IP Library Granted Patent US 9,463,978
Granted Patent B2
US 9,463,978 · App. 15/013,224 · Granted Oct 11, 2016

Process for making trisilylamine

Inventors: Rajiv Krishan Agarwal (Malvern, PA); Sai-Hong Andrew Lo (Allentown, PA); Howard Paul Withers, Jr. (Breinigsville, PA); Joseph T. Sluzevich (Frackville, PA); James Joseph Hart (Fogelsville, PA)
Assignee: Air Products and Chemicals, Inc.
C01B21/087B01J8/0015B01J8/02B01J8/10B01J8/24B01J2208/00761B01J2208/00823
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Quick Facts
Patent No.
US 9,463,978
App. No.
15/013,224
Granted
Oct 11, 2016
Kind
B2
Abstract

The method described herein provides a method for preparing trisilylamine. In one aspect, the method comprises: providing a reaction mixture of trisilylamine and monochlorosilane into a reactor wherein the reaction mixture is at a temperature and pressure sufficient to provide trisilylamine in a liquid phase wherein the reaction mixture is substantially free of an added solvent; contacting the reaction mixture with ammonia to provide a crude mixture comprising trisilylamine and an ammonium chloride solid wherein monochlorosilane is in stoichiometric excess in relation to ammonia; purifiying the crude mixture to provide trisilylamine wherein the trisilyamine is produced at purity level of 90% or greater; and optionally removing the ammonium chloride solid from the reactor.

Claims (26)

1. A system for preparing trisilylamine, the system comprising:

a reactor comprising a reaction mixture of trisilylamine which is in communication with monochlorosilane and ammonia and wherein the density of trisilyamine in the reactor ranges from about 1.5 to about 100 grams/liter which react with the reaction mixture to provide a crude mixture comprising monochlorosilane and dichlorosilane in a liquid phase and an ammonium chloride solid wherein the reactor is substantially free of an added solvent;

a vacuum conveyor for removing the ammonium chloride solid from the reactor; and

a distillation column wherein the crude mixture is transferred from the reactor to the distillation column and purified in the distillation column to provide trisilylamine at a purity level of 90% or greater.

2. The system of claim 1 wherein the reactor is selected from a batch reactor or a continuous stirred tank reactor.

3. The system of claim 2 wherein the reactor comprises the batch reactor.

4. The system of claim 3 wherein the monochlorosilane is added to the reactor before the ammonia is added to the reactor.

5. The system of claim 1 wherein the density of trisilylamine in the reactor comprises about 1.7 g/I or greater.

6. The system of claim 2 wherein the reactor comprises the continuous stirred tank reactor.

7. The system of claim 1 wherein the trisilylamine is added as a solvent in the reactor.

8. The system of claim 1 wherein the vacuum conveyor comprises in situ vacuum removal.

9. The system of claim 1 wherein an inert gas is used to fluidize the ammonium chloride solids in the reactor to provide fluidized solids.

10. The system of claim 9 wherein the fluidized solids are carried out to a venturi vacuum system via the inert gas for collection and disposal.

11. The system of claim 1 wherein a temperature in the reactor ranges from 20 to 120° C.

12. The system of claim 1 wherein a pressure in the reactor ranges from 0.1 to 115 psia.

13. The system of claim 1 further comprising a collector which is communication with the reactor to collect the crude mixture from the reactor.

14. The system of claim 1 wherein the trisilylamine is purified in the distillation column to a purity level of 99% or greater.

15. The system of claim 1 wherein polysilazanes are removed from the reactor by evaporation and collection.

16. The system of claim 1 wherein the reaction mixture comprises up to 30% by weight stoichiometric excess monochlorosilane relative to ammonia.

17. The system of claim 1 wherein the reaction mixture comprises from about 3%® to about 5% by weight stoichiometric excess monochlorosilane relative to ammonia.

18. A method for preparing trisilylamine, the method comprising:

providing a reaction mixture of trisilylamine and monochlorosilane into a reactor wherein the reaction mixture is at a temperature and pressure sufficient to provide trisilylamine in a liquid phase wherein the reaction mixture is substantially free of an added solvent and wherein the trisilyamine in the reactor acts as solvent in the reaction mixture;

contacting the reaction mixture with ammonia to provide a crude mixture comprising trisilylamine and an ammonium chloride solid wherein monochlorosilane is in stoichiometric excess in relation to ammonia; and

purifiying the crude mixture to provide trisilylamine wherein the trisilyamine is produced at purity level of 90% or greater.

19. The method of claim 18 wherein the method further comprises removing the ammonium chloride solid from the reactor.

20. The method of claim 18 wherein the reactor is selected from a batch reactor or a continuous stirred tank reactor.

Assignments (4)
RELEASE OF SECURITY INTEREST Recorded Oct 7, 2019
From: CITIBANK, N.A., AS AGENT
To: VERSUM MATERIALS US, LLC
Reel/Frame 050647/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 20, 2017
From: AIR PRODUCTS AND CHEMICALS, INC.
To: VERSUM MATERIALS US, LLC
Reel/Frame 041772/0733 →
PATENT SECURITY AGREEMENT Recorded Oct 27, 2016
From: VERSUM MATERIALS US, LLC
To: CITIBANK, N.A., AS COLLATERAL AGENT
Reel/Frame 040503/0442 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 29, 2016
From: AGARWAL, RAJIV KRISHAN; LO, SAI-HONG ANDREW; WITHERS, HOWARD PAUL, JR.; SLUZEVICH, JOSEPH T.; HART, JAMES JOSEPH
To: AIR PRODUCTS AND CHEMICALS, INC.
Reel/Frame 038119/0714 →
Continuity (3)
Division 14284983 · May 22, 2014
Provisional Application 61840940 · Jun 28, 2013
Related Publication 20160145102A1 · May 26, 2016