IP Library Granted Patent US 9,656,869
Granted Patent B2
US 9,656,869 · App. 14/131,126 · Granted May 23, 2017

Process for the preparation of trisilylamine from monochlorosilane and ammonia

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Quick Facts
Patent No.
US 9,656,869
App. No.
14/131,126
Granted
May 23, 2017
Kind
B2
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.

Claims (22)

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.

Assignments (2)
CHANGE OF NAME Recorded Jan 31, 2020
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051765/0166 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 6, 2014
From: HOPPE, CARL-FRIEDRICH; RAULEDER, HARTWIG; LUNT-RIEG, INGRID; GOETZ, CHRISTIAN
To: EVONIK DEGUSSA GMBH
Reel/Frame 031898/0804 →