KR101625823B1 - Titanium tetrachloride refine apparatus - Google Patents

Titanium tetrachloride refine apparatus Download PDF

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Publication number
KR101625823B1
KR101625823B1 KR1020150090332A KR20150090332A KR101625823B1 KR 101625823 B1 KR101625823 B1 KR 101625823B1 KR 1020150090332 A KR1020150090332 A KR 1020150090332A KR 20150090332 A KR20150090332 A KR 20150090332A KR 101625823 B1 KR101625823 B1 KR 101625823B1
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South Korea
Prior art keywords
titanium tetrachloride
tank
separation column
tank member
reactor
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KR1020150090332A
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Korean (ko)
Inventor
이경주
김영국
정종화
서재용
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오션브릿지 주식회사
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/02—Halides of titanium
    • C01G23/022—Titanium tetrachloride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D8/00—Cold traps; Cold baffles

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A titanium tetrachloride purification apparatus is disclosed.
A titanium tetrachloride purifying apparatus is provided with a raw material receiving tank member containing titanium tetrachloride (TiCl 4 ) to be purified; A refill reactor member capable of heating titanium tetrachloride supplied from the raw material receiving tank member; A separation column member capable of separating foreign substances in titanium tetrachloride heated in the refining reactor member; A condensing member for condensing the titanium tetrachloride from which the foreign substance is separated from the separation column member; A refining tank member for containing titanium tetrachloride condensed in the condensing member; And the separation tank member, the purification reactor member, the separation tank member, the separation tank member, the separation tank member, the separation tank member, the separator column member, the condensation member, and the purification tank member, And a vacuum forming member for depressurizing the column member, the condensing member, and the tablet tank member.
According to the disclosed titanium tetrachloride purification apparatus, the titanium tetrachloride purification apparatus includes a raw material tank member, a purification reactor member, a separation column member, a condensation member, a purification tank member, and a vacuum forming member, Each component of the apparatus can be in a depressurized state and the depressurized state can be refined with respect to titanium tetrachloride so that the boiling point of titanium tetrachloride and the like can be lowered thereby reducing energy consumption But also titanium tetrachloride can be purified.

Description

Titanium tetrachloride refine apparatus "

The present invention relates to a titanium tetrachloride purification apparatus.

Titanium tetrachloride (TiCl 4 ) is an electrode material of a capacitor for storing electrons in the fabrication of a semiconductor memory device. It is used as a diffusion barrier layer by being deposited with titanium nitride (TiN). For this use, It is the substance that is required to be purified.

There are registered patents listed below which can be presented as conventional examples for purifying titanium tetrachloride.

However, according to the conventional method of purifying titanium tetrachloride, excessive energy is consumed for purifying titanium tetrachloride, and there is a demand for a device capable of reducing such energy consumption.

Patent Document No. 1994-0000013, Date of Publication: January 05, 1994 Title of Invention: Method of removing contaminants from liquid TiCl 4 phase

It is an object of the present invention to provide a titanium tetrachloride purification apparatus capable of purifying titanium tetrachloride while reducing energy consumption.

According to an aspect of the present invention, there is provided an apparatus for purifying titanium tetrachloride, comprising: a raw material receiving tank member containing titanium tetrachloride (TiCl 4 ) to be purified; A refill reactor member capable of heating titanium tetrachloride supplied from the raw material receiving tank member; A separation column member capable of separating foreign substances in titanium tetrachloride heated in the refining reactor member; A condensing member for condensing the titanium tetrachloride from which the foreign substance is separated from the separation column member; A refining tank member for containing titanium tetrachloride condensed in the condensing member; And the separation tank member, the purification reactor member, the separation tank member, the separation tank member, the separation tank member, the separation tank member, the separator column member, the condensation member, and the purification tank member, And a vacuum forming member for depressurizing the column member, the condensing member, and the tablet tank member.

According to one aspect of the present invention, there is provided a titanium tetrachloride purification apparatus comprising a raw material tank member, a purification reactor member, a separation column member, a condensation member, a purification tank member, and a vacuum forming member Accordingly, each component of the titanium tetrachloride purification apparatus can be in a depressurized state, and purification can be performed on titanium tetrachloride in such a depressurized state, whereby the boiling point of titanium tetrachloride or the like can be lowered, It is possible to purify titanium tetrachloride while reducing energy consumption.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view showing a configuration of a titanium tetrachloride purifying apparatus according to an embodiment of the present invention; FIG.
2 is a view showing the structure of a separation column member constituting a titanium tetrachloride purification apparatus according to an embodiment of the present invention;
3 is a view showing a structure of a cold trap member constituting a titanium tetrachloride purifying apparatus according to an embodiment of the present invention.

Hereinafter, a titanium tetrachloride purifying apparatus according to an embodiment of the present invention will be described with reference to the drawings.

FIG. 1 is a view schematically showing the construction of a titanium tetrachloride purifying apparatus according to an embodiment of the present invention. FIG. 2 is a view showing the structure of a separation column member constituting a titanium tetrachloride purifying apparatus according to an embodiment of the present invention. And FIG. 3 is a view showing the structure of a cold trap member constituting the titanium tetrachloride purifying apparatus according to an embodiment of the present invention.

1 to 3, the titanium tetrachloride purification apparatus 100 according to the present embodiment includes a raw material receiving tank member 110, a purification reactor member 115, a separation column member 120, A cleaning tank 130, a purification tank member 145, and a vacuum forming member 170.

In the raw material receiving tank member 110, titanium tetrachloride as a raw material to be refined is contained in a liquid state.

The refill reactor member 115 has a built-in heater to heat titanium tetrachloride supplied from the raw material receiving tank member 110.

The separation column member 120 separates the foreign substances in the titanium tetrachloride heated in the purification reactor member 115.

The separation column member 120 includes an isolation column main body 121 sealed to the outside, a separation column inflow pipe 122 communicating the separation column main body 121 and the purification reactor member 115, A separating column reducing pipe 124 for reducing an object to be reduced to the purifying reactor member 115 among the substances separated from the separating column main body 121 to the purifying reactor member 115, And a separation column outlet pipe 123 for discharging a substance not to be reduced to the purified reactor member 115 out of the separated materials.

The separation column inlet pipe 122 is connected to the bottom of the separation column body 121 at a predetermined height and the separation column reduction pipe 124 is connected to a lower portion of the separation column body 121 , And the separation column outlet pipe (123) is connected to the upper part of the separation column body (121). The liquid component of the material flowing from the purification reactor member 115 through the separation column inlet pipe 122 into the separation column body 121 flows through the separation column reduction pipe 124 into the purification reactor member 122, And the gaseous component of the substance introduced into the separation column body 121 through the separation column inlet pipe 122 from the purification reactor member 115 flows into the separation column outlet pipe 123, And is discharged from the separation column body 121 through the separation column body 121.

The condensing member 130 condenses titanium tetrachloride from which the foreign substance is separated from the separation column member 120.

The condensing member 130 is a part of a refrigeration cycle (not shown) having a compressor, an expansion valve, an evaporator, and the like, and functions as a condenser.

The purification tank member 145 accommodates condensed titanium tetrachloride in the condensing member 130.

The titanium tetrachloride purification apparatus 100 may include a foreign matter receiving tank member 140 for receiving a foreign object separated from the separation column member 120 separately from the tablet tank member 145.

The foreign matter receiving tank member 140 and the tablet tank member 145 are separately installed.

Reference numeral 160 denotes a filter member for filtering titanium tetrachloride contained in the refining tank member 145. Reference numeral 161 denotes a particle counting member for counting foreign substances in titanium tetrachloride via the filter member 160. Reference numeral 161 Is a purified water receiving tank member for containing titanium tetrachloride in which foreign matter is counted in the particle counting member (161) and a foreign substance value is lowered within a required range.

The purified titanium tetrachloride contained in the purified water containing tank member 165 can be charged into the container for external transfer.

The vacuum forming member 170 is formed of titanium tetrachloride (TiCl4) in the raw material receiving tank member 110, the refill reactor member 115, the separating column member 120, the condensing member 130, The separating column member 120, the condensing member 130, and the refill tank member 145 can be decompressed (pressurized) so that the raw material containing tank member 110, the refining reactor member 115, the separating column member 120, I will.

In detail, the vacuum forming member 170 includes a vacuum pump 171 for applying a negative pressure for depressurizing, and a vacuum pump 171 for connecting the vacuum pump 171 and each component of the titanium tetrachloride purifying apparatus 100, The negative pressure of the vacuum pump 171 by connecting the tank member 110, the refill reactor member 115, the separating column member 120, the condensing member 130 and the refill tank member 145, A vacuum forming piping for allowing the raw material storing tank member 110, the purifying reactor member 115, the separating column member 120, the condensing member 130 and the purifying tank member 145 to be in a depressurized state, Lt; / RTI >

High purity nitrogen, argon, or the like, which is an inert gas, may flow into the vacuum forming pipe 172.

The vacuum forming pipe 172 may be directly connected to each component as in the raw material receiving tank member 110 or the like and may be connected to the purification tank member 145 indirectly connected through the condensing member 130, Or indirectly connected to each component.

A cold trap member 150 capable of liquefying titanium tetrachloride flowing out of the refining tank member 145 is disposed between the refining tank member 145 and the vacuum forming member 170. In this embodiment,

In detail, the cold trap member 150 includes a cold trap body 151, a cold trap inflow pipe 152 through which the titanium tetrachloride flows from the outside into the cold trap body 151, A plurality of protrusions 154 protruding from the inner wall of the cold trap body 151 in a staggered manner so as to flow zigzag in the cold trap body 151; And a chiller 155 capable of delivering cold air into the cold trap body 151.

The titanium tetrachloride introduced through the cold trap inflow pipe 152 is raised by the cool air supplied from the chiller 155 in a zigzag manner inside the cold trap body 151 by the protrusion 154 And can be cooled and liquefied.

As described above, when the cold trap member 150 is installed, the problem that the titanium tetrachloride is sucked out through the vacuum forming pipe 172 is eliminated when the titanium tetrachloride is in a gaseous state, The foreign matter can be removed once more.

In this embodiment, heating is performed to the boiling point of the foreign substances in the titanium tetrachloride supplied from the raw material receiving tank member 110 and heating up to the boiling point of titanium tetrachloride in the refining reactor member 115 in sequence, In the case where heating is performed from the member 115 to the boiling point of the foreign substance in the titanium tetrachloride, the foreign substance receiving tank member 140 is opened to receive foreign matter separated from the titanium tetrachloride, and from the refining reactor member 115 to the boiling point of titanium tetrachloride When heating is performed, the refining tank member 145 is opened to accommodate the titanium tetrachloride in which the foreign substance is separated.

That is, when the refining reactor member 115 heats the titanium tetrachloride to the boiling point of the foreign material in the titanium tetrachloride supplied from the raw material containing tank member 110, the foreign substances in titanium tetrachloride are vaporized first. At this time, the refining tank member 145 is closed and the foreign material receiving tank member 140 is opened, so that the vaporized foreign material is received in the foreign material receiving tank member 140, and the liquid titanium tetrachloride And is reduced toward the refill reactor member 115.

After this process, when the refining reactor member 115 heats the titanium tetrachloride to the boiling point of the titanium tetrachloride supplied from the raw material receiving tank member 110, titanium tetrachloride is vaporized. At this time, the foreign matter containing tank member 140 is closed and the purified tank member 145 is opened, so that the vaporized titanium tetrachloride can be received in the purified tank member 145.

As described above, according to the titanium tetrachloride purifying apparatus 100 according to the present embodiment, purification, filtering and container charging up to titanium tetrachloride can be performed all at once in one system, and thus, in the purification process of titanium tetrachloride, And exposure to moisture can be minimized, formation of titanium dioxide and the like due to exposure to such air and moisture can be suppressed.

The container of each component of the titanium tetrachloride purifying apparatus 100 may be made of stainless steel and Teflon which are treated by electrolytic polishing (EP) to withstand corrosion of titanium tetrachloride.

Hereinafter, the operation of the titanium tetrachloride purification apparatus 100 will be described with reference to the drawings.

A negative pressure formed by operating the vacuum pump 171 is entirely hung through each component of the titanium tetrachloride purifying apparatus 100 through the vacuum forming pipe 172 to remove the components of the titanium tetrachloride purifying apparatus 100 Is in a decompressed state as a whole.

In this state, titanium tetrachloride flows from the raw material storing tank member 110 to the refining reactor member 115 side.

In the refining reactor member 115, the heating up to the boiling point of the foreign substances in the titanium tetrachloride supplied from the raw material receiving tank member 110 and the heating to the boiling point of titanium tetrachloride are sequentially performed, The foreign matter is received in the foreign matter receiving tank member 140 via the separating column member 120 through the condensing member 130 and the titanium tetrachloride is received in the refining tank member 145 via the condensing member 130. [ do.

The titanium tetrachloride contained in the refining tank member 145 is liquefied while passing through the cold trap member 150 and sequentially passes through the filter member 160 and the particle counting member 161, And is finally accommodated in the tank member 165.

As described above, the titanium tetrachloride purification apparatus 100 includes the raw material receiving tank member 110, the purification reactor member 115, the separating column member 120, the condensing member 130, the refining tank member 145 And the vacuum forming member 170, each component of the titanium tetrachloride purifying apparatus 100 can be depressurized, and since purification against titanium tetrachloride can be made in such a depressurized state, As a result, the boiling point of titanium tetrachloride and the like can be lowered, so that the heating energy is reduced and the titanium tetrachloride can be purified while reducing energy consumption.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the following claims And can be changed. However, it is intended that the present invention covers the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.

The titanium tetrachloride purifying apparatus according to one aspect of the present invention can purify titanium tetrachloride while reducing energy consumption, so that the titanium tetrachloride purifying apparatus has high industrial applicability.

100: titanium tetrachloride refining apparatus 110: raw material receiving tank member
115: Purification reactor member 120: Separation column member
130: condensing member 140: foreign matter receiving tank member
145: refill tank member 150: cold trap member
160: Filter member 161: Particle counting member
165: purified water receiving tank member 170: vacuum forming member

Claims (4)

A raw material receiving tank member containing titanium tetrachloride (TiCl 4 ) to be refined;
A refill reactor member capable of heating titanium tetrachloride supplied from the raw material receiving tank member;
A separation column member capable of separating foreign substances in titanium tetrachloride heated in the refining reactor member;
A condensing member for condensing the titanium tetrachloride from which the foreign substance is separated from the separation column member;
A refining tank member for containing titanium tetrachloride condensed in the condensing member; And
The purification reactor member, the separation column member, the separation column member, the separation column member, the separation column member, and the separation column member so that the titanium tetrachloride can be processed in the decompressed state in the raw material containing tank member, the purified reactor member, And a vacuum forming member for decompressing the member, the condensing member, and the purification tank member. The method according to claim 1,
The titanium tetrachloride purification apparatus
And a cold trap member disposed between the refill tank member and the vacuum forming member and capable of liquefying titanium tetrachloride flowing out of the refill tank member. The method according to claim 1,
The titanium tetrachloride purification apparatus
And a foreign matter receiving tank member for receiving foreign matter separated from the separation column member. The method of claim 3,
In the refining reactor member, heating up to the boiling point of the foreign substance in the titanium tetrachloride supplied from the raw material receiving tank member and heating to the boiling point of titanium tetrachloride are sequentially performed,
Wherein when the refining reactor member is heated up to the boiling point of the foreign substance in the titanium tetrachloride, the foreign substance receiving tank member is opened to receive the foreign substance separated from the titanium tetrachloride,
Wherein when the refining reactor member is heated to the boiling point of titanium tetrachloride, the refining tank member is opened to receive the titanium tetrachloride from which the foreign substance is separated.
KR1020150090332A 2015-06-25 2015-06-25 Titanium tetrachloride refine apparatus KR101625823B1 (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107162045A (en) * 2017-07-04 2017-09-15 贵州省分析测试研究院 Method for removing impurity in titanium tetrachloride
KR102017682B1 (en) * 2018-02-27 2019-09-03 고등기술연구원연구조합 Purification method for titanium tetrachloride
CN112062151A (en) * 2020-09-01 2020-12-11 洛阳双瑞万基钛业有限公司 Titanium tetrachloride slurry drying device and drying method
KR20210085314A (en) * 2019-12-30 2021-07-08 고등기술연구원연구조합 Manufacturing apparatus of refining titanium tetrachloride and manufacturing method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002187718A (en) 2000-12-20 2002-07-05 Sumitomo Titanium Corp METHOD OF REFINING TiCl4
JP2007302522A (en) 2006-05-12 2007-11-22 Toho Titanium Co Ltd Method of refining titanium tetrachloride and refiner used for the same
JP2010030857A (en) 2008-07-30 2010-02-12 Toho Titanium Co Ltd Distillation refining apparatus for titanium tetrachloride, method of maintenance of the apparatus and method for refining titanium tetrachloride with the apparatus
JP2013063893A (en) 2011-08-29 2013-04-11 Osaka Titanium Technologies Co Ltd Maintenance method of titanium tetrachloride production facility, and titanium tetrachloride production facility

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002187718A (en) 2000-12-20 2002-07-05 Sumitomo Titanium Corp METHOD OF REFINING TiCl4
JP2007302522A (en) 2006-05-12 2007-11-22 Toho Titanium Co Ltd Method of refining titanium tetrachloride and refiner used for the same
JP2010030857A (en) 2008-07-30 2010-02-12 Toho Titanium Co Ltd Distillation refining apparatus for titanium tetrachloride, method of maintenance of the apparatus and method for refining titanium tetrachloride with the apparatus
JP2013063893A (en) 2011-08-29 2013-04-11 Osaka Titanium Technologies Co Ltd Maintenance method of titanium tetrachloride production facility, and titanium tetrachloride production facility

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107162045A (en) * 2017-07-04 2017-09-15 贵州省分析测试研究院 Method for removing impurity in titanium tetrachloride
KR102017682B1 (en) * 2018-02-27 2019-09-03 고등기술연구원연구조합 Purification method for titanium tetrachloride
KR20210085314A (en) * 2019-12-30 2021-07-08 고등기술연구원연구조합 Manufacturing apparatus of refining titanium tetrachloride and manufacturing method thereof
KR102321997B1 (en) 2019-12-30 2021-11-08 고등기술연구원연구조합 Manufacturing apparatus of refining titanium tetrachloride and manufacturing method thereof
CN112062151A (en) * 2020-09-01 2020-12-11 洛阳双瑞万基钛业有限公司 Titanium tetrachloride slurry drying device and drying method

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