Hydrogen fluoride purification method

Patent metadata

Field	Value
Publication number	US-9260306-B2
Application number	US-200913131703-A
Country	US
Kind code	B2
Filing date	Nov 25, 2009
Priority date	Nov 28, 2008
Publication date	Feb 16, 2016
Grant date	Feb 16, 2016

Abstract

A novel method for purifying hydrogen fluoride, capable of efficiently reducing the content of arsenic in hydrogen fluoride. The method includes the steps of (a) bringing a crude hydrogen fluoride containing arsenic trifluoride into contact with an oxidizing agent of a metal fluoride in a liquid state in a reactor to obtain a reaction mixture, wherein arsenic pentafluoride is formed by oxidizing arsenic trifluoride with the oxidizing agent of the metal fluoride through a liquid-liquid reaction; and (b) separating purified hydrogen fluoride from the reaction mixture by a separator, the thus obtained purified hydrogen fluoride having a lower content of arsenic than that of the crude hydrogen fluoride.

First claim

The invention claimed is:

1. A method for purifying hydrogen fluoride, which comprises the steps of:
(a) bringing a crude hydrogen fluoride containing arsenic trifluoride into contact with an oxidizing agent of a metal fluoride in a liquid state to obtain a reaction mixture wherein arsenic pentafluoride is formed by oxidizing arsenic trifluoride with the oxidizing agent of the metal fluoride through a liquid-liquid reaction, wherein the oxidizing agent of the metal fluoride is used in the form of a double salt or a complex salt of the metal fluoride, and
(b) separating purified hydrogen fluoride from the reaction mixture, the thus obtained purified hydrogen fluoride having a lower content of arsenic than that of the crude hydrogen fluoride.

2. The method according to claim 1 , wherein the double salt or complex salt of the metal fluoride comprises at least one kind selected from the group consisting of AgFAsF 6 , AgFSbF 6 , AgFBiF 6 , AgFBF 4 , AgFAuF 6 , AgFIrF 6 , AgFRuF 6 , AgFAuF 4 , Cs 2 KAgF 6 , and the following formulas:
A II M II F 4 ,
A I M III F 4 ,
A II M III F 5 ,
A I M IV F 5 ,
A II M IV F 6 ,
A I M V F 6 , and
A II M V F 7

wherein
A I =Li, Na, Ag, K, Rb, or Cs
A II =Ca, Sr, Ba, Cd, or Hg
M II =Ag,
M III =Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zr, Mo, Ru, Rh, Pd, Ag, Ir, or Au,
M IV =Ti, V, Cr, Mn, Co, Ni, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, Hf, W, Re, Os, Ir, Pt, or Hg, and
M V =Nb, Mo, Ru, Rh, Ta, W, Re, Os, Ir, Pt, Au, or Bi.

3. The method according to claim 1 , wherein the reaction mixture obtained in the step (a) comprises a reduced metal fluoride derived from the oxidizing agent, and the reduced metal fluoride is utilized so as to obtain the oxidizing agent of the metal fluoride.

4. The method according to claim 1 , wherein the step (b) is carried out by the steps of:
(i) bringing the reaction mixture into contact with a Lewis basic fluoride to form a double salt or a complex salt of arsenic pentafluoride and the Lewis basic fluoride, thereby obtaining a contact mixture in which arsenic pentafluoride is immobilized, and
(ii) separating a purified hydrogen fluoride from the contact mixture.

5. The method according to claim 4 , wherein the step (i) comprises separating a hydrogen fluoride fraction containing arsenic pentafluoride from the reaction mixture, and bringing the hydrogen fluoride fraction into contact with the Lewis basic fluoride.

6. The method according to claim 4 , wherein the Lewis basic fluoride contains at least one kind selected from the group consisting of LiF, NaF, KF, RbF, CsF, AgF, BeFz, MgF 2 , SrF 2 , CaF 2 , and BaF 2 .

7. The method according to claim 1 , wherein a double salt or a complex salt of arsenic pentafluoride and the metal fluoride derived from the oxidizing agent is formed in the reaction mixture obtained in the step (a), thereby immobilizing arsenic pentafluoride, and
step (b) is carried out by directly separating a purified hydrogen fluoride from the reaction mixture.

8. The method according to claim 1 , wherein the content of arsenic of the crude hydrogen fluoride is from 3,000 to 3 ppm by mass.

9. The method according to claim 1 , wherein the content of arsenic of the purified hydrogen fluoride is 3 ppm by mass or less.

10. A method for producing hydrogen fluoride, which comprises:
reacting fluorite with sulfuric acid to obtain a crude hydrogen fluoride, and
subjecting the crude hydrogen fluoride to the purification method according to claim 1 to obtain a purified hydrogen fluoride.

11. The method according to claim 10 , wherein the content of arsenic of fluorite is from 10,000 to 3 ppm by mass.

12. The method according to claim 1 , wherein the oxidizing agent of the metal fluoride is at least one selected from the group consisting of (i) a complex salt of AgF 2 and a Lewis acidic fluoride and (ii) a complex salt of NiF 4 or MnF 4 and a Lewis basic fluoride.

13. The method according to claim 10 , wherein the oxidizing agent of the metal fluoride is at least one selected from the group consisting of (i) a complex salt of AgF 2 and a Lewis acidic fluoride and (ii) a complex salt of NiF 4 or MnF 4 and a Lewis basic fluoride.

Assignees

• Hagiwara Rika
• Matsumoto Kazuhiko
• Univ Kyoto

Inventors

• Hagiwara Rika
• Matsumoto Kazuhiko

Classifications

• C01B7/195 Primary

  Separation; Purification · CPC title