Method for surface-modifying metal silicide, and method and apparatus for preparing trichlorosilane using surface-modified metal silicide

Patent metadata

Field	Value
Publication number	US-2016332149-A1
Application number	US-201515110229-A
Country	US
Kind code	A1
Filing date	Jan 19, 2015
Priority date	Jan 23, 2014
Publication date	Nov 17, 2016
Grant date	—

Abstract

A method for preparing trichlorosilane according to an embodiment of the present invention comprises the steps of: supplying surface-modified metal silicide and metal grade silicon to a reaction unit; supplying silicon tetrachloride and hydrogen to the reaction unit; and supplying a product, which is generated by a reaction of metal grade silicon, silicon tetrachloride, and hydrogen in the presence of metal silicide in the reaction unit, to a separation unit, and separating a trichlorosilane component. In cases where a silicon tetrachloride hydrochlorination reaction is performed using the method for preparing trichlorosilane according to the embodiment of the present invention, the yield of trichlorosilane can be raised.

First claim

1 . A method for surface-modifying metal silicide, the method comprising:
supplying silicon tetrachloride and inert gas to a modification reaction unit filled with metal silicide; modifying the surface of the metal silicide by heating the modification reaction unit to which the silicon tetrachloride and the inert gas are supplied; and cooling the surface-modified metal silicide while flowing the inert gas in the heated modification reaction unit.

2 . The method for surface-modifying metal silicide of claim 1 , wherein the metal silicide includes copper (Cu), aluminum (Al), and iron (Fe) as metal components.

3 . The method for surface-modifying metal silicide of claim 2 , wherein the content of aluminum (Al) in the metal silicide is 0.2 wt % or more to 0.76 wt % or less, and the content of iron (Fe) is 0.1 wt % or more to 0.24 wt % or less.

4 . The method for surface-modifying metal silicide of claim 2 , wherein a molar ratio of silicon (Si) and copper (Cu) which are present on the surface of the metal silicide has a range of 1 or more to 30 or less.

5 . The method for surface-modifying metal silicide of claim 1 , wherein the metal silicide includes nickel (Ni), aluminum (Al), and iron (Fe) as metal components.

6 . The method for surface-modifying metal silicide of claim 5 , wherein the content of aluminum (Al) in the metal silicide is 0.16 wt % or more to 0.61 wt % or less, and the content of iron (Fe) is 0.04 wt % or more to 0.39 wt % or less.

7 . The method for surface-modifying metal silicide of claim 5 , wherein a molar ratio of silicon (Si) and nickel (Ni) which are present on the surface of the metal silicide has a range of 1 or more to 40 or less.

8 . The method for surface-modifying metal silicide of claim 1 , wherein the silicon tetrachloride and the inert gas are supplied to the modification reaction unit with a molar ratio in a range of 1:1 to 1:10.

9 . A method for preparing trichlorosilane, the method comprising:
supplying surface-modified metal silicide and metal grade silicon to a reaction unit; supplying silicon tetrachloride and hydrogen to the reaction unit; and supplying a product, which is generated by a reaction of the metal grade silicon, the silicon tetrachloride, and the hydrogen in the presence of the metal silicide in the reaction unit, to a separation unit, and separating a trichlorosilane component, wherein the surface-modified metal silicide is formed by a reaction of the metal silicide and the silicon tetrachloride in an inert gas atmosphere.

10 . The method for preparing trichlorosilane of claim 9 , wherein the metal silicide includes at least one selected from copper (Cu) and nickel (Ni) and at least one selected from aluminum (Al) and iron (Fe) as a metal component.

11 . The method for preparing trichlorosilane of claim 9 , wherein the metal grade silicon is repetitively supplied to the reaction time at a time interval.

12 . The method for preparing trichlorosilane of claim 9 , wherein the pressure of the reaction unit is set to a range of 1 atm or more to 50 atm or less.

13 . The method for preparing trichlorosilane of claim 9 , wherein the temperature of the reaction unit is set to a range of 300° C. or more to 1,000° C. or less.

14 . The method for preparing trichlorosilane of claim 9 , the method further comprising: recirculating the remaining components except for the trichlorosilane of the product from the separation unit to the reaction unit.

15 . An apparatus for preparing trichlorosilane, the apparatus comprising:
a modification reaction unit in which while metal silicide is charged and inert gas and silicon tetrachloride are supplied onto the metal silicide, a surface-modification reaction of the metal silicide occurs; a reaction unit which is connected to the modification reaction unit to generates trichlorosilane while the surface-modified metal silicide flows into the reaction unit and metal grad silicon, hydrogen, and the silicon tetrachloride are supplied on to the surface-modified metal silicide; and a separation unit which is connected to the reaction unit to receive the product generated in the reaction unit and separate a trichlorosilane component from the product.

16 . The apparatus for preparing trichlorosilane of claim 15 , the apparatus further comprising: a storage unit which temporarily stores the trichlorosilane separated from the separation unit.

17 . The apparatus for preparing trichlorosilane of claim 15 , wherein the separation unit further includes a first processing pipe which transfers the trichlorosilane separated from the product to the storage unit and a second processing pipe which recirculates the remaining components except for the trichlorosilane of the product to the reaction unit.

18 . The apparatus for preparing trichlorosilane of claim 15 , wherein the metal silicide includes at least one selected from copper (Cu) and nickel (Ni) and at least one selected from aluminum (Al) and iron (Fe) as a metal component.

19 . The apparatus for preparing trichlorosilane of claim 15 , wherein the reaction unit is formed by at least one selected from a fixed bed reactor, a mixing type reactor, and a fluidized bed reactor.

Assignees

• Korea Res Inst Chemical Tech
• Hanwha Chemical Corp

Inventors

• Choi Won Choon
• Park Yong Ki
• Lee Woo Hyung
• Seo Hwi Min
• Kang Na Young
• Han Joo Hee
• Lee Dong Ho
• Ahn Gui Ryong
• Kim Gil Ho

Classifications

• B01J4/002

  Nozzle-type elements (nozzle-type reactors B01J19/26) · CPC title

• C01B33/10763

  from silicon · CPC title

• C01B33/06

  Metal silicides (alloys C22) · CPC title

• B01J2523/00

  Constitutive chemical elements of heterogeneous catalysts · CPC title

• B01J37/0209

  involving a reaction between the support and a fluid · CPC title