KR20010018327A - Appratus and method of titanium production by contineous process - Google Patents

Abstract

PURPOSE: A manufacturing device of titanium by a continuous process is provided which is able to perform the continuous process for preparing titanium by installing a device, which continuously supplies and collects raw materials, a reductant and reaction salts. CONSTITUTION: The device comprises: (i) a heating element(1); (ii) a gas inlet(2); (iii) a stirrer(3); (iv) a vacuum pump(4); (v) a gas outlet(5); (vi) a reaction container(6); (vii) a vacuum container(7); (viii) an outside conductor(8); (ix) a reductant and reaction salt injecting pipe; (x) a raw materials injecting hole(10); (xi) a secondary cooler(11); (xii) a primary cooler(12); (xiii) a reductant and reaction salt injecting container(13); (xiv) a raw materials injecting container(14); (xv) a reductant and reaction salt injecting and collecting hole(15); (xvi) a raw materials injecting and collecting hole(16); and (xvii) a vacuum valve(17).

Description

Apparatus and method of titanium production by contineous process

The present invention relates to a titanium manufacturing apparatus and method by a continuous process, and more particularly, it is possible to control the position, form and shape of the precipitated titanium by participating in the reduction reaction of the electrons generated during the reaction in the production of titanium, raw material The present invention relates to a titanium production apparatus and method by a continuous process that enables continuous production of titanium by providing a device capable of continuously supplying and recovering a reducing agent and a reaction salt.

In general, titanium is a metal material that is widely used in aircraft materials, chemical industry requiring medical corrosion, and medical and biological materials because of its high specific strength and excellent chemical corrosion resistance.

At present, titanium is manufactured by the Kroll method, which is a kind of metal thermal reduction method as illustrated in FIG. 1, and an approximate manufacturing process thereof includes titanium tetrachloride (Ti ₂ Cl ₄ ) as a raw material in the reaction vessel (6). ) And magnesium (Mg) as a reducing agent and magnesium chloride (MgCl ₂ ), potassium chloride (KCl) and lithium chloride (LiCl) as reaction salts were mixed and charged, followed by a reduction process for several hours at a temperature of 700 to 1000 ° C. Thereafter, the temperature is cooled to room temperature to prepare titanium, which is fixed in the reaction vessel, by dissolving and recovering the titanium from the reaction salt or the reducing agent.

However, such a titanium manufacturing process is a one-time intermittent process in which titanium is precipitated by a reduction reaction by direct physical contact of charge materials by simultaneously charging and mixing raw materials, a reducing agent, and a reaction salt in the reaction vessel (6). The reactor and the reactants must be exchanged every time the furnace is charged.In addition to the temperature rise and cooling required for the reaction, it takes a long time to cool down. 6) There are many problems in that productivity and efficiency are low and production cost is high, because it is not easy to recover precipitates because it sticks to the wall.

The present invention, in order to solve the above problems, the reaction can be carried out by the movement of electrons rather than the reduction production process of titanium by direct physical contact of the charges in the reaction vessel (6) as in the conventional titanium production method. By connecting a good conductor 8 between the reaction vessel 6 and the raw material charging vessel 14 so as to enable control of the position, form and shape of the precipitated titanium, and also the necessary raw materials for the reaction period without stopping the operation. It is an object of the present invention to continuously produce titanium by installing a device capable of continuously supplying and recovering reducing agents and salts.

In order to achieve the above object, the present invention, in the production of metal titanium, by connecting the conductor (8) having good movement of electrons between the reaction vessel (6) and the raw material charging container (14) the movement of the electrons formed during the reaction It is possible to control the position, form and shape of precipitated tantalum by providing a path, and also by installing a device that can continuously supply and recover necessary raw materials, reducing agents and salts during the reaction period, without interrupting operation It relates to an apparatus and method for producing titanium by a continuous process, characterized in that the continuous process and production of.

1 is a conventional titanium manufacturing apparatus

Figure 2 is a titanium continuous manufacturing apparatus used in the present invention

<Explanation of symbols for main parts of drawing>

1: heating element 2: gas inlet

3: stirrer 4: vacuum pump

5: gas outlet 6: reaction vessel

7: vacuum container 8: outer conductor

9: reducing agent and reaction salt loading rod 10: raw material inlet

11: 2nd cooling device 12: 1st cooling device

13: reductant and reactive salt charging container 14: raw material charging container

15 charging and recovery port of reducing agent and reaction salt 16 charging and recovery of raw material

17: vacuum valve

Hereinafter, described in detail by the accompanying drawings as follows.

Figure 2 is a schematic diagram of the titanium continuous manufacturing apparatus used in the present invention is largely composed of the reactor and the raw material, the reducing agent and the reaction salt and the device designed to enable continuous supply and recovery during the reaction period and peripheral devices.

Meanwhile, the titanium production process according to the present invention will be described in detail. First, the mixture is charged with magnesium chloride, potassium chloride, lithium chloride, and the like as a reducing agent in a reaction vessel 6 at room temperature, and then vacuum pump 4 After maintaining a vacuum of about 10 ^-3 torr (torr), and after raising the temperature to 200 ~ 300 ℃, by blowing the argon gas (2) to form the inside of the reaction vessel (6) in an argon atmosphere When the reaction temperature is increased to 700 to 1000 ° C. to completely dissolve the reducing agent and the reaction salt in the reaction vessel 6, the magnesium reducing agent present in the reaction vessel 6 is ionized as shown in the equation 1 to generate electrons. .

^{2Mg → 2Mg 2+ + 4e - ---------} ①

At this time, the raw material loading container 14 is suspended in the reaction container 6 in the raw material charging inlet 10 made of a conductor which can easily move electrons, and titanium tetrachloride, which is a raw material, is injected through the raw material charging inlet 10. Then, the electrons generated by the equation 1 through the conductor 8 which is an external circuit connected between the reaction vessel 6 and the raw material charging container 14 from the reaction container 6 through the raw material charging container 14 And react with the titanium ions produced by ② in the raw material charging container 14 to reduce it to titanium as shown in Equation ③. Therefore, the overall reaction in the reaction container 6 is expressed as Can be expressed.

_{^{TiCl 4 → Ti 4+ + 4Cl -}} --------- ②

^{Ti 4+ + 4e - → Ti ---------} ③

TiCl ₄ + 2Mg → Ti + 2MgCl ₂ --------- ④

On the other hand, after the predetermined process is completed, the recovery of titanium deposited in the raw material loading container 14 is performed after the raw material charging container 14 is sufficiently cooled in the primary cooling zone 12,

It is taken out through the raw material charging inlet 16 and is sufficiently cooled in the secondary cooling zone 11 to room temperature and then recovered.

As described above, when applying the manufacturing apparatus and process used in the present invention, it is possible to continuously manufacture titanium, and to stop the operation in the same manner as supplying and recovering the raw materials, reducing agents and reaction salts necessary during the operation period as described above. In addition to being able to continuously supply and recover, and for higher productivity, various operations are possible by installing the number, size, and shape of the supply and recovery devices of the above materials on a scale desired by an operator.

As described above, the present invention, unlike the conventional titanium production method by direct physical contact of the reactants, because of the reduction reaction by the movement of electrons, the choice of raw materials is wide, the use of low-grade raw materials and high-purity precipitates In addition to being able to obtain, there is an advantage that can control the position, form and shape of the precipitate, in particular the continuous operation is possible, there are a number of advantages, such as high productivity, low cost, high efficiency compared to the intermittent manufacturing method.

Claims (1)

In manufacturing metal titanium, It is possible to control the position, form and shape of the precipitated titanium by providing a moving path of electrons formed during the reaction by connecting a good conductor of electrons between the reaction vessel and the raw material charging container. Apparatus for producing titanium by the continuous process, characterized in that the continuous process and manufacturing of titanium without interrupting the operation by providing a device for continuously supplying and recovering the necessary raw materials, reducing agents and reaction salts during the reaction period and Way.