IP Library Granted Patent US 8,834,825
Granted Patent B2
US 8,834,825 · App. 13/528,386 · Granted Sep 16, 2014

Processes for producing silane in a bubble column

Inventors: Baisheng Zou (Pearland, TX); Puneet Gupta (Houston, TX)
Assignee: SunEdison, Inc.
C01B33/043B01J10/002B01J2219/00164B01J2219/00186B01J2219/00202B01J19/0066B01J2219/00063B01J2219/00094B01J19/006B01J2219/00777B01J19/18B01J2219/00231B01J19/0013B01J2219/002B01J2219/00159B01J2219/00213
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Quick Facts
Patent No.
US 8,834,825
App. No.
13/528,386
Granted
Sep 16, 2014
Kind
B2
Abstract

Methods for producing silane by reacting a hydride and a halosilane are disclosed. Some embodiments involve use of a column which is not mechanically agitated and in which reactants may be introduced in a counter-current arrangement. Some embodiments involve use of a baffled column which has multiple reaction zones.

Claims (58)

1. A process for preparing silane in a columnar reaction vessel, the vessel comprising a lower inlet, a lower outlet, an upper inlet and an upper outlet and having a reaction mixture therein, the process comprising:

introducing a hydride feed comprising a hydride into the upper inlet of the reaction vessel;

introducing a feed gas comprising a halosilane into the lower inlet of the reaction vessel to bubble the feed gas through the reaction mixture, the hydride reacting with the halosilane to produce silane and a halide salt;

discharging a product gas comprising silane from the upper outlet; and

discharging an effluent comprising the halide salt from the lower outlet, the reaction vessel not being mechanically agitated while reacting the hydride with halosilane.

2. The process as set forth in claim 1 wherein the hydride is selected from the group consisting of alkali or alkaline earth metal hydrides, alkali or alkaline earth metal salts of aluminum tetrahydride, and combinations thereof.

3. The process as set forth in claim 1 wherein the halosilane is selected from the group consisting of silicon tetrahalide, trihalosilane, dihalosilane, monohalosilane and combinations thereof.

4. The process as set forth in claim 1 wherein the hydride is an alkali or alkaline earth metal salt of aluminum tetrahydride, the halosilane is silicon tetrahalide and the halide salt is an alkali or alkaline earth-metal salt of aluminum tetrahalide.

5. The process as set forth in claim 1 wherein the hydride is the sodium salt of aluminum tetrahydride, the halosilane is silicon tetrafluoride and the halide salt is the sodium salt of aluminum tetrafluoride.

6. The process as set forth in claim 1 wherein the discharged effluent is a slurry.

7. The process as set forth in claim 1 wherein the hydride feed and feed gas are introduced continuously into the reaction vessel and the product gas and effluent are discharged continuously from the reaction vessel.

8. The process as set forth in claim 1 wherein the hydride feed is a solution that comprises a solvent and a hydride.

9. The process as set forth in claim 8 wherein the solvent is selected from the group consisting of polyethers, hydrocarbons and mixtures thereof.

10. The process as set forth in claim 9 wherein the polyethers are selected from the group consisting of diglyme, monoglyme, dioxane and mixtures thereof and the hydrocarbons are selected from toluene, pentane and mixtures thereof.

11. The process as set forth in claim 1 wherein the hydride feed comprises solid hydride.

12. The process as set forth in claim 1 wherein the conversion of the hydride is at least about 80%.

13. The process as set forth in claim 1 wherein the conversion of the hydride is at least about 80%.

14. The process as set forth in claim 1 wherein the conversion of the halosilane is at least about 80%.

15. The process as set forth in claim 1 wherein the conversion of the halosilane is at least about 80%.

16. A process for preparing silane in a reaction vessel having a reaction mixture therein, the vessel having one or more baffles, the baffles creating two or more reaction zones connected in series, the process comprising:

introducing a hydride feed comprising a hydride into the reaction vessel;

introducing a feed gas comprising a halosilane into the reaction vessel to bubble the feed gas through the reaction mixture, the hydride reacting with the halosilane to produce silane and a halide salt;

discharging a product gas comprising silane from the reaction vessel;

discharging an effluent comprising the halide salt from the reaction vessel; and

agitating the reaction mixture.

17. The process as set forth in claim 16 wherein a mechanical agitator is disposed within the reaction vessel.

18. The process as set forth in claim 17 wherein the agitator agitates the contents of one or more reaction zones of the vessel, the reaction between the hydride and halosilane in each agitated reaction zone being performed under conditions that approach a continuously ideally-stirred tank reactor.

19. The process as set forth in claim 17 wherein the mechanical agitator is an impeller having one or more blades disposed within each agitated reaction zone.

20. The process as set forth in claim 17 wherein each reaction zone of the reaction vessel is agitated.

21. The process as set forth in claim 16 wherein the vessel comprises an upper inlet in which the hydride feed is introduced, a lower inlet in which the feed gas is introduced, an upper outlet from which the product gas is discharged and a lower outlet from which the effluent is discharged.

22. The process as set forth in claim 16 wherein the hydride feed and feed gas are introduced continuously into the reaction vessel and the product gas and effluent are discharged continuously from the reaction vessel.

23. The process as set forth in claim 16 wherein the hydride feed is a solution that comprises a solvent and a hydride.

24. The process as set forth in claim 23 wherein solvent is selected from the group consisting of polyethers, hydrocarbons and mixtures thereof.

25. The process as set forth in claim 24 wherein the polyethers are selected from the group consisting of diglyme, monoglyme, dioxane and mixtures thereof and the hydrocarbons are selected from toluene, pentane and mixtures thereof.

26. The process as set forth in claim 16 wherein the hydride feed comprises solid hydride.

27. The process as set forth in claim 16 wherein the reaction mixture is cooled in at least one of the reaction zones.

28. The process as set forth in claim 16 wherein the reaction vessel includes a baffle which defines a lower reaction zone and an upper reaction zone.

29. The process as set forth in claim 28 wherein the reaction mixture in the upper reaction zone is cooled.

30. The process as set forth in claim 29 wherein the reaction mixture in the lower reaction zone is not cooled.

31. The process as set forth in claim 16 wherein the reaction vessel includes two baffles which define a lower reaction zone, an intermediate reaction zone and an upper reaction zone.

32. The process as set forth in claim 31 wherein the reaction mixtures in the upper reaction zone is cooled.

33. The process as set forth in claim 32 wherein the reaction mixture in the intermediate reaction zone is cooled.

34. The process as set forth in claim 33 wherein the reaction mixture in the lower reaction zone is not cooled.

35. The process as set forth in claim 16 wherein the reaction vessel is cylindrical and the baffles are annular.

36. The process as set forth in claim 16 wherein the conversion of the hydride is at least about 80%.

37. The process as set forth in claim 16 wherein the conversion of the hydride is at least about 99%.

38. The process as set forth in claim 16 wherein the conversion of halosilane is at least about 80%.

39. The process as set forth in claim 16 wherein the conversion of halosilane is at least about 99%.

40. The process as set forth in claim 16 wherein the reaction mixture is agitated by gas-phase bubble action.

41. The process as set forth in claim 16 wherein the hydride is selected from the group consisting of alkali or alkaline earth metal hydrides, alkali or alkaline earth metal salts of aluminum tetrahydride, and combinations thereof.

42. The process as set forth in claim 16 wherein the halosilane is selected from the group consisting of silicon tetrahalide, trihalosilane, dihalosilane, monohalosilane and combination thereof.

43. The process as set forth in claim 16 wherein the hydride is an alkali or alkaline earth metal salts of aluminum tetrahydride, the halosilane is silicon tetrahalide and the halide salt is an alkali or alkaline earth-metal salt of aluminum tetrahalide.

44. The process as set forth in claim 16 wherein the hydride is the sodium salt of aluminum tetrahydride, the halosilane is silicon tetrafluoride and the halide salt is the sodium salt of aluminum tetrafluoride.

45. The process as set forth in claim 16 wherein the discharged effluent is a slurry.

46. The process as set forth in claim 16 wherein the temperature of the reaction mixture within one of the reaction zones is monitored to control the flow rate of at least one of the hydride feed and feed gas.

47. The process as set forth in claim 46 wherein the temperature is compared to a temperature, T 100 , at which 100% conversion is achieved based on the respective reactant flow rates.

48. The process as set forth in claim 16 wherein the difference in temperature between two reaction zones is monitored to control the flow rate of at least one of the hydride feed and feed gas.

49. The process as set forth in claim 48 wherein the temperature difference is compared to a temperature difference, T Δ , at which 100% conversion is achieved based on the respective reactant flow rates.

Assignments (10)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 27, 2017
From: SUNEDISON, INC.; SUNEDISON PRODUCTS SINGAPORE PTE. LTD.; MEMC PASADENA, INC.; SOLAICX
To: CORNER STAR LIMITED
Reel/Frame 042351/0659 →
PATENT SECURITY AGREEMENT Recorded Apr 28, 2016
From: SUNEDISON, INC.
To: DEUTSCHE BANK AG NEW YORK BRANCH, AS ADMINISTRATIVE AGENT
Reel/Frame 038557/0472 →
RELEASE OF SECURITY INTEREST Recorded Jan 13, 2016
From: GOLDMAN SACHS BANK USA, AS ADMINISTRATIVE AGENT
To: SUNEDISON, INC.; SUN EDISON LLC; SOLAICX; NVT, LLC
Reel/Frame 037508/0884 →
SECURITY INTEREST Recorded Jan 13, 2016
From: SUNEDISON, INC.; SUN EDISON LLC; SOLAICX; NVT, LLC
To: WILMINGTON TRUST, NATIONAL ASSOCIATION, SOLELY IN ITS CAPACITY AS COLLATERAL TRUSTEE
Reel/Frame 037508/0606 →
SECURITY INTEREST Recorded Aug 11, 2015
From: SUNEDISON, INC.; SUN EDISON LLC; SOLAICX; NVT, LLC
To: GOLDMAN SACHS BANK USA, AS ADMINISTRATIVE AGENT
Reel/Frame 036329/0470 →
CHANGE OF NAME Recorded Aug 8, 2014
From: MEMC ELECTRONIC MATERIALS, INC.
To: SUNEDISON, INC
Reel/Frame 033501/0530 →
RELEASE OF SECURITY INTEREST Recorded Mar 3, 2014
From: DEUTSCHE BANK AG NEW YORK BRANCH
To: NVT, LLC; SUN EDISON LLC; SOLAICX; SUNEDISON, INC.
Reel/Frame 032382/0724 →
SECURITY AGREEMENT Recorded Feb 28, 2014
From: SUNEDISON, INC.; SUN EDISON LLC; SOLAICX; NVT, LLC; ENFLEX CORPORATION
To: WELLS FARGO BANK, NATIONAL ASSOCIATION, AS ADMINISTRATIVE AGENT
Reel/Frame 032372/0610 →
SECURITY AGREEMENT Recorded Jan 30, 2014
From: SUNEDISON, INC.; SOLAICX; SUN EDISON, LLC; NVT, LLC
To: DEUTSCHE BANK AG NEW YORK BRANCH
Reel/Frame 032177/0359 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 10, 2012
From: ZOU, BAISHENG; GUPTA, PUNEET
To: MEMC ELECTRONIC MATERIALS, INC.
Reel/Frame 028519/0877 →
Continuity (2)
Provisional Application 61502145 · Jun 28, 2011
Related Publication 20130004405A1 · Jan 3, 2013