High purity tungsten pentachloride and production method thereof

Patent metadata

Field	Value
Publication number	US-2019233301-A1
Application number	US-201716338020-A
Country	US
Kind code	A1
Filing date	Oct 6, 2017
Priority date	Dec 5, 2016
Publication date	Aug 1, 2019
Grant date	—

Abstract

Provided are high purity tungsten pentachloride, and a method for obtaining such high purity tungsten pentachloride at a high yield and in an efficient manner. Tungsten pentachloride in which a total content of metal impurities excluding Sb, Ti, and As is less than 10 wtppm is obtained by uniformly mixing one or more types of reducing agents selected from Sb, Ti, and As and tungsten hexachloride at a molar ratio of 1.0:2.0 to 1.0:5.0 (reducing agent/WCl6 ratio) in an inert atmosphere to obtain a mixture, heating and reducing the mixture for 1 to 100 hours in a temperature range in which a chloride of tungsten and the reducing agent becomes a liquid phase to obtain a reduced product, heating the reduced product for 1 to 100 hours at 100 Pa or less and in a temperature range of 90 to 130° C., and performing reduced-pressure distillation thereto to obtain a reduced-pressure distilled product, heating and sublimating the reduced-pressure distilled product for 1 to 100 hours at 100 Pa or less and in a temperature range of 130 to 170° C., and performing sublimation purification of achieving precipitation at 70 to 120° C.

First claim

1 . Tungsten pentachloride, wherein a total content of metal impurities excluding Sb, Ti, and As is less than 10 wtppm.

2 . The tungsten pentachloride according to claim 1 , wherein a content of Mo is 2 wtppm or less.

3 . The tungsten pentachloride according to claim 1 or claim 2 , wherein a total content of one or more elements selected from Sb, Ti, and As falls within a range of 0.01 wtppm or more and 200000 wtppm or less.

4 . The tungsten pentachloride according to claim 3 , wherein a content of any one of elements among Sb, Ti, and As falls within a range of either 0.01 wtppm or more and less than 1 wtppm, or 500 wtppm or more and 200000 wtppm or less.

5 . The tungsten pentachloride according to claim 4 , wherein a total content of tungsten dichloride, tungsten tetrachloride, tungsten hexachloride, and tungsten acid chloride is 5 wt % or less.

6 . A method of producing tungsten pentachloride, comprising the steps of:
uniformly mixing one or more types of reducing agents selected from Sb, Ti, and As and tungsten hexachloride at a molar ratio of 1.0:2.0 to 1.0:5.0 (reducing agent/WCl 6 ratio) in an inert atmosphere to obtain a mixture; heating and reducing the mixture for 1 to 100 hours in a temperature range in which a chloride of tungsten and the reducing agent becomes a liquid phase to obtain a reduced product; heating the reduced product for 1 to 100 hours at 100 Pa or less and in a temperature range of 90 to 130° C., and performing reduced-pressure distillation thereto to obtain a reduced-pressure distilled product; and heating and sublimating the reduced-pressure distilled product for 1 to 100 hours at 100 Pa or less and in a temperature range of 130 to 170° C., and performing sublimation purification of achieving precipitation at 70 to 120° C. to obtain tungsten pentachloride.

7 . The production method of tungsten pentachloride according to claim 6 , wherein a grain size of raw materials upon reduction is 200 μm or less.

8 . The production method of tungsten pentachloride according to claim 7 , wherein Ti is used as the reducing agent.

9 . The production method of tungsten pentachloride according to claim 8 , wherein a pressure and a temperature in which a chloride of tungsten and the reducing agent becomes a liquid phase are 0.1 to 2 MPa and 70 to 130° C., respectively.

10 . The production method of tungsten pentachloride according to claim 9 , wherein reduction is performed in a dry nitrogen flow atmosphere having a moisture content of 10 wtppm or less.

11 . The production method of tungsten pentachloride according to claim 10 , wherein a yield of tungsten pentachloride is 65% or higher.

12 . The production method of tungsten pentachloride according to claim 6 , wherein Ti is used as the reducing agent.

13 . The production method of tungsten pentachloride according to claim 6 , wherein a pressure and a temperature in which a chloride of tungsten and the reducing agent becomes a liquid phase are 0.1 to 2 MPa and 70 to 130° C., respectively.

14 . The production method of tungsten pentachloride according to claim 6 , wherein reduction is performed in a dry nitrogen flow atmosphere having a moisture content of 10 wtppm or less.

15 . The production method of tungsten pentachloride according to claim 6 , wherein a yield of tungsten pentachloride is 65% or higher.

16 . The tungsten pentachloride according to claim 1 , wherein a total content of one or more elements selected from Sb, Ti, and As falls within a range of 0.01 wtppm or more and 200000 wtppm or less.

17 . The tungsten pentachloride according to claim 1 , wherein a content of any one of elements among Sb, Ti, and As falls within a range of either 0.01 wtppm or more and less than 1 wtppm, or 500 wtppm or more and 200000 wtppm or less.

18 . The tungsten pentachloride according to claim 1 , wherein a total content of tungsten dichloride, tungsten tetrachloride, tungsten hexachloride, and tungsten acid chloride is 5 wt % or less.

Assignees

• Jx Nippon Mining & Metals Corp

Inventors

• Takahashi Hideyuki

Classifications

• C01P2006/80

  Compositional purity · CPC title

• C01G41/04 Primary

  Halides · CPC title

• C01G30/007

  of binary type SbX3 or SbX5 with X representing a halogen, or mixed of the type SbX3X'2 with X,X' representing different halogens · CPC title

• C01G28/007

  Halides (C01G28/001 takes precedence) · CPC title

• C01G23/022

  Titanium tetrachloride · CPC title