Process for making trisilylamine

Patent metadata

Field	Value
Publication number	US-2016145102-A1
Application number	US-201615013224-A
Country	US
Kind code	A1
Filing date	Feb 2, 2016
Priority date	Jun 28, 2013
Publication date	May 26, 2016
Grant date	—

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.

First claim

1 - 20 . (canceled)

21 . 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.

22 . The system of claim 21 wherein the reactor is selected from a batch reactor or a continuous stirred tank reactor.

23 . The system of claim 22 wherein the reactor comprises the batch reactor.

24 . The system of claim 23 wherein the monochlorosilane is added to the reactor before the ammonia is added to the reactor.

25 . The system of claim 21 wherein the density of trisilylamine in the reactor comprises about 1.7 g/l or greater.

26 . The system of claim 22 wherein the reactor comprises the continuous stirred tank reactor.

27 . The system of claim 27 wherein the trisilylamine is added as a solvent in the reactor.

28 . The system of claim 21 wherein the vacuum conveyor comprises in situ vacuum removal.

29 . The system of claim 29 wherein an inert gas is used to fluidize the ammonium chloride solids in the reactor to provide fluidized solids.

30 . The system of claim 30 wherein the fluidized solids are carried out to a venturi vacuum system via the inert gas for collection and disposal.

31 . The system of claim 21 wherein a temperature in the reactor ranges from 20 to 120 ° C.

32 . The system of claim 21 wherein a pressure in the reactor ranges from 0.1 to 115 psia.

33 . The system of claim 21 further comprising a collector which is communication with the reactor to collect the crude mixture from the reactor.

34 . The system of claim 21 wherein the trisilylamine is purified in the distillation column to a purity level of 99% or greater.

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

36 . The system of claim 21 wherein the reaction mixture comprises up to 30% by weight stoichiometric excess monochlorosilane relative to ammonia.

37 . The system of claim 21 wherein the reaction mixture comprises from about 3% to about 5% by weight stoichiometric excess monochlorosilane relative to ammonia.

38 . 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.

39 . The method of claim 38 wherein the method further comprises removing the ammonium chloride solid from the reactor.

40 . The method of claim 38 wherein the reactor is selected from a batch reactor or a continuous stirred tank reactor.

Assignees

• Air Prod & Chem

Inventors

• Agarwal Rajiv Krishan
• Lo Sai-Hong Andrew
• Withers Jr Howard Paul
• Sluzevich Joseph T
• Hart James Joseph

Classifications

• B01J2208/00761

  Discharging · CPC title

• B01J8/02

  with stationary particles, e.g. in fixed beds · CPC title

• B01J8/10

  moved by stirrers or by rotary drums or rotary receptacles {or endless belts} · CPC title

• B01J8/0015

  Feeding of the particles in the reactor; Evacuation of the particles out of the reactor · CPC title

• B01J8/24

  according to "fluidised-bed" technique (B01J8/20 takes precedence) · CPC title