Process for the preparation of trisilylamine from monochlorosilane and ammonia

Patent metadata

Field	Value
Publication number	US-9656869-B2
Application number	US-201214131126-A
Country	US
Kind code	B2
Filing date	May 15, 2012
Priority date	Jul 6, 2011
Publication date	May 23, 2017
Grant date	May 23, 2017

Abstract

The present invention relates to a specific process for producing trisilylamine from monochlorosilane and ammonia in the liquid phase. The invention further relates to a plant in which such a process can be carried out with advantage.

First claim

The invention claimed is:

1. A process for production of trisilylamine, comprising:
charging monochlorosilane as a liquid to a reactor;
passing ammonia into the liquid monochlorosilane in the reactor;
reacting the ammonia and the monochlorosilane in a liquid phase in the reactor to obtain a reaction mixture comprising liquid monochlorosilane, liquid trisilylamine and solid ammonium chloride;
transferring the reaction mixture from the reactor into and through a filter unit;
collecting the solid ammonium chloride on the filter unit to obtain a filtrate of the liquid reaction mixture comprising monochlorosilane and trisilylamine;
passing the filtrate from the filter unit into a first distillation column;
distilling the monochlorosilane in the distillation column overhead, condensing the monochlorosilane and feeding the condensed monochlorosilane to the reactor; and
removing gaseous substances from the first distillation column overhead to obtain a first distillation bottoms comprising trisilylamine;
conveying the first bottoms into a second distillation column;
distilling the trisilylamine from the first bottoms in the second distillation column overhead and condensing the distillate to obtain a condensate consisting of trisilylamine; and
removing higher boilers from the system via second bottoms remaining in the second column;
wherein the process is a continuous method.

2. The process according to claim 1 , wherein
the monochlorosilane is in a molar excess relative to the ammonia.

3. The process according to claim 1 , wherein
the reactor is filled with the reaction mixture of the monochlorosilane and the ammonia up to 99% of a reactor volume to perform the reaction.

4. The process according to claim 1 , wherein
the reaction in the reactor is carried out at temperature of from −60 to +40 ° C.

5. The process for production of trisilyla mine of claim 1 , further comprising purging the reactor, filter unit and distillation columns with a protective gas and carrying out the process under a protective gas.

6. The process of claim 5 , wherein the protective gas is nitrogen or a noble gas.

7. The process for production of trisilylamine of claim 1 wherein the reaction of the monochlorosilane and ammonia is conducted in the absence of oxygen and moisture.

Assignees

• Hoppe Carl-Friedrich
• Rauleder Hartwig
• Lunt-Rieg Ingrid
• Goetz Christian
• Evonik Degussa Gmbh

Inventors

• Hoppe Carl-Friedrich
• Rauleder Hartwig
• Lunt-Rieg Ingrid
• Goetz Christian

Classifications

• B01J19/24

  Stationary reactors without moving elements inside (B01J19/08, B01J19/26 take precedence; with stationary particles B01J8/02) · CPC title

• C01B21/087 Primary

  containing one or more hydrogen atoms · CPC title

• C01C1/164

  Ammonium chloride · CPC title

• C01B33/043

  Monosilane · CPC title

• B01J8/00

  Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes · CPC title