KR101254971B1 - Method for preparing titanium powder with excellent productability and apparatus for preparing the titanium powder - Google Patents

Method for preparing titanium powder with excellent productability and apparatus for preparing the titanium powder Download PDF

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KR101254971B1
KR101254971B1 KR1020100135345A KR20100135345A KR101254971B1 KR 101254971 B1 KR101254971 B1 KR 101254971B1 KR 1020100135345 A KR1020100135345 A KR 1020100135345A KR 20100135345 A KR20100135345 A KR 20100135345A KR 101254971 B1 KR101254971 B1 KR 101254971B1
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South Korea
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titanium
reducing agent
titanium powder
reaction chamber
reaction
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KR1020100135345A
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Korean (ko)
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KR20120073546A (en
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최미선
이고기
이창규
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재단법인 포항산업과학연구원
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Abstract

The present invention relates to a method and apparatus for producing a titanium powder, and more specifically, to a titanium powder by reducing a liquid reducing agent injected into a reaction chamber and titanium tetrachloride in a gas phase to obtain a titanium powder, and to collect and transport the obtained titanium powder. It recovers the titanium powder by transporting by a stream, and additionally injects titanium tetrachloride into the transport stream to react with the unreacted reducing agent in the reduction reaction, furthermore, a liquid reducing agent A reaction chamber in which titanium tetrachloride is injected into the gas phase and the titanium tetrachloride is reduced with the reducing agent to produce titanium powder; And a transfer tube positioned below the reaction chamber, the reaction product including titanium powder by the reduction reaction being collected, and a transfer stream configured to transfer the collected reaction product. The transfer tube includes titanium tetrachloride. It provides a titanium powder manufacturing apparatus, characterized in that the gas injection pipe is formed is injected gas.

Description

TECHNICAL FOR PREPARING TITANIUM POWDER WITH EXCELLENT PRODUCTABILITY AND APPARATUS FOR PREPARING THE TITANIUM POWDER}

The present invention relates to a method for producing titanium powder and a titanium powder production apparatus suitable for the method.

More specifically, the present invention relates to a method and apparatus for improving the productivity of the titanium powder produced by the reaction of a reducing agent and titanium tetrachloride in the reaction chamber in the production of fine titanium powder and for smooth transfer of the titanium powder.

Titanium or a titanium alloy has a high melting point, high strength, high toughness, low density, and excellent corrosion resistance. Therefore, titanium or titanium alloy is widely used as a material for various components such as aircraft and chemical industry equipment.

However, the manufacture of various parts of titanium or titanium alloys by precision casting is not easy due to the high melting point (1668 ° C.) of titanium or titanium alloys, resulting in high manufacturing costs. Therefore, in order to manufacture components made of titanium at a lower cost, a powder metallurgy method is required in which titanium powder is prepared, the titanium powder is pressed to be molded into a predetermined shape, and the molded article thus obtained can be sintered.

In addition, a component made of a titanium alloy could be produced by mixing titanium powder with a metal powder to be alloyed, pressing the obtained mixed powder to form a predetermined shape, and then sintering the obtained molded product.

As described above, it is necessary to use titanium powder as the raw material for the production of various parts of titanium or titanium alloy by powder metallurgy. Such titanium powder has been manufactured by the following method using a reducing device as shown in FIG. 1.

That is, while supplying the liquid titanium tetrachloride to the reaction chamber 21 through the injection tube, the reducing agent is supplied to the reaction chamber 21 in the liquid phase from a separate reducing agent storage container 11, thereby reducing the reaction between the titanium tetrachloride and the reducing agent. To produce titanium powder and reaction byproducts. Magnesium or sodium may be used as the reducing agent, and the reducing reaction between the reducing agent and titanium tetrachloride may be expressed as in the following reaction formulas (1) and (2).

TiCl 4 (g) + 2Mg (l) = Ti (s) + 2MgCl 2 (l) (1)

TiCl 4 (g) + 4Na (l) = Ti (s) + 4NaCl (l) (2)

The titanium powder and the reaction by-products generated by the reaction are dropped to the bottom of the reaction chamber 21 by their own weight, and are moved to the transport pipe under the reaction chamber 21, and are transported along the transport pipe and collected by a separate collecting device. do.

At this time, the reducing agent is injected in excess of 30-50% of the theoretically required amount in order to increase the reduction probability of titanium tetrachloride. Therefore, the reaction product falling into the transfer pipe 31 includes, in addition to the titanium powder and the reaction byproduct, an excessive amount of the unreacted reducing agent injected.

However, the excess unreacted reducing agent is accumulated in the transfer pipe 31 apart from the transfer pipe 31 in the lower portion of the reaction chamber (21). The reducing agent accumulated on the bottom of the transfer pipe 31 prevents the flow of the transfer stream in which the titanium is moved to the titanium collecting device (not shown) by the transfer device, so that the titanium powder produced by the reduction reaction is not smoothly transferred. As a result, it lowers the yield of titanium powder and acts as a cause of lowering productivity.

The present invention seeks to smooth the flow of the transport stream by inhibiting or reducing the accumulation of excess reducing agent in the transport pipe. For this reason, it is intended to increase the yield of obtaining titanium powder and to improve productivity.

Accordingly, the present invention is to provide a method for producing titanium powder in which the unreacted reducing agent in the transfer pipe may additionally participate in the reduction reaction.

Furthermore, the present invention provides a device in which an unreacted reducing agent can additionally cause a reduction reaction in such a delivery pipe.

The present invention relates to a method for producing a titanium powder, by reducing the liquid reducing agent injected into the reaction chamber and titanium tetrachloride in the gas phase to obtain a titanium powder, by collecting the obtained titanium powder and transported by a transport stream titanium powder Recovering, and further injecting titanium tetrachloride into the transport stream provides a method for producing titanium powder, characterized in that for reacting with the unreacted reducing agent in the reduction reaction.

In the titanium powder manufacturing method of the present invention, the reducing agent is preferably magnesium or sodium, and titanium tetrachloride injected into the transport stream is preferably injected with an inert gas.

The present invention also relates to a titanium powder production apparatus, comprising: a reaction chamber in which a liquid reducing agent and titanium tetrachloride in a gas phase are injected, and the titanium tetrachloride is reduced with the reducing agent to generate titanium powder; And a transfer tube positioned below the reaction chamber, the reaction product including titanium powder by the reduction reaction being collected, and a transfer stream configured to transfer the collected reaction product. The transfer tube includes titanium tetrachloride. It provides a titanium powder manufacturing apparatus, characterized in that the gas injection pipe is formed is injected gas.

In the titanium powder production apparatus of the present invention, the reducing agent is preferably magnesium or sodium.

In addition, the transfer pipe is preferably provided with a heating element for maintaining the unreacted reducing agent remaining in the liquid phase after the reduction reaction, more preferably the heating element may be a heating coil.

Further, the gas injection pipe may be injected with an inert gas together with titanium tetrachloride gas.

According to the present invention, it is possible to suppress the flow of the transport stream by stacking the reducing agent introduced in excess for the reduction of titanium tetrachloride in the further reduction reaction by accumulating in the transport pipe under the reaction chamber. For this reason, a titanium recovery rate can be improved.

Furthermore, by additionally injecting titanium tetrachloride into the delivery pipe, an additional reduction reaction may be generated with an unreacted reducing agent, thereby further producing titanium powder, thereby improving productivity of the titanium powder.

1 is a view schematically showing a conventional titanium powder production apparatus.
2 is a view schematically showing an example of a titanium powder production apparatus according to the present invention, which has a gas injection pipe 33 for injecting additional titanium tetrachloride gas into the transfer pipe 31 below the reaction chamber 21. The titanium powder manufacturing apparatus 1 which has the heat generating body 32 in the conveyance pipe 31 is shown.

The present invention relates to a method and apparatus for producing sponge titanium, hereinafter, the present invention will be described in detail with reference to the drawings.

2 is a view showing an example of the titanium powder production apparatus 1 according to the present invention, a gas injection pipe 33 for injecting additional titanium tetrachloride gas into the transfer pipe 31 below the reaction chamber 21. It is provided, the titanium powder production apparatus 1 is provided with a heating element 32 in the transfer pipe (31).

In general, the reducing device 1 used in the production of titanium powder is injected with a reducing agent and titanium tetrachloride, and reacted with the reaction chamber 21 to reduce the titanium tetrachloride to titanium and injected into the reaction chamber 21. It is divided into a reducing agent storage container 11 for storing a reducing agent and a transfer pipe 31 for transferring titanium powder, a reaction by-product and an unreacted reducing agent generated by the reducing reaction.

The reducing agent storage container 11 is a reducing agent for the reduction of titanium tetrachloride is stored, it is injected into the reaction chamber 21, in which the reducing agent is injected into the liquid phase. Accordingly, the reducing agent storage container 11 is provided with a heating element 12 for maintaining the reducing agent in the liquid phase, thereby maintaining the temperature of the reducing agent storage container 11 above the melting temperature of the reducing agent.

In the present invention, magnesium or sodium can be used as the reducing agent. In this case, since magnesium has a melting temperature of 650 ° C. and sodium of 97.72 ° C., when magnesium is used as a reducing agent, it should be maintained above the respective temperatures.

The reducing agent storage container 11 is provided with a reducing agent injection nozzle 13 to inject a reducing agent into the reaction chamber 21, whereby the reducing agent is injected into the reaction chamber 21 to participate in the reduction reaction of titanium tetrachloride. do. Since the reducing agent storage container 11 is usually located above the reaction chamber 21, the reducing agent injection nozzle 13 is generally installed at the bottom of the reducing agent storage container 11, so that the reducing agent is reacted with the reaction chamber 21. It can be injected from the top of the.

The reducing agent in the liquid phase injected from the upper portion of the reaction chamber 21 is in contact with the titanium tetrachloride in the reaction chamber 21 to produce titanium powder by reducing titanium tetrachloride. The titanium tetrachloride is injected into the reaction chamber 21 through the injection tube 23. At this time, titanium tetrachloride is injected into the reaction chamber 21 in a gaseous state and reacted with a liquid reducing agent to reduce the titanium powder.

The titanium tetrachloride is present in the liquid phase at room temperature, the evaporation temperature is 136.4 ℃, it is usually supplied in the liquid phase. However, in the process of being supplied into the reaction chamber 21 through the injection tube 23, the gas is heated by the ambient temperature of the reaction chamber 21 to change into a gaseous phase, and titanium tetrachloride of gas is injected into the reaction chamber 21. At this time, the reducing agent is added in an excess of about 30-50% compared to the stoichiometry required for the reduction reaction for the smooth reduction of titanium tetrachloride.

The reducing agent and titanium tetrachloride injected into the reaction chamber 21 are injected to be in easy contact with each other as shown in FIG. 2. As a result, a reduction reaction in which titanium tetrachloride is reduced by a reducing agent proceeds, and the reaction formulas are as shown in the above formulas (1) and (2). In such a reaction, the reducing agent is in a liquid phase and titanium tetrachloride is carried out under a gaseous phase, and the reaction chamber 21 can maintain an atmospheric temperature under conditions in which the reducing agent maintains a liquid phase and titanium tetrachloride maintains a gaseous phase. It is desirable to have a temperature to ensure that.

Specifically, when the reducing agent is magnesium, the melting temperature of the magnesium is 650 ℃, higher than the temperature of titanium tetrachloride, so that the reaction chamber 21 at a temperature above the melting temperature of magnesium, more preferably 700 ℃ or more. It is desirable to maintain. On the other hand, when the reducing agent is sodium, since the melting temperature of sodium is 97.17 ° C., which is lower than the evaporation temperature of titanium tetrachloride, maintaining the reaction chamber 21 above the evaporation temperature of titanium tetrachloride, more preferably 150 ° C. or higher. desirable.

As described above, titanium powder, sodium chloride or magnesium chloride (hereinafter also referred to as 'chloride') is produced by the reduction reaction in the reaction chamber 21, and the reducing agent which is injected in excess and does not participate in the reduction reaction is caused by its own weight. It falls to the lower part of the reaction chamber 21 and falls to the transfer pipe 31 located in the lower part of the reaction chamber 21.

The transfer pipe 31 is transferred to the titanium powder, chloride and titanium tetrachloride falling from the reaction chamber 21 through the transfer pipe 31 by a transfer stream to be collected in a separate collecting device.

However, since the transfer pipe 31 is exposed to the atmosphere, all components falling from the reaction chamber 21 to the transfer pipe 31 are solidified, but the reducing agent is accumulated at the bottom of the transfer pipe 31. This impedes the flow of the transport stream. As a result, the transfer of titanium powder is inhibited, thereby lowering the recovery rate of the titanium powder and eventually lowering the titanium production rate.

The reason for this is that the reducing agent solidifies as it falls into the conveying pipe 31 and is transferred to the collecting device by the conveying stream. However, some of the reducing agent cannot solidify and solidifies on the bottom of the conveying pipe 31 so as to solidify. It is understood that it is accumulated at the bottom of the).

Accordingly, by additionally injecting titanium tetrachloride gas into the delivery pipe 31 and reacting with the unreacted reducing agent, it is possible to prevent the unreacted reducing agent from dropping and accumulating in the delivery pipe 31. At this time, it is preferable to inject an inert gas such as argon, helium or nitrogen together with the titanium tetrachloride gas.

The titanium tetrachloride further injected into the transfer pipe 31 is preferably injected before the transfer stream passes through the place where the reducing agent falls from the reaction chamber 21. To this end, the transfer pipe 31 may include a separate gas injection pipe 33 for injecting the titanium tetrachloride gas.

The conveying stream is a mechanism operated by a mechanical force, for example, can also be formed by the operation of the screw, and by periodically pumping the conveying pipe to form a conveying stream in the conveying pipe, titanium powder in the conveying pipe, reaction By-products and unreacted reducing agents can be transferred.

On the other hand, since the transfer pipe 31 is exposed to the atmosphere, the reducing agent falling into the transfer pipe 31 tends to solidify, and reaction with titanium tetrachloride may not be easy, so that the heating element 32 is transferred to the transfer pipe 31. ) Is preferably heated above the melting temperature of the reducing agent. By installing the heating element 32 on the outer surface of the transfer pipe 31 it is possible to maintain the temperature inside the transfer pipe 31 above the melting temperature of the reducing agent. Preferably, the heating element 32 may be a heating coil.

As such, by installing the heating element 32 in the transfer pipe 31 to melt the reducing agent, the titanium tetrachloride injected into the gas injection pipe 33 may be reduced to additionally obtain titanium powder, as well as the transfer pipe 31. ) Can solve the problem of obstructing the flow of the transport stream due to the accumulation of the reducing agent.

On the other hand, the reaction of the titanium tetrachloride and the reducing agent is accompanied by an exotherm, the temperature in the transfer tube may exceed a predetermined temperature to be controlled by the reduction reaction caused by injecting titanium tetrachloride into the transfer tube. Therefore, in order to keep the temperature around the transfer pipe constant, a cooling device such as an air cooling device such as a water cooling device or a blower provided with a coil capable of flowing cooling water can be provided.

The titanium powder thus obtained, the chloride by-product and the remaining reducing agent are transferred to a separate collecting device by a transfer stream, and the titanium powder of high purity is removed by a known method such as removing the chloride and the reducing agent with a solvent therefrom. Can be obtained.

1: reducing device 11: reducing agent storage container
12: reducing agent storage heating element 13: reducing agent injection nozzle
21: reaction chamber 22: reactor heating element
23: titanium tetrachloride injection pipe 24: titanium tetrachloride injection nozzle
31: transfer pipe 32: transfer pipe heating element
33: gas injection pipe

Claims (8)

Titanium powder is obtained by reducing the liquid reducing agent injected into the reaction chamber and titanium tetrachloride in the gas phase to obtain titanium powder. The titanium powder is collected by collecting the titanium powder and transported by a transport stream to recover titanium powder.
And adding titanium tetrachloride together with an inert gas into the transport stream to react with an unreacted reducing agent in the reduction reaction.
The method of claim 1, wherein the reducing agent is magnesium or sodium.
delete A reaction chamber in which a liquid reducing agent and gaseous titanium tetrachloride are injected and the titanium tetrachloride is reduced with the reducing agent to produce titanium powder;
A transfer tube disposed below the reaction chamber, the reaction product including titanium powder by the reduction reaction being collected, and a transfer stream configured to transfer the collected reaction product;
A heating element positioned on an outer surface of the transfer pipe and configured to maintain an unreacted reducing agent remaining in the liquid phase after the reduction reaction; And
Located on the upper stream of the transfer pipe connected to the lower portion of the reaction chamber, titanium powder manufacturing apparatus comprising a gas injection pipe is injected titanium titanium gas with an inert gas.
5. The apparatus of claim 4, wherein the reducing agent is magnesium or sodium.
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KR1020100135345A 2010-12-27 2010-12-27 Method for preparing titanium powder with excellent productability and apparatus for preparing the titanium powder KR101254971B1 (en)

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KR20130076269A (en) * 2011-12-28 2013-07-08 재단법인 포항산업과학연구원 Method for preparing sponge metal and apparatus for preparing sponge metal
CN107350485B (en) * 2017-06-19 2019-08-02 西安建筑科技大学 A kind of gas phase reaction preparation method of V-Ti-Fe hydrogen storing alloy powder
CN108356280B (en) * 2018-03-13 2021-07-16 昆明理工大学 Method for preparing spherical nano titanium powder
KR102260400B1 (en) * 2019-12-27 2021-06-03 고등기술연구원연구조합 MANUFACTURING METHOD OF Ti POWDER AND MANUFACTURING APPARATUS THEREOF

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6415334A (en) * 1987-07-09 1989-01-19 Toho Titanium Co Ltd Production of metal from metal halide
JPH02311316A (en) * 1989-05-24 1990-12-26 N K R:Kk Production of titanium powder or titanium composite powder
JPH0559413A (en) * 1991-08-30 1993-03-09 Showa Denko Kk Production of metal

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6415334A (en) * 1987-07-09 1989-01-19 Toho Titanium Co Ltd Production of metal from metal halide
JPH02311316A (en) * 1989-05-24 1990-12-26 N K R:Kk Production of titanium powder or titanium composite powder
JPH0559413A (en) * 1991-08-30 1993-03-09 Showa Denko Kk Production of metal

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