JP2005213548A - Method and apparatus for manufacturing metal titanium by reducing lower chloride of titanium - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To prevent contamination by impurities such as iron from a reaction vessel and to accelerate a reduction reaction, and to provide a method for manufacturing metallic titanium by which a reaction by-product is easily removed. <P>SOLUTION: The method for manufacturing metallic titanium includes a reduction step of obtaining metal titanium by reducing titanium dichloride or titanium trichloride as raw material with metal magnesium or a magnesium alloy using a reaction vessel 2 made of titanium. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  TECHNICAL FIELD The present invention relates to a method for producing titanium metal and an apparatus for producing the same, and in particular, using titanium lower chloride as a starting material, in a small titanium reaction vessel, the metal titanium is efficiently semi-continuously by a reduction reaction. Can be manufactured.

The pioneering method for producing titanium metal is a hunter method in which titanium tetrachloride (TiCl ₄ ) is used as a raw material to perform a reduction reaction with metal sodium (Na). This reaction formula is represented by TiCl ₄ + 4Na → Ti + 4NaCl, but since the heat of reaction is large, the two-stage reduction method is advantageous.

First, in the first stage, titanium tetrachloride and molten metal sodium are continuously fed into a steel reaction vessel to produce a eutectic of titanium dichloride (TiCl ₂ ) and sodium chloride (NaCl).
Next, this eutectic is transferred to a sintering pot in a molten state, and metal sodium is added and heated to reduce titanium dichloride to metal titanium. The product is leached with dilute hydrochloric acid to remove sodium chloride which is a reaction by-product, washed with water and vacuum dried to obtain “sponge titanium”.
In addition, by controlling the temperature, the hunter method can be manufactured by one-stage reduction.

  However, this Hunter method has a problem that the process is complicated because it requires washing to remove sodium chloride which is a reaction by-product.

  Therefore, at present, the most commonly used method for producing titanium is the crawl method. This crawl method is a one-step reduction with metallic magnesium (Mg) using titanium tetrachloride as a raw material.

In this method, titanium tetrachloride is dropped into molten metal magnesium packed in a steel reaction vessel, and a metal thermal reduction reaction represented by TiCl ₄ + 2Mg → Ti + 2MgCl ₂ is performed. During the reaction, magnesium chloride (MgCl ₂ ) which is a reaction by-product is sometimes extracted. The produced titanium grows as a porous sponge-like solid (sponge titanium), and the massive sponge titanium adheres to the inner wall of the steel reaction vessel.
After completion of the reduction reaction, unreacted magnesium metal and magnesium chloride are adhered to the sponge titanium. Therefore, this steel reaction vessel is evacuated and heated to 1000 ° C. or higher to evaporate and separate metallic magnesium and magnesium chloride.
Thereafter, this steel reaction vessel is cut, and the produced sponge titanium is crushed and pulverized, and then compression molded, and this is melt cast to produce a titanium ingot.

  In this crawl method, magnesium chloride and unreacted metal magnesium can be effectively removed by vacuum evaporation, so the removal of reaction byproducts is easier than the Hunter method, and a relatively simple reactor is used. Thus, it is possible to produce metallic titanium having a low content of oxygen as an impurity.

Recently, a method of producing titanium metal by using titanium oxide as a raw material and reducing it directly as a next-generation process replacing the crawl method has attracted attention.
Among them, a raw material titanium oxide (TiO ₂ ) is electrolyzed in molten calcium chloride (CaCl ₂ ) to directly produce titanium metal, for example, a reduction process called FFC method (see, for example, Patent Document 1), calcium chloride ( A mixed molten salt of CaCl ₂ ) and calcium oxide (CaO) is electrolyzed to form a strongly reducible molten salt in which metallic calcium is dissolved in molten calcium chloride, and titanium oxide is formed inside the strongly reducible molten salt. A reduction process called OS method for reducing and deoxidizing this titanium oxide is proposed (for example, see Patent Document 2).
JP-T-2002-517613 JP 2003-129268 A

In the manufacturing method of metallic titanium by the above-mentioned crawl method, which has become mainstream, the process has been increased in size, and about 10 tons of titanium can be manufactured at a time.
However, the speeding up of the process cannot be achieved, (1) the reduction reaction with metallic magnesium requires 10 days or more, and (2) the massive sponge titanium obtained after the reduction needs to be crushed and dissolved. , It takes 2 days or more per ton of titanium to reach the melting and casting process, and (3) the formed titanium metal is deposited in a steel reaction vessel as a spongy solid, so the titanium is steel. It is difficult to continue the process because it cannot be continuously taken out from the reaction vessel made of steel, and (4) it is easy to be contaminated with impurities such as iron from the steel reaction vessel, and it is impossible with this technology to avoid iron contamination. There were problems such as being.

  The main reasons why the reduction reaction cannot be accelerated are that although this reduction reaction is a very large exothermic reaction, it is difficult to remove heat from the steel reaction vessel, and the titanium tetrachloride raw material with high vapor pressure. This is because a large amount of the reducing agent cannot be reacted at once.

  In the future, the demand for titanium is expected to increase. However, as long as the current crawl method is used, in order to increase the production amount, in order to compensate for the slowness of the reduction reaction and the separation process of reaction byproducts, 5 An inefficient method of preparing a large number of steel reaction vessels with a scale of 10 tons and processing them in parallel is unavoidable.

In addition, the production methods according to Patent Document 1 and Patent Document 2 are mainly reduction methods using titanium oxide as a raw material, and the main feature is to use a molten salt such as calcium chloride (CaCl ₂ ) as a reaction medium. .
In this manufacturing method, since the molten salt electrolysis is basically used, the disadvantage of using a large amount of molten salt and the electrochemical reaction at the electrode interface, the space utilization efficiency is low. There was a problem that it was difficult to speed up the reduction process and improve energy efficiency.
Furthermore, the production methods according to Patent Document 1 and Patent Document 2 have a problem in that washing is necessary in the same manner as the Hunter method in order to remove calcium oxide as a reaction byproduct.

  In view of the above-mentioned problems of the conventional technology, the present invention provides a method for producing titanium metal that speeds up the reduction reaction, prevents contamination of impurities such as iron from the reaction vessel, and facilitates removal of reaction by-products. For the purpose.

To solve this problem,
The invention according to claim 1 has a reduction step of obtaining titanium metal by reducing titanium dichloride or titanium trichloride as a raw material with metal magnesium or a magnesium alloy using a titanium reaction vessel. This is a method for producing metallic titanium.

  The invention according to claim 2 is characterized in that after the reduction step, the titanium metal is fed together with the titanium reaction vessel to the melting and casting step without passing through a crushing and pulverizing step. It is a manufacturing method of the metal titanium of description.

  In the invention according to claim 3, the charged amount of the raw material titanium dichloride or titanium trichloride and the reducing agent metal magnesium or magnesium alloy is 0.05 to 120 kg, and the reaction time of the reduction reaction is 1 to 500. It is a minute, It is a manufacturing method of the titanium metal of Claim 1 or 2.

  The invention according to claim 4 is characterized in that the titanium sponge obtained in the reduction step has a maximum length of 400 mm or less, and the metal titanium according to any one of claims 1 to 3 It is a manufacturing method.

  The invention according to claim 5 is characterized in that the reduction step and the separation step of the reaction by-product are performed in one process, and the method for producing titanium metal according to any one of claims 1 to 4 It is.

  The invention according to claim 6 is the method for producing titanium metal according to any one of claims 1 to 5, wherein titanium or magnesium chloride is added to the reduction step.

  The invention according to claim 7 is characterized in that the magnesium alloy is a magnesium alloy containing at least one metal selected from the group consisting of silver, nickel, copper and tin. The method for producing titanium metal according to any one of the above.

  The invention according to claim 8 is an apparatus for producing titanium metal, wherein the reaction vessel is made of titanium.

  The invention according to claim 9 is the apparatus for producing titanium metal according to claim 8, wherein the reaction vessel comprises an upper kettle and a lower kettle, and the upper kettle is a titanium vessel.

  The invention according to claim 10 is the apparatus for producing metal titanium according to claim 8 or 9, characterized in that the apparatus has a reaction vessel having a charged amount of 0.05 to 120 kg.

  The invention according to claim 11 has a reaction vessel in which the dimension of the obtained titanium sponge is 400 mm or less at the maximum length, and the metal titanium according to any one of claims 8 to 10 It is a manufacturing device.

According to the method for producing titanium metal of the present invention, by using a lower chloride of titanium such as titanium dichloride (TiCl ₂ ) or titanium trichloride (TiCl ₃ ) as a raw material, the vapor pressure is extremely low at room temperature. Compared with the case of reducing titanium tetrachloride (TiCl ₄ ), which is very high, the amount of heat generated by the reaction is low, and the heat removal from the reaction vessel can be facilitated.

  In addition, these lower chlorides are solid at room temperature and have a low vapor pressure, so that high-density loading into the reaction vessel is facilitated.

  Furthermore, according to the method for producing titanium metal of the present invention, the raw material and the reducing agent can be reacted in large quantities at a time by using a solid lower titanium chloride as the raw material. Speed can be increased.

  In addition, according to the method for producing titanium metal of the present invention, since the amount of raw materials charged is small and the reaction time is short, the amount of heat generated by the reaction is reduced, the reaction by-products can be easily removed, and the process is continued. -Speed can be increased.

  Furthermore, according to the method for producing titanium metal of the present invention, since the titanium sponge obtained is small, a small titanium reaction vessel can be used, and therefore the reduction process can be speeded up.

  Also, by preparing a large number of small reaction vessels made of titanium and processing them in parallel or sequentially, the process can be made semi-continuous.

  According to the method for producing titanium metal of the present invention, the reduction step and the reaction by-product separation step are performed in one process, so that the process can be continuous and speeded up.

  According to the method for producing titanium metal of the present invention, since magnesium is used as the reducing agent, washing with water or the like is unnecessary, and magnesium chloride as a reaction byproduct is easily removed by vacuum heating or the like. it can.

  Furthermore, in the production method of the present invention, only titanium or magnesium chloride is added to the reaction vessel as an additive other than the raw material and the reducing agent, so that the reaction by-product can be easily separated.

  Moreover, according to the manufacturing method of the titanium metal of this invention, since a crushing / crushing process is unnecessary, a process can be continued and it can be sped up.

  And according to the manufacturing method and metallic titanium manufacturing apparatus of this invention, since titanium reaction containers are used, impurity contamination, such as iron from a reaction container, can be prevented.

  Furthermore, in the present invention, by using a small titanium reaction vessel, heat removal from the vessel is facilitated, and the time required for the reduction reaction can be shortened.

  And, in the present invention, by using a small titanium reaction vessel, without passing through the crushing and pulverization step in the crawl method, the generated sponge titanium is fed together with the titanium reaction vessel to the melt casting step, Metallic titanium can be produced semi-continuously.

The present invention aims to break away from the current crawl method, and instead of titanium tetrachloride raw material, titanium low chloride raw material (subhalide, solid at room temperature) such as titanium dichloride or titanium trichloride is used in a small titanium reaction vessel. Among them, a high-purity and small-sized titanium lump that can be reduced using metallic magnesium and dissolved as it is is semi-continuously efficiently produced.
No attempt has been made to produce titanium efficiently by high-speed and continuous treatment by reducing lower chloride of titanium as in the present invention with magnesium in a small titanium reaction vessel.

  Hereinafter, an example of an apparatus for producing metallic titanium according to an embodiment of the present invention will be described in detail with reference to the drawings.

[First Embodiment]
FIG. 1 is a cross-sectional view of a titanium metal manufacturing apparatus 1 according to the first embodiment. The titanium metal manufacturing apparatus 1 includes a reaction vessel 2, a lid 3, a partition wall 6, and a heating device 7.

The reaction vessel 2 is a cylindrical or box-like vessel having a thickness of 0.1 to 10 mm, preferably 1 to 2 mm. The size of the container 2 is such that 0.05 to 120 kg of the mixture 8 of the raw material and the reducing agent can be accommodated therein. This is because if the size of the container 2 is too large, heat removal from the container 2 is not easy, and if the size of the container 2 is too small, the amount of sponge titanium produced is reduced, which is uneconomical.
Further, a hole 5 having a diameter of 5 to 20 mm is provided at the bottom of the container 2.
Further, a lid 3 is provided at the head of the container 2, and the lid 3 can be removed from the container 2. Further, the lid portion 3 is provided with a hole 4 having a diameter of 5 to 20 mm.

  The container 2 and the lid 3 are accommodated in a heating device 7 partitioned by a partition wall 6. The heating device 7 is preferably a high-frequency induction heating device, but a highly versatile heating device such as a resistance heating furnace can also be used. The interior of the partition wall 6 is filled with an inert gas such as argon gas or helium from the viewpoint of preventing oxidation during the reduction reaction. A heating device 7 is provided outside the partition wall 6 so that the container 2 can be heated to a desired temperature in an inert gas atmosphere.

The reaction vessel 2 is made of titanium metal having a purity of 98 to 99.99%, preferably 99 to 99.8%. In the conventional crawl method, titanium tetrachloride is used as a raw material, and therefore a titanium reaction vessel cannot be used. This is because the reaction of Ti + TiCl ₄ → TiCl ₂ proceeds and the titanium container is melted. On the other hand, in the present invention, when titanium dichloride is used as a raw material, a titanium reaction vessel can be used because it is thermodynamically balanced with titanium metal.
Metal titanium may also be used for the lid 3, but any material may be used when the lid 3 is not fed to the melting and casting process described later. Among them, it is preferable to use a material such as steel.

Inside the container 2, a mixture 8 of the raw material and the reducing agent is accommodated. The amount of the mixture 8 charged into the container 2 is, as described above, 0.05 to 120 kg, preferably 0.1 to 50 kg, more preferably 1 to 30 kg. Since the container 2 can be downsized by setting the amount of the mixture 8 to be 0.05 to 120 kg, the calorific value is reduced, and the reaction by-products such as magnesium chloride are also small, so this can be easily removed. The process can be continued and speeded up.
In consideration of the point of removing the lid 3, the mixture 8 is accommodated in the container 2 with a gap between the lid 3 so that the generated titanium sponge does not grow up to the lid 3. Is preferred.

  The sponge titanium obtained from the container 2 has a maximum length of 400 mm or less, preferably 200 mm or less. This size of sponge titanium has a weight of 40 kg or less, preferably 20 kg or less. This is because, when the dimension of the sponge titanium obtained is 400 mm or less at the maximum length, the heat removal from the container 2 and the separation of the reaction by-products are accelerated, and the speeding up of the process can be achieved. .

  In the titanium metal manufacturing apparatus 1 according to the present embodiment, since the titanium reaction vessel 2 is used, contamination from impurities such as iron from the reaction vessel 2 can be prevented.

  FIG. 2 is a flowchart showing basic manufacturing steps in the method for manufacturing titanium metal according to the present invention. As shown in FIG. 2, the method for producing titanium metal includes a reduction step S1.

In the reducing step S1, lower titanium chloride and reducing agent as raw materials are accommodated in the titanium reaction vessel 2 according to the present embodiment, and 700 to 1000 ° C. in an inert gas atmosphere in the heating device 7, preferably Is heated to 800 to 950 ° C. for 1 to 500 minutes, preferably 10 to 60 minutes, to produce sponge titanium. The reason why the heating temperature is set to 700 to 1000 ° C. is that the reduction reaction does not proceed when the heating temperature is lower than 700 ° C., and the evaporation amount of the reducing agent increases when the heating temperature exceeds 1000 ° C.
In addition, since the reduction reaction is performed in an inert gas atmosphere, the generated sponge titanium can be prevented from being oxidized and the oxygen content as an impurity can be reduced.

  The lower chloride of titanium used as a raw material is solid titanium dichloride or titanium trichloride. Titanium dichloride can be produced using a conventional method in which liquid titanium tetrachloride is reduced with metallic magnesium, metallic sodium, metallic titanium, or the like. Titanium trichloride can be obtained by reducing titanium tetrachloride with metallic magnesium, metallic aluminum, metallic sodium, metallic titanium, or the like. When producing these lower chlorides of titanium, it is necessary to reduce the amount of the reducing agent used in the Hunter method and the Kroll method so that the reduction reaction does not proceed excessively to produce a large amount of metallic titanium. is there.

Titanium tetrachloride is liquid at room temperature and has a very high vapor pressure, whereas titanium dichloride or titanium trichloride is solid and has a low vapor pressure. The heat generated by the reduction reaction is 434 kJ per mole of titanium for titanium tetrachloride, and 93.5 kJ and 191 kJ for titanium dichloride or titanium trichloride, respectively.
Therefore, if titanium dichloride or titanium trichloride is used as a raw material in place of titanium tetrachloride, the amount of heat generated by the reaction is small, so heat removal from the reaction vessel 2 is facilitated, and a large amount of raw material and reducing agent are added at a time. Can be reacted. Furthermore, since titanium dichloride or titanium trichloride is solid and has a low vapor pressure, the reaction vessel 2 can be filled with the raw material at a high density.

In this embodiment, metallic magnesium is used as the reducing agent. As the reduction reaction proceeds, titanium sponge and reaction by-products are generated in the container 2. The sponge titanium is fused to the inner wall of the container 2 and grows in a lump shape. Further, most of the reaction by-product is magnesium chloride and contains an unreacted reducing agent (metallic magnesium) added in excess. Since magnesium chloride is a liquid, it can be discharged from the hole 5 at the bottom of the container 2 and separated.
By discharging and separating the reaction by-products from the bottom hole 5, the reduction step and the reaction by-product separation step can be performed in one process, so that the process can be continued and speeded up. it can.

  After completion of the reduction reaction, the container 2 is evacuated to 10 to 1000 Pa, heated to 900 to 1200 ° C., the magnesium chloride remaining in the sponge titanium and unreacted metal magnesium are evaporated, and the hole in the lid 3 Volatilize from 4 and separate. Since the vapor pressures of metallic magnesium and magnesium chloride at 1000 ° C. are as high as 55000 Pa and 2700 Pa, respectively, they can be easily vaporized and removed by vacuum heating without using a washing step with water or the like like the Hunter method.

  As described above, the sponge titanium obtained by this reduction reaction has a maximum dimension as small as 400 mm or less, and thus a small titanium reaction vessel as in this embodiment can be used. By preparing a large number of such small titanium reaction vessels and processing them in parallel or sequentially, titanium titanium can be produced semi-continuously in a short time.

Although the manufacturing method of this metal titanium was set as the structure which consists of reduction process S1, you may provide melt | dissolution and casting process S2. In the crawl method, after this reduction step, a step of crushing and pulverizing the generated sponge titanium was necessary.
On the other hand, in the present invention, by using the titanium reaction vessel 2 as described above, the titanium sponge produced together with the titanium reaction vessel 2 is subjected to the melt casting step S2 without going through this crushing and pulverization step. In addition to preventing contamination occurring in the crushing process, energy can be saved, the process can be continued and speeded up, and the time can be shortened.
In the melting / casting step S2, titanium sponge is heated and melted together with the titanium reaction vessel 2 in a melting furnace to produce a titanium ingot.

[Second Embodiment]
FIG. 3 is a cross-sectional view of the titanium metal manufacturing apparatus 1 according to the second embodiment. The titanium metal manufacturing apparatus 1 includes a reaction vessel 2, a lid 3, a partition wall 6, and a heating device 17. Below, a different part from 1st Embodiment is demonstrated and description of the part similar to 1st Embodiment is abbreviate | omitted.

  The reaction vessel 2 is composed of a cylindrical or box-shaped upper kettle 20 and a lower kettle 21. The upper hook 20 is made of metal titanium similar to that of the first embodiment. Further, the lower pot 21 may be any material because it is not fed to the melting and casting process, but among these, it is preferable to use a material such as steel. A lid 3 similar to that of the first embodiment is provided on the head of the container 2. And this container 2 and the cover part 3 are accommodated in the inside of the heating apparatus 17 partitioned off by the partition 6 similarly to 1st Embodiment.

  In the present embodiment, the bottom portion of the lower hook 21 and the lid portion 3 are not provided with holes, but holes may be provided as in the first embodiment. Further, the mixture 8 of the raw material and the reducing agent is accommodated in the upper pot 20.

In this embodiment, metallic magnesium or a magnesium alloy is used as the reducing agent. This magnesium alloy is preferably a magnesium alloy containing at least one metal selected from the group consisting of silver, nickel, copper and tin. As the reducing agent to be housed together with the raw material in the upper pot 20, metallic magnesium is preferable.
Further, a small amount of the reducing agent 9 made of a magnesium alloy or an alloy element may be added to the bottom of the lower pot 21 in advance. If a reducing agent 9 made of a magnesium alloy or an alloy element is put in the lower pot 21 in advance, after the reduction reaction, an excessive amount of reducing agent inside the upper pot 20 is reduced to a reducing agent 9 made of a magnesium alloy in the lower pot 21 or an alloy. It reacts with the element to become a magnesium alloy, which selectively collects in the lower pot 21 and can reduce the reducing agent remaining in the sponge titanium. As such an alloy element, an element containing one or more metals such as silver, nickel, copper, and tin is preferable.

  In the present embodiment, a reaction aid and a sealing agent can be added in addition to the lower chloride of titanium and the reducing agent. When titanium trichloride is used as a raw material, the upper kettle 20 is corroded by reacting with the upper kettle 20 to produce titanium dichloride. In order to prevent this phenomenon, it is preferable to add powdered titanium as a reaction aid together with the reducing agent.

  Moreover, you may add the sealing agent 10 to the upper part of the mixture 8 accommodated in the upper pot 20. As shown in FIG. By adding the sealing agent 10, excessive evaporation of magnesium chloride as a reaction by-product can be prevented. As such a sealing agent 10, metallic magnesium and magnesium chloride are preferable. This sealant 10 can also be used as a reaction aid.

  In the present invention, only powdered titanium or magnesium chloride, which is a sealing agent, is added to the reaction vessel as an additive other than the raw material and the reducing agent. Therefore, even when the additive is added, the reaction by-products become excess metal magnesium and magnesium chloride, so that they can be easily vaporized and removed by vacuum heating, and separation of these can be easily performed. it can.

The method for producing metal titanium is the same as that in the first embodiment. The reaction vessel 2 and the lid 3 are heated in an inert gas atmosphere in the heating device 17 to produce sponge titanium.
In this embodiment, sponge titanium grows in the upper kettle 20 by the reduction reaction, and liquid magnesium chloride as a reaction by-product accumulates at the bottom of the lower kettle 21. At that time, a hole may be provided in the bottom of the lower pot 21 and the magnesium chloride may be gradually extracted.

After the reduction reaction is completed, the upper kettle 20 is heated to 1000 to 1100 ° C., the lower kettle 21 is cooled to 300 to 800 ° C., and metal magnesium and magnesium chloride remaining in the sponge titanium are volatilized and collected in the lower kettle 21 having a low temperature. Remove.
Next, the upper pot 20 is fed to the melting and casting step S <b> 2 while the generated sponge titanium is put in the upper pot 20.
The lower pot 21 from which magnesium chloride has been removed is used again in the reduction step S1. Also. Magnesium chloride is electrolyzed back to metallic magnesium and reused.

  Table 1 summarizes the differences in characteristics between the titanium production method of the present invention and the conventional crawl method.

  Hereinafter, the present invention will be described in more detail by way of examples. The present invention is not limited to the following examples.

[Example 1]
A cylindrical titanium reaction vessel having a diameter of 20 mm and a length of 40 mm shown in FIG. 1 is filled with 6 g of powdered titanium trichloride and 4 g of metal magnesium, and the vessel is placed in a high-frequency heating apparatus in an argon gas atmosphere. Heated at 800 ° C. for 60 minutes.
During the reduction reaction, about 80% or more of magnesium chloride as a reaction by-product was taken out from the hole at the bottom of the reaction vessel. However, some magnesium chloride and an excess amount of metallic magnesium remained in the reaction vessel, so after completion of the reduction reaction, the reaction vessel was heated to 1000 ° C. with a heating device and the inside of the reaction vessel was ^{maintained at} about 10 ⁻³ atm for 20 minutes. A vacuum was applied and then cooled to room temperature. Sponge-like titanium metal was obtained in the reaction vessel.

  The content of metal impurities in the obtained sponge titanium was measured using a fluorescent X-ray analyzer (manufactured by JEOL, JSX-3210). Moreover, the iron content in the sponge titanium was measured using a high frequency inductively coupled plasma optical emission spectrometry (ICP) apparatus (manufactured by SEIKO). Furthermore, the oxygen content in the titanium sponge was measured with an inert gas melting infrared absorption analyzer (manufactured by LECO, TC-436).

  X-ray fluorescence analysis did not detect metal impurities in the sponge titanium. In the ICP analysis, the iron content in the sponge titanium was 500 ppm. In the inert gas melting infrared absorption analysis, the oxygen content in the titanium sponge was 1000 ppm.

[Example 2]
3 g of powdered titanium dichloride and 5 g of magnesium metal are filled in a cylindrical titanium reaction vessel having a diameter of 30 mm and a length of 40 mm corresponding to the upper kettle shown in FIG. 3, and sealed with a stainless steel vessel hitting the lower kettle. These containers were heated in a resistance heating type electric furnace at 800 ° C. for 20 minutes in an argon gas atmosphere.
At the start of heating, the vapor pressure of the reducing agent was increased by heating from the lower kettle. During the reduction reaction, magnesium chloride as a reaction by-product was taken out from the hole at the bottom of the lower kettle. And after completion | finish of a reductive reaction, it cooled from the lower kettle, maintaining the upper kettle at 1000 degreeC for 20 minutes, and magnesium chloride remaining in sponge titanium and excess metal magnesium were separated and removed to the lower kettle.
The content of metal impurities and oxygen in the obtained sponge titanium was analyzed by the same method as in Example 1.

  X-ray fluorescence analysis did not detect metal impurities in the sponge titanium. In the ICP analysis, the iron content in the sponge titanium was 500 ppm. In the inert gas melting infrared absorption analysis, the oxygen content in the titanium sponge was 1000 ppm.

  From the above results, according to the metal titanium production method and metal titanium production apparatus of the present invention, it is possible to prevent contamination of impurities such as iron from the reaction vessel, the time required for the process is short, and the crushing step is unnecessary. Therefore, it was confirmed that the titanium manufacturing process can be speeded up and streamlined.

It is sectional drawing of the manufacturing apparatus of the metal titanium which concerns on 1st Embodiment. It is a flowchart which shows the basic manufacturing process in the manufacturing method of the metal titanium which concerns on this invention. It is sectional drawing of the manufacturing apparatus of the metal titanium which concerns on 2nd Embodiment.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Metal titanium manufacturing apparatus 2 Reaction container 20 Upper pot 21 Lower pot S1 Reduction process S2 Melting and casting process

Claims (11)

Using titanium dichloride or titanium trichloride as a raw material, using a titanium reaction vessel,
A method for producing metal titanium, comprising a reduction step of obtaining metal titanium by reduction with metal magnesium or a magnesium alloy. Without going through the crushing and grinding process after the reduction process,
2. The method for producing titanium metal according to claim 1, wherein the titanium metal is fed together with the titanium reaction vessel in the melt casting step. Preparation amount of titanium dichloride or titanium trichloride as a raw material and metallic magnesium or magnesium alloy as a reducing agent is 0.05 to 120 kg,
The method for producing titanium metal according to claim 1 or 2, wherein the reaction time of the reduction reaction is 1 to 500 minutes.   4. The method for producing titanium metal according to claim 1, wherein the dimension of the titanium sponge obtained in the reduction step is 400 mm or less at the maximum length. 5.   The method for producing metallic titanium according to any one of claims 1 to 4, wherein the reduction step and the reaction by-product separation step are performed in one process.   Titanium or magnesium chloride is added to the said reduction | restoration process, The manufacturing method of the titanium metal of any one of Claims 1-5 characterized by the above-mentioned.   7. The magnesium alloy according to claim 1, wherein the magnesium alloy is a magnesium alloy containing at least one metal selected from the group consisting of silver, nickel, copper, and tin. A method for producing metallic titanium.   An apparatus for producing titanium metal, wherein the reaction vessel is made of titanium.   9. The apparatus for producing titanium metal according to claim 8, wherein the reaction vessel is composed of an upper kettle and a lower kettle, and the upper kettle is a titanium vessel.   The apparatus for producing metallic titanium according to claim 8 or 9, comprising a reaction vessel having a charging amount of 0.05 to 120 kg. The apparatus for producing metallic titanium according to any one of claims 8 to 10, wherein the titanium titanium obtained has a reaction vessel having a maximum length of 400 mm or less.

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