IP Library Granted Patent US 9,120,673
Granted Patent B2
US 9,120,673 · App. 14/344,793 · Granted Sep 1, 2015

Production of trisilylamine from monochlorosilane and ammonia by use of inert solvent

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Quick Facts
Patent No.
US 9,120,673
App. No.
14/344,793
Granted
Sep 1, 2015
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 wherein such a process can be carried out with advantage.

Claims (24)

1. Process for production of trisilylamine in the liquid phase,

which process comprises

initially charging monochlorosilane (A or A′) to a reactor ( 1 ) in the liquid form of a solution in a solvent (H), wherein the solvent is inert with regard to monochlorosilane, ammonia as well as TSA and has a higher boiling point than TSA has, and

passing ammonia (B) into the reactor in the form of a solution in the solvent (H),

performing the reaction in reactor ( 1 ),

subsequently passing the resultant product mixture from reactor ( 1 ) into and through a filter unit ( 2 ) and removing solid ammonium chloride (C) from the product mixture, and

passing the filtrate from the filter unit ( 2 ) into the distillation column ( 3 ),

excess monochlorosilane (A′) being distilled in distillation column ( 3 ) overhead, condensed and fed to reactor ( 1 ) in liquid form under admixture of the solvent, and also

removing gaseous substances (D) from the distillation column ( 3 ) overhead, and

conveying the bottoms (E) into the distillation column ( 4 ),

the product trisilylamine (G) being distilled in the distillation column ( 4 ) overhead and condensed, and

conveying the bottoms (F) into the distillation column ( 5 ),

the solvent (H) being distilled in distillation column ( 5 ) overhead, condensed and returned to the reactor feedstreams (A), (A′), (B) as a solvent, and

exporting higher boilers via the bottoms (I).

2. Process according to claim 1 , characterized in that component (A or A′) is used in a molar stoichiometric excess relative to component (B).

3. Process according to claim 1 , characterized in that the reactor ( 1 ) is filled with the reaction mixture of components (A, A′), (B) and also (H) as solvent up to 99% of the reactor volume to perform the reaction.

4. Process according to claim 1 , characterized in that the reaction in reactor ( 1 ) is carried out at temperature of −60 to +40° C.

5. Process according to claim 1 , characterized in that the process is carried out batchwise or continuously.

6. Process according to claim 1 , wherein the solvent (H) is toluene.

7. Plant for reacting at least the reactants monohalosilane (A, A′) and ammonia (B) with the solvent (H) in the liquid phase to form a product mixture for production of trisilylamine comprising

a reactor ( 1 ) with feeds for the components (A), (A′), (B) and also (H) as solvent and a product mixture outlet opening into a

filter unit ( 2 ) which is connected to reactor ( 1 ) at the downstream end thereof and which in turn is equipped with a solids outlet for component (C) and with a line for conveying the filtrate out of unit ( 2 ) into

a subsequent distillation unit which consists of at least three distillation columns ( 3 ), ( 4 ) and ( 5 ) and the distillation column ( 3 ) is equipped with an outlet overhead for a gaseous stream (D) and with an outlet overhead with a return line for condensed monochlorosilane (A′) into the reactor ( 1 ) under admixture of solvent (H) and also with a line for transferring bottoms (E) from the distillation column ( 3 ) into the subsequent distillation column ( 4 ) to recover trisilylamine (G) and also with a line for transferring bottoms (F) from the distillation column ( 4 ) into the subsequent distillation column ( 5 ) to recover solvent (H) and also export bottoms (I).

8. Plant according to claim 7 , wherein the solvent (H) is toluene.

Assignments (3)
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 Dec 1, 2015
From: EVONIK INDUSTRIES AG
To: EVONIK DEGUSSA GMBH
Reel/Frame 037174/0982 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 22, 2014
From: HOPPE, CARL-FRIEDRICH; RAULEDER, HARTWIG; GOETZ, CHRISTIAN
To: EVONIK INDUSTRIES AG
Reel/Frame 034003/0112 →