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 mm

2. 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

 

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1 tbl, 1 ex

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