The method of producing titanium carbide

 

(57) Abstract:

The invention relates to a method for producing titanium carbide, including the recovery of a mixture of titanium tetrachloride and carbon magnesium and subsequent vacuum separation. Essence: before restoring a mixture of titanium tetrachloride and carbon or magnesium saturated with hydrogen, while magnesium is saturated up to 1 - 2% of hydrogen content. 1 C.p. f-crystals, 1 table.

The invention relates to ferrous metallurgy, in particular to the production of carbides of refractory metals, and can be used to produce titanium carbide, which is widely used in engineering, to create compositions, operating at high temperatures. Titanium carbide can be used as a covering layer of detail, providing anti-corrosion and heat-resistant properties of the products.

Known methods for producing carbides of titanium by reacting titanium dioxide with soot direct synthesis of a mixture of powders of titanium and carbon black by the interaction of Halogens with carbon components (Cypress S. S. Levinsky Y. C. Petrov A. P. titanium Carbide. M. 1987. C. 6 19). For the prototype accepted method of producing titanium carbide of titanium halides recovery. (Kip the UB> or TiI4as the carbon-containing components of different hydrocarbons, phenols and other Application TiI4in a production environment is not practiced because of its high cost. For the formation of titanium carbide process shall be carried out in the temperature range of 1200 to 1500oC.

The proposed method increases the yield of product by increasing the number of the resulting homogeneous titanium carbide.

To do this, before recovering a mixture of titanium tetrachloride and carbon or magnesium saturated with hydrogen; magnesium saturate to 1 -2% of hydrogen content.

The essence of the proposed method lies in the joint for magnesium recovery of a mixture of TiCl4and CCL4with the formation of titanium carbide and magnesium chloride. The process of interaction CCl4with magnesium proceeds relatively slowly, at the same time it is possible disproportionation CCl4with the release of sooty carbon. Eventually in the reactor pressure increases and decreases the speed of the process and the yield of the product (titanium carbide). Use as a reductant magnesium containing hydrogen, allows to intensify the process: forming hydrides and cargonaut more vigorously. Ultimately, the process proceeds with high speed, the yield of the product increases, also increases the homogeneity of the products.

Similar processes occur when using titanium tetrachloride and carbon, in which the dissolved hydrogen.

The choice of technological parameters of which are determined as follows: when the saturation of magnesium hydrogen is less than 1% of the number of the latter is insufficient to activate the formation of titanium carbide, as a consequence, the interaction of initial reagents will be provided with a low speed and the efficiency of the process will be small, at the same time will be reduced and the yield of the product. In the case of saturated magnesium hydrogen more than 2% of the speed of the process does not increase the amount of hydrogen becomes excessive. In this case, he will play the role of ballast and its application in such quantities does not seem rational from a technical and economic perspective.

Example 1. Experiments were performed at the facility, which included measuring Cup for TiCl4and CCl4airtight reactor cover (for recovery) or capacitor (for vacuum separation). Heating was carried out shaft furnace. Letters, get it warm and was carried out by feeding a mixture of TiCl4and CCl4. The total loading of the mixture was about 350 g, the carbon tetrachloride was taken with a 5% excess of stoichiometry. The process temperature of 800 850oC, the speed of feed of the mixture of tetrachloride 0,6 0,8 g/cm2H. Upon completion of the recovery process, the reaction mass was cooled and made remounting with the installation of the capacitor. Vacuum separation was carried out at 980 1000oC for 4 to 7 o'clock the Obtained product was weighed and analyzed. The results of the experiments are shown in the table.

Example 2. The process was performed according to the following technology: source of magnesium were loaded into the reactor, heated to melting and through volumetric capacity was barbotirovany hydrogen to the calculated content in magnesium 2 wt. Other parameters were the same as described above. This experience achieved: the feed rate of chloride 0.75 g/cm2/h, yield 85%

Example 3. As initial reagents used metallic magnesium and a mixture of TiCl4and CCl4rich in the process of reduction with hydrogen, as it was carried out in an atmosphere of argon and hydrogen. The obtained homogeneous product, the feed rate of chlorides was 0.7 g/cm2.h, yield 86%

1. The method of producing titanium carbide, including the recovery of a mixture of titanium tetrachloride and carbon magnesium and subsequent vacuum separation, characterized in that before restoring a mixture of titanium tetrachloride and carbon or magnesium saturated with hydrogen.

2. The method according to p. 1, characterized in that the magnesium saturate to 1 2% of hydrogen content.

 

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21 cl, 22 dwg, 1 tbl

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