Method for preparing a halosilane

Patent metadata

Field	Value
Publication number	US-9688703-B2
Application number	US-201415026272-A
Country	US
Kind code	B2
Filing date	Oct 30, 2014
Priority date	Nov 12, 2013
Publication date	Jun 27, 2017
Grant date	Jun 27, 2017

Abstract

A method for preparing a reaction product includes: steps (1) and (2). Step (1) is contacting, at a temperature from 200° C. to 1400° C., a first ingredient including a silane of formula H a R b SiX (4-a-b) , where subscript a is an integer from 0 to 4, subscript b is 0 or 1, a quantity (a+b)<4, each R is independently a monovalent organic group, and each X is independently a halogen atom, with the proviso that when the quantity (a+b)<4, then the ingredient further includes H2; with a spinel catalyst including copper; thereby forming a reactant. Step (2) is contacting the reactant with a second ingredient including an organohalide at a temperature from 100° C. to 600° C.; thereby forming the reaction product and a spent reactant. The reaction product is distinct from the silane used in step (1). The method may be used to prepare diorganodihalosilanes from silicon tetrahalides.

First claim

The invention claimed is:

1. A method for preparing a reaction product comprising a halosilane comprises steps (1) and (2), where:
step (1) is contacting, at a temperature from 200° C. to 1400° C., a first ingredient comprising a silane of formula H a R b SiX (4-a-b) , where subscript a is an integer from 0 to 4, subscript b is 0 or 1, a quantity (a+b)≦4, each R is independently a monovalent organic group, and each X is independently a halogen atom; with a spinel catalyst comprising copper; thereby forming a reactant, with the proviso that when the quantity (a+b)<4, then the first ingredient further comprises H 2 ; and
step (2) is contacting the reactant with a second ingredient comprising an organohalide at a temperature from 100° C. to 600° C.; thereby forming the reaction product and a spent reactant; and
where the method optionally further comprises steps (3) and (4), and where
step (3) is contacting, at a temperature from 200° C. to 1400° C., the spent reactant with an additional first ingredient comprising additional silane of formula H a R b SiX (4-a-b) , where subscript a is an integer from 0 to 4, subscript b is 0 or 1, the quantity (a+b)≦4, each R is independently a monovalent organic group, and each X is independently a halogen atom, with the proviso that when the quantity (a+b)<4, then the additional ingredient further comprises H 2 ; thereby re-forming the reactant, and
step (4) is contacting the reactant re-formed in step (3) with an additional second ingredient comprising organohalide at a temperature from 100° C. to 600° C.; thereby forming an additional reaction product and an additional spent reactant, and
where the method optionally further comprises step (5), where step (5) is repeating steps (3) and (4) at least one time; and
where the method optionally further comprises step (6) after any one or more of steps (2) to (5), where step (6) is recovering the halosilane.

2. The method of claim 1 , where the spinel catalyst meets one of conditions (A) to (E), where
Condition (A) is that copper is part of the spinel;
Condition (B) is that copper is part of the spinel and the spinel catalyst further comprises excess support;
Condition (C) is that copper is part of the spinel and the spinel catalyst further comprises a promoter;
Condition (D) is that the spinel catalyst comprises copper supported on a spinel; or
Condition (E) is that the spinel catalyst comprises both copper supported on a spinel and copper forming part of the spinel.

3. The method of claim 1 , where the spinel catalyst comprises one or more of CuAl 2 O 4 or CuFe 2 O 4 , 20% CuAl 2 O 4 , 30% CuAl 2 O 4 , 43.8% CuAl 2 O 4 , 13% CuAl 2 O 4 , Au—Mg—CuAl 2 O 4 , CuO/NiAl 2 O 4 , Cu/CuAl 2 O 4 , Cu/NiAl 2 O 4 , Cu/MgAl 2 O 4 , 30% Cu/10% NiAl 2 O 4 , or 2CuO.Cr 2 O 3 , CuO/CuAl 2 O 4 , 30% Cu/10% CuAl 2 O 4 or 30% Cu/20% CuAl 2 O 4 .

4. The method of claim 1 , where the spinel catalyst comprises a spinel of empirical formula CuM′ 2 O 4 , where M′ is Al, Cr, Fe, Mg, or Ni.

5. The method of claim 1 , where the spinel catalyst is prepared by a method comprising:
i) combining a support and a precursor, thereby forming a combination; and
ii) calcining the combination at a temperature for a time and in an atmosphere sufficient to form the spinel catalyst.

6. The method of claim 5 , further comprising: steps a) and b) before step i) and/or after step ii), where
step a) is combining the support and an additional metal precursor, thereby forming a further combination; and
step b) is calcining the further combination to form the spinel catalyst; wherein the metal in the metal precursor is a metal other than copper.

7. The method of claim 1 , further comprising:
purging and/or treating the spinel catalyst, before contacting the spinel catalyst with the ingredient comprising the silane in step (1); and/or
purging and/or treating the reactant, before contacting the reactant with the organohalide in step (2); and/or
purging and/or treating, the spent reactant before contacting the spent reactant with the additional ingredient in step (3); and/or
purging and/or treating the reactant re-formed in step (3), before the contacting the reactant re-formed in step (3) with the (additional) organohalide in step (4); and/or
purging and/or treating the additional spent reactant.

8. The method of claim 1 , where the silane comprises one or more of a tetrahalosilane of formula SiX 4 , a trihalosilane of formula HSiX 3 , a dihalosilane of formula H 2 SiX 2 , a monohalosilane of formula H 3 SiX, silane of formula SiH 4 , or a combination thereof.

9. The method of claim 1 , where a=0, b=0, and the silane is a tetrahalosilane of formula SiX 4 .

10. The method of claim 1 , where the organohalide has formula RX, where R is alkyl or aryl, and X is Cl.

11. The method of claim 1 , where contacting the reactant with the organohalide in step (2), and optionally step (4), when present, is performed in the absence of H 2 .

12. The method of claim 1 , where the reaction product comprises a halosilane of formula R (4-c) SiX c , where subscript c is 1, 2, 3, or 4.

13. The method of claim 1 , where the reaction product comprises a halosilane of formula R 2 SiX 2 .

14. The method of claim 12 , where R is methyl and X is Cl.

15. The method of claim 1 further comprising using the halosilane as a reactant to make a polyorganosiloxane.

16. The method of claim 1 , where the spinel catalyst is prepared by a method comprising:
i) combining copper oxide and a second metal oxide, where the second metal oxide differs from copper oxide,
ii) calcining the combination to form the spinel catalyst.

17. The method of claim 16 , where step ii) is performed in a reactor, and step (1) is performed in the same reactor.

18. The method of claim 16 , where the second metal oxide is selected from the group consisting of Al 2 O 3 , Cr 2 O 3 , and Fe 2 O 3 .

19. The method of claim 17 , where the second metal oxide is selected from the group consisting of Al 2 O 3 , Cr 2 O 3 , and Fe 2 O 3 .

20. The method of claim 13 , where R is methyl and X is Cl.

Assignees

• Dow Corning

Inventors

• Coppernoll Aaron
• Janmanchi Krishna
• Horner Catharine

Classifications

• B01J23/72

  Copper · CPC title

• C07F7/122

  by reactions involving the formation of Si-C linkages (hydrosilylation reactions C07F7/14; direct synthesis C07F7/16) · CPC title

• B01J37/08

  Heat treatment {(B01J37/0009, B01J37/0018 take precedence)} · CPC title

• B01J23/005

  Spinels · CPC title

• B01J23/8993

  with chromium, molybdenum or tungsten · CPC title