov C. S. Drozdenko Century A. Ukrniinti, Kiev, 1971, S. 19).Known metallotrejderskih methods (reduction of titanium chlorides of sodium or magnesium and recovery of titanium dioxide by Gericom calcium) is most developed to an industrial scale, is the way nitratereductor recovery of titanium chlorides and subsequent hydrometallurgical treatment of the reaction mixture. The method has high performance; powders have good quality, well-pressed and are sintered. The disadvantage of this method is that due to the high activity of sodium (Flammability, vzryvaet) requires strict adherence to precautionary measures, and in addition, to obtain 1T titanium spent sodium in two times more than that of magnesium. In domestic proizvedeniya Tio2hydride calcium are very small, enriched gas impurities, powders with an average particle size of not more than 10 μm (I S. 11), which limits their field of application. Because of the low technical and economic efficiency of the method and of low quality powders interest in theoretical and technological developments of this method in recent years is not shown (2 Titan. Abundant C. A., Petrunko A. N. Galitsky N.In. and other M metallurgy, 1983, S. 492-493).A prototype of the proposed method is magnesium combined method of obtaining titanium powders (I Powder metallurgy of titanium. Ed. 2nd, Ustinov C. S. olasov Y. G. Drozdenko C. A. and other M metallurgy, 1881, S. 10-13). The method consists in the following. Tetrachloride to titanium metal restore magnesium technology current production of titanium sponge. The resulting reaction mass is subjected to a preliminary vacuum separation for cleaning from metal and magnesium chloride to 0.5 and 2-3 wt. accordingly: the cooled reaction mass after crushing (particle size fractions is not specified), sent for final clearance from chloride and magnesium metal leaching in hydrochloric acid rattlebrained experiments reaction mass content of 2.5-3% magnesium chloride according to their mechanical properties resembled a typical titanium sponge. Output fractions with grain size less than 12 mm was approximately 20%
the need to install special equipment for leaching the reaction mass at the enterprises of the current production of titanium sponge and disposal of large quantities of acid solutions.The objective of the invention is to increase the output of powder fractions due to the receipt of allospecies, krupjanoj high content of magnesium chloride the reaction mass.The problem is solved in that in the method of obtaining titanium powders, including magnesium recovery of titanium chloride, pre-treatment of the resulting reaction mass temperature vacuum separation, grinding her final purification crushed the reaction mass from volatile impurities by high-temperature vacuum separation or hydrometallurgical processing, it is new that pre-treatment of the reaction mass is maintained till the content of magnesium chloride 5-12% and grinding the reaction mixture is carried out until the particle size of the powder fractions 0-12 mm, and when the final cleaning vacuum separation after grinding the reaction mass is pre-dried and after Otello drying the reaction mass is performed in vacuum at stepwise increasing temperature from 20 to 250oC.Pre-vacuum separation to the content of magnesium chloride 5-12% allows to obtain a reaction mass less crust, which allows you to grind it to fine powder fractions (0-12 mm). When the content of magnesium chloride is less than 5% of the reaction mass is badly crushed not only by reducing the content of chloride, but also because of the increased duration of the separation process, and thus more strong sintering of the reaction mass. When the content of magnesium chloride above 12% in the reaction mass increased content of magnesium metal, which makes it grinding, but also more intensive hydrolysis of crystalline magnesium chloride by heating the reaction mass.When carrying out the final purification of high-temperature vacuum separation step, the heating of the reaction mass in the range 20-250owhen continuous vacuum treatment can improve the quality of the obtained powders.Received after the final cleaning vacuum separation of the sintered powders are subjected to regrinding to size according to customer's demands.Example.In a preheated 850oWith tightly closed lid, is in the amount of 2250 kg and for a given mode has fed 5200 kg of titanium tetrachloride (STF 05-01-243-89) so, to the utilization of magnesium was 58% Formed in the process of recovering magnesium chloride was poured on the adopted technology schedule. After the recovery process in the retort reactor remained 850 kg underutilized metal magnesium and about 250 kg Nelidovo magnesium chloride, which can not be drained completely due to the spongy structure of the reaction mass.After completion of recovery process, the recovery apparatus has parametervalue in the device separation and conducted a preliminary vacuum separation at a temperature 850-1020oC. the Process is finished when sudden pressure drop in the device separation and consumed in heating apparatus power, which indicates the end of the distillation of magnesium metal. The duration of the separation process accounted for 27% of the duration of the technological cycle. After cooling block of the reaction mass was removed from the retort reactor and selected 6 samples from the surface and from the center of the block to define it residual metal and magnesium chloride. On average it amounted to 0.4 and 9.2%, respectively. The reaction mass to grind to a particle size 0-12 mm loaded in the device separation and vacuumization. High-temperature exposure was carried out at 980-1000oWith over 30 hours. After cooling, the sintered product was grinded and scattered fraction of a desired size. Quality and granulometric characteristics of titanium powder are presented in table.1. 1. The method of obtaining titanium powder comprising magnesium recovery of titanium chlorides, pre-treatment of the resulting reaction mass temperature vacuum separation, grinding her final purification crushed the reaction mass from volatile impurities by high-temperature vacuum separation, or hydrometallurgical processing, characterized in that the pre-treatment of the reaction mass is maintained till the content of magnesium chloride 5-12% and grinding the reaction mixture is carried out until the particle size of the powder fractions 0-12 mm2. The method according to p. 1, characterized in that during final cleaning vacuum separation after grinding the reaction mass is pre-dried and after cooling produce regrinding the sintered powders to the desired size.3. The method according to PP.1 and 2, characterized in that the pre-drying of the reaction mixture produced in VA
FIELD: non-ferrous metallurgy, possibly production of highly purified powders of tantalum and niobium with large specific surface by metal thermal reduction.
SUBSTANCE: method is realized at using as corrosion protection means layer of halide of alkali metal formed on inner surface of vessel before creating in reaction vessel atmosphere of inert gas. Charge contains valve metal compound and halide of alkali metal. It is loaded into reaction vessel and restricted by protection layer of halide of alkali metal having melting temperature higher than that of charge by 50 - 400°C. Before loading charge, valve metal compound and alkali metal halide may be mixed one with other. Mass of protection layer of alkali metal halide Ml and charge mass Mc are selected in such a way that that to satisfy relation Ml = k Mc where k - empiric coefficient equal to 0.05 - 0.5. Gas atmosphere of reaction vessel contains argon, helium or their mixture. Fluorotantalate and(or) oxyfluorotantalate or fluoroniobate and(or) oxyfluoroniobate of potassium is used as valve metal compound. Sodium, potassium or their mixture is used as alkali metal. Chloride and(or) fluoride is used as alkali metal halide. Valve metal compound and alkali metal halide may contain alloying additives of phosphorus, sulfur, nitrogen at content of each additive in range 0.005 - 0.1% and 0.005 - 0.2% of mass valve metal compound respectively. Invention lowers by 1.3 - 2 times contamination of powder with metallic impurities penetrating from vessel material. Value of specific surface of powder is increased by 1.2 - 1.8 times, its charge is increased by 10 - 30 %, leakage current are reduced by 1.2 - 1.5 times.
EFFECT: improved quality of valve metal powder, enhanced efficiency of process due to using heat separated at process of reducing valve metal for melting protection layer.
9 cl, 1 tbl, 4 ex
FIELD: powder metallurgy, possibly production of finely dispersed powder of molybdenum, its composites with tungsten, namely for producing hard alloy materials on base of molybdenum and tungsten.
SUBSTANCE: method provides production of molybdenum and its composites with tungsten at temperature no more than 900°C and also production of materials in the form of finely dispersed powders. Method comprises steps of reducing compounds of molybdenum and tungsten (MoO3 and WO3) by metallic magnesium in medium of melt chlorides such NaCl, KCl or carbonates such as Na2CO3, K2CO3 or their binary mixtures such as NaCl - KCl, Na2CO3 - K2CO3, NaCl - Na2CO3, KCl - K2CO3 at temperature 770 -890°C. According to results of fineness analysis produced powder of molybdenum represents homogenous material having 80% of particles with fraction size 2.2 - 3 micrometers. Composition material depending upon Mo content includes particles with fraction size 5 - 15 micrometers.
EFFECT: enhanced efficiency of method.
1 tbl, 3 ex
FIELD: treatment of powdered, especially metal containing initial material introduced together with treating gas such as reducing gas for creating fluidized bed in fluidized bed chamber, for example in fluidized-bed reactor.
SUBSTANCE: treating gas at least after partial conversion in fluidized bed is removed out of fluidized bed and then outside fluidized bed it is partially recovered, preferably oxidized due to performing chemical, namely exothermal reaction with gaseous and(or) liquid oxidizer. Heat energy of such reaction at least partially is fed to fluidized-bed chamber, especially to fluidized bed or it is taken out of it. Cyclone is arranged over fluidized bed in fluidized-bed chamber. Powdered initial material is heated or cooled in zone of cyclone, namely near inlet opening of cyclone due to using treating gas at least partially recovered over fluidized bed in fluidized-bed chamber, possibly heated or cooled, and(or) due to using system for recovering treating gas.
EFFECT: possibility for decreasing caking on distributing collector of fluidized-bed reactor, lowered slagging in zone of fluidized bed.
10 cl, 1 dwg
FIELD: nonferrous metallurgy.
SUBSTANCE: invention relates to manufacturing zirconium powder for making pyrotechnic articles, in particular explosive and inflammable mixtures. By-layers prepared powered mixture of potassium fluorocirconate and alkali metal chloride, preferably sodium chloride, at ratio 1:(0.15-0.6) and sodium metal in amount exceeding its stoichiometrically required amount by 10-20%. Preparation involves grinding of potassium fluorocirconate and alkali metal chloride to fineness below 50 μm as well as preliminary recrystallization of potassium fluorocirconate. Charge is heated to temperature 450-600°C, at which reduction reaction starts and during this reaction reaction mixture heats to 700-800°C and reduction of potassium fluorocirconate takes place. Reaction products are cooled to 400-650°C and freed of sodium through vacuum distillation at residual pressure 1.3-13.3 Pa for 0.5-2.0 h, after which they are discharged from reaction vessel and ground. Zirconium powder is washed with water to remove fluoride and chloride salts and then dried. Zirconium powder contains 95-98% of fine fractions, including fraction below 10 μm in amount 45-55%.
EFFECT: enhanced fineness of prepared zirconium powder end assured fire safety of the process.
8 cl, 3 ex
SUBSTANCE: invention pertains to procurement of metallic device; in particular, parts for gas turbines of the flying constructions made from titanium alloys. To produce such metallic devices, the following range of procedures must be brought into action. Firstly, one or several non-metallic junction-predecessors should be made ready, each containing metallic composition element therein. These need to be chemically restored to procure a multitude of initial metallic particles, preferably those whose size varies between 0.0254 mm to approximately 13 mm, which do not have to be melted down. After having been fused at a later stage, they will solidify. The melted and solidified metal can be used either as a casting metal product or can be transferred into a partially finished product (billet) to be processed additionally until it is ultimately ready. The invention permits to substantially reduce the frequency of chemical faults in a metal product.
EFFECT: procurement of metal products by means of reconstruction of non-metal junction-predecessors and by fusion with a view to decrease the frequency of any chemical faults.
19 cl, 4 dwg
SUBSTANCE: method includes reduction of fluorine tantalite of potassium with liquid sodium in medium of melted saline bath of halogenides of alkali metals by means of alternate portioned dozing of sodium, and further - of fluorine tantalite of potassium. Fluorine tantalite of potassium is introduced into mixtures with part of the charge of halogenides of alkali metals, used for making of a saline bath. Amount of halogenides of alkali metals in the mixture introduced into melt with fluorine tantalite of potassium constitutes from 60 to 125% (wt) from weight of fluorine tantalite of potassium.
EFFECT: dimension in size of powder particles, reduction of duration of reduction process, decreasing of power consumption for melting of saline charge and forced cooling of reaction vessel.
1 tbl, 1 ex
SUBSTANCE: invention concerns rare-metal industry. Particularly it concerns receiving of metallic tantalum by metallothermic reduction of its salts. For receiving of metallic tantalum charge, containing mixture of double complex chloride salt of tantalum - KTaCl6 and potassium chloride - KCl in ratio 1:(0.2÷0.5) by mass are fed by portions or uninterruptedly in the form of powder or melt on melt mirror of metallic sodium, taken in excess 60-80% of stoichiometrically necessary amount. Reduction is implemented at temperature 550-650°C, with speed of charge feeding 15-20 g/cm2·hour of area melt mirror of metallic sodium melt. Received reduced reactionary mass is subject to vacuum- thermal processing at temperature 500-540°C and residual pressure, not exceeding equilibrium pressure of sodium steams at temperature of vacuum- thermal processing of unreacted sodium. After vacuum- thermal processing it is implemented hydro metallurgical treatment of reactionary mass.
EFFECT: exclusion of ecological pollution of environment.
4 cl, 2 tbl, 2 ex
SUBSTANCE: double complex chlorides of ittrium and potassium is reduced by lithium at temperature 450-720°C in inert atmosphere and high pressure. Received reacting mass is heated at a rate 3-5°C/min up to the temperature for 60-300°C higher the reduction temperature and then it is implemented vacuum separation at a temperature 750-780°C and evacuation 1·10-4 millimetres of mercury.
EFFECT: it is provided receiving of microcrystalline metallic powder of itrrium with minimal content of oxygen and gas-producing admixtures, described by high dispersity.
5 cl, 1 tbl, 1 dwg, 1 ex
SUBSTANCE: method includes heating of charge, containing oxygenous or oxygenous and oxygen-free composition of tantalum or niobium and halogenide of alkali metal with formation of melt. Into melt it is introduced alkali metal at blending and it is implemented reduction of tantalum or niobium at temperature 550-850°C. Additionally amount of oxygen in melt is regulated by means of changing of ratio of components of harge according to relation where n(O) - amount of oxygen, mol, k - empirically determined coefficient, k=60-350 mol, m1 and M1 - mass and molar mass of oxycompound of tantalum or niobium correspondingly in kg and kg/mol, m2 and M2 - mass and molar mass of oxygen-free composition of tantalum or niobium correspondingly in kg and kg/mol, m3 and M3 - mass and molar mass of alkali metal halogenide correspondingly in kg and kg/mol.
EFFECT: increased purity of powder, increasing of its specific surface area.
5 cl, 1 tbl, 7 ex
SUBSTANCE: invention refers to production of item out of alloy alloyed with alloying agent without melting. There is prepared a mixture of a non-metallic compound-precursor of basic metal and a non-metallic compound-precursor of an alloying element. Compounds-precursors are chemically reduced to metal alloy without melting. There is introduced one or more component-additive and metal alloy is compacted producing a packed metal item without melting. Also the component-additive is introduced during preparation of mixture or during chemical reduction, or upon chemical reduction. Additionally, an element, mixture of elements or a chemical compound are used as the component-additive. Notably, the component-additive is dissolved in a matrix or creates discrete phases in micro-structure of the alloy and is not reduced at the stage of chemical reduction.
EFFECT: facilitating production of items out of homogeneous alloy without melting its constituents causing oxidation; also composition of this alloy is impossible to produce by any other procedure.
9 cl, 3 dwg