Method for purifying chlorosilane

Patent metadata

Field	Value
Publication number	US-2017190585-A1
Application number	US-201515325127-A
Country	US
Kind code	A1
Filing date	Jul 2, 2015
Priority date	Jul 10, 2014
Publication date	Jul 6, 2017
Grant date	—

Abstract

First, at least one of silanol and a siloxane compound is generated in a chlorosilane (S 101 ). In the step, for example, an inert gas having a moisture concentration of 0.5 to 2.5 ppm is brought into contact with the chlorosilane to dissolve the moisture, and at least one of silanol and a siloxane compound is generated through a hydration reaction of a moiety of the chlorosilane. Next, a boron-containing compound contained in the chlorosilane is reacted with the silanol or the siloxane compound, thereby converting the boron-containing compound to a boron oxide (S 102 ). Through the step (S 102 ), the boron-containing compound being a low boiling point compound is converted to a boron oxide being a high boiling point compound, and therefore the difference in boiling point from the boiling point of chlorosilane becomes larger to make later separation easy.

First claim

1 . A method for purifying a chlorosilane by removing a boron-containing compound in the chlorosilane, comprising the following (A) to (C):
(A) generating at least one of silanol and a siloxane compound in the chlorosilane; (B) reacting a boron-containing compound comprised in the chlorosilane with the silanol or the siloxane compound, thereby converting the boron-containing compound to a boron oxide; and (C) distilling the chlorosilane to remove the boron oxide.

2 . The method for purifying a chlorosilane according to claim 1 , wherein (B) further comprises allowing the boron oxide to adsorb a metal-containing compound comprised in the chlorosilane, thereby converting the metal-containing compound to an addition compound, and (C) further comprises removing the addition compound.

3 . A method for purifying a chlorosilane by removing a metal-containing compound in the chlorosilane, comprising the (D) to (F):
(D) generating at least one of silanol and a siloxane compound in the chlorosilane; (E) allowing the silanol or the siloxane compound to adsorb the metal-containing compound comprised in the chlorosilane, thereby converting the metal-containing compound to an addition compound; and (F) distilling the chlorosilane to remove the addition compound.

4 . The method for purifying a chlorosilane according to claim 1 , wherein, in (A), an inert gas having a moisture concentration of 0.5 to 2.5 ppm is brought into contact with the chlorosilane to dissolve the moisture, thereby generating at least one of the silanol and the siloxane compound through a hydration reaction of a moiety of the chlorosilane.

5 . The method for purifying a chlorosilane according to claim 1 , wherein, in (A), an unpurified chlorosilane comprising at least one of silanol and a siloxane compound is added to the chlorosilane to generate at least one of the silanol and the siloxane compound in the chlorosilane.

6 . The method for purifying a chlorosilane according to claim 5 , wherein the unpurified chlorosilane is at least one of an unpurified chlorosilane obtained by reacting metallic silicon with hydrochloric acid, an unpurified chlorosilane obtained by reacting metallic silicon with silicon tetrachloride, and an unreacted chlorosilane obtained in synthesis of polysilicon using trichlorosilane as a raw material.

7 . The method for purifying a chlorosilane according to claim 1 , wherein the boron-containing compound is at least one compound of a boron chloride and a boron hydride.

8 . The method for purifying a chlorosilane according to claim 3 , wherein the metal-containing compound is at least one chloride of chlorides of any one of iron, chromium, nickel, copper, zinc, aluminum, calcium, and magnesium.

9 . The method for purifying a chlorosilane according to claim 1 , wherein the chlorosilane has a single composition of any one of SiCl 4 , SiHCl 3 , SiH 2 Cl 2 , SiH 3 Cl, and SiH 4 , or the chlorosilane has a mixed composition of a plurality of the single compositions.

10 . The method for purifying a chlorosilane according to claim 2 , wherein, in (A), an inert gas having a moisture concentration of 0.5 to 2.5 ppm is brought into contact with the chlorosilane to dissolve the moisture, thereby generating at least one of the silanol and the siloxane compound through a hydration reaction of a moiety of the chlorosilane.

11 . The method for purifying a chlorosilane according to claim 3 , wherein, in (D), an inert gas having a moisture concentration of 0.5 to 2.5 ppm is brought into contact with the chlorosilane to dissolve the moisture, thereby generating at least one of the silanol and the siloxane compound through a hydration reaction of a moiety of the chlorosilane.

12 . The method for purifying a chlorosilane according to claim 2 , wherein, in (A), an unpurified chlorosilane comprising at least one of silanol and a siloxane compound is added to the chlorosilane to generate at least one of the silanol and the siloxane compound in the chlorosilane.

13 . The method for purifying a chlorosilane according to claim 3 , wherein, in (D), an unpurified chlorosilane comprising at least one of silanol and a siloxane compound is added to the chlorosilane to generate at least one of the silanol and the siloxane compound in the chlorosilane.

14 . The method for purifying a chlorosilane according to claim 12 , wherein the unpurified chlorosilane is at least one of an unpurified chlorosilane obtained by reacting metallic silicon with hydrochloric acid, an unpurified chlorosilane obtained by reacting metallic silicon with silicon tetrachloride, and an unreacted chlorosilane obtained in synthesis of polysilicon using trichlorosilane as a raw material.

15 . The method for purifying a chlorosilane according to claim 13 , wherein the unpurified chlorosilane is at least one of an unpurified chlorosilane obtained by reacting metallic silicon with hydrochloric acid, an unpurified chlorosilane obtained by reacting metallic silicon with silicon tetrachloride, and an unreacted chlorosilane obtained in synthesis of polysilicon using trichlorosilane as a raw material.

16 . The method for purifying a chlorosilane according to claim 2 , wherein the boron-containing compound is at least one compound of a boron chloride and a boron hydride.

17 . The method for purifying a chlorosilane according to claim 2 , wherein the chlorosilane has a single composition of any one of SiCl 4 , SiHCl 3 , SiH 2 Cl 2 , SiH 3 Cl, and SiH 4 , or the chlorosilane has a mixed composition of a plurality of the single compositions.

18 . The method for purifying a chlorosilane according to claim 3 , wherein the chlorosilane has a single composition of any one of SiCl 4 , SiHCl 3 , SiH 2 Cl 2 , SiH 3 Cl, and SiH 4 , or the chlorosilane has a mixed composition of a plurality of the single compositions.

Assignees

• Shinetsu Chemical Co

Inventors

• Miyao Shuichi
• Ishida Masahiko
• Yoshida Atsushi
• Netsu Shigeyoshi

Classifications

• B01D3/14

  Fractional distillation {or use of a fractionation or rectification column} · CPC title

• C01B33/107

  Halogenated silanes · CPC title

• C01B33/10794 Primary

  by forming addition compounds or complexes, the reactant being possibly contained in an adsorbent · CPC title

• C01B33/1071

  Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof · CPC title

• C01B33/10789

  the adsorbing material being formed in situ, e.g. by partial hydrolysis · CPC title