High purity tungsten pentachloride and method for synthesizing same

Patent metadata

Field	Value
Publication number	US-10843934-B2
Application number	US-201716073288-A
Country	US
Kind code	B2
Filing date	Jan 13, 2017
Priority date	Jan 28, 2016
Publication date	Nov 24, 2020
Grant date	Nov 24, 2020

Abstract

The purpose of the present invention is to safely synthesize high purity tungsten pentachloride at a higher yield and at a higher purity than in prior art. This method for producing tungsten pentachloride includes: a step of mixing a reducing agent selected from the group consisting of Bi, Hg, Sb, Ti, Al, P, and As with tungsten hexachloride uniformly in an inert atmosphere with a molar ratio of the tungsten hexachloride to the reducing agent being 2.8:1.0 to 3.2:1.0 to obtain a mixture; a step of heating the mixture of the reducing agent and the tungsten hexachloride to 80 to 210° C. at 13 Pa or lower and reducing the same; a step of heating the reduced product of the mixture of the reducing agent and the tungsten hexachloride to 120 to 290° C. at 66 Pa or lower and vacuum distilling the same to remove impurities; and a step of heating the reduced product from which impurities have been removed by the vacuum distillation to 140 to 350° C. at 13 Pa or lower and purifying the same by sublimation to obtain the tungsten pentachloride.

First claim

The invention claimed is:

1. A method for producing tungsten pentachioride, comprising the steps of:
uniformly mixing at least one reducing agent selected from the group consisting of Bi, Hg, Sb, Ti, Al, P and As with tungsten hexachloride in a molar ratio of tungsten hexachloride:reducing agent of from 2.8:1.0 to 3.2:1.0 in an inert atmosphere to obtain a mixture;
reducing the mixture by heating the mixture at a temperature of from 80 to 210° C. under a pressure of 13 Pa or less thereby producing a crude mixture;
heating the crude mixture to a temperature of from 120 to 290° C. under a pressure of 66 Pa or less to remove impurities; and
subjecting the resulting mixture obtained from the heating step to sublimation purification by heating the resulting mixture at a temperature of from 140 to 350° C. under a reduced pressure of 13 Pa or less to obtain a purified tungsten pentachloride.

2. The method for producing tungsten pentachloride according to claim 1 , wherein the step of uniformly mixing the reducing agent with the tungsten hexachloride in the inert atmosphere to obtain the mixture comprises grinding the tungsten hexachloride and the reducing agent using an mortar or a ball mill in an inert atmosphere such that the maximum particle diameter of each of the tungsten hexachloride and the reducing agent is 300 pm or less, and uniformly mixing them to obtain the mixture.

3. The method for producing tungsten pentachloride according to claim 1 , wherein the tungsten pentachloride has a compound purity of 95% by mass or more.

4. The method for producing tungsten pentachloride according to claim 1 , wherein the total content of metal impurities excluding the reducing agent is less than 10 ppm (purity 5N).

5. The method for producing tungsten pentachloride according to claim 1 , wherein the tungsten pentachloride comprises 1 ppm to 350 ppm of at least one element of the reducing agent.

6. The method for producing tungsten pentachloride according to claim 1 , wherein the tungsten pentachloride has a Mo content of 0.5 ppm or less.

7. The method for producing tungsten pentachloride according to claim 2 , wherein the tungsten pentachloride has a compound purity of 95% by mass or more.

8. The method for producing tungsten pentachloride according to claim 2 , wherein the total content of metal impurities excluding the reducing agent is less than 10 ppm (purity 5N).

9. The method for producing tungsten pentachloride according to claim 7 , wherein the total content of metal impurities excluding the reducing agent is less than 10 ppm (purity 5N).

10. The method for producing tungsten pentachloride according to claim 2 , wherein the tungsten pentachloride comprises 1 ppm to 350 ppm of at least one element of the reducing agent.

11. The method for producing tungsten pentachloride according to claim 3 , wherein the tungsten pentachloride comprises 1 ppm to 350 ppm of at least one element of the reducing agent.

12. The method for producing tungsten pentachloride according to claim 4 , wherein the tungsten pentachloride comprises 1 ppm to 350 ppm of at least one element of the reducing agent.

13. The method for producing tungsten pentachloride according to claim 2 , wherein the tungsten pentachloride has a Mo content of 0.5 ppm or less.

14. The method for producing tungsten pentachloride according to claim 3 , wherein the tungsten pentachloride has a Mo content of 0.5 ppm or less.

15. The method for producing tungsten pentachloride according to claim 4 , wherein the tungsten pentachloride has a Mo content of 0.5 ppm or less.

16. The method for producing tungsten pentachloride according to claim 5 , wherein the tungsten pentachloride has a Mo content of 0.5 ppm or less.

Assignees

• Jx Nippon Mining & Metals Corp

Inventors

• Takahashi Hideyuki
• Momoi Hajime

Classifications

• C01G41/04 Primary

  Halides · CPC title

• C01P2006/80

  Compositional purity · CPC title