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

Patent metadata

Field	Value
Publication number	US-9359205-B2
Application number	US-201514724114-A
Country	US
Kind code	B2
Filing date	May 28, 2015
Priority date	Dec 16, 2011
Publication date	Jun 7, 2016
Grant date	Jun 7, 2016

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.

First claim

The invention claimed is:

1. A plant for reacting at least monohalosilane (A) and/or recycled monosilane (A′), and ammonia (B) in a solvent (H) in the liquid phase to form a product mixture for production of trisilylamine, said plant comprising:
a) a stirred reactor equipped with liquid feed lines for the components (A) as solution in (H), and (A′) as solution in (H), a feed line for (B), optionally as a solution in (H) and a bottom liquid product mixture outlet opening into
b) a filter unit which is connected to said reactor at the downstream end thereof and which in turn is equipped with a solids outlet for ammonium chloride (C) and with a line for conveying a filtrate out of said filter unit into
c) a subsequent distillation unit which comprises at least three distillation columns and a first distillation column of said at least three distillation columns is equipped with an outlet overhead for a gaseous stream (D) and with an outlet overhead with a return line for condensed recycled monochlorosilane (A′) into the reactor under admixture of solvent (H) and also with a line for transferring bottoms (E) from the first distillation column of said at least three distillation columns into a subsequent second distillation column of said at least three distillation columns to recover trisilylamine (G) and also with a line for transferring bottoms (F) from the second distillation column of said at least three distillation columns into a subsequent third distillation column of said at least three distillation columns to recover solvent (H) and also export bottoms (I);
wherein the solvent (H) is toluene; and
wherein component (A) and/or (A′) is used in a molar stoichiometric excess relative to component (B).

2. The plant according to claim 1 , wherein the reactor is filled with the reaction mixture of components (A) and/or (A′), (B) and (H) up to 99% of the reactor volume to perform the reaction.

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

4. The plant according to claim 1 , wherein the process is carried out batchwise.

5. The plant according to claim 1 , wherein the process is carried out continuously.

6. The plant according to claim 1 , which is dried and purged with protective gas before a first filling operation with said reactants and/or said solvent.

7. The plant according to claim 1 , wherein a plant component which comes into contact with any reaction component in said process comprises stainless steel.

8. The plant according to claim 1 , wherein a plant component which comes into contact with any reaction component in said process is coolable and/or heatable in a controlled manner.

9. A plant for reacting at least monohalosilane (A) and/or recycled monosilane (A′), and ammonia (B) in a solvent (H) in the liquid phase to form a product mixture for production of trisilylamine, said plant comprising:
a) a stirred reactor equipped with liquid feed lines for the components (A) as solution in (H), and (A′) as solution in (H), a feed line for (B), optionally as a solution in (H) and a bottom liquid product mixture outlet opening into
b) a filter unit which is connected to said reactor at the downstream
end thereof and which in turn is equipped with a solids outlet for ammonium chloride (C) and with a line for conveying a filtrate out of said filter unit into
c) a subsequent distillation unit which comprises at least three distillation columns and a first distillation column of said at least three distillation columns is equipped with an outlet overhead for a gaseous stream (D) and with an outlet overhead with a return line for condensed recycled monochlorosilane (A′) into the reactor under admixture of solvent (H) and also with a line for transferring bottoms (E) from the first distillation column of said at least three distillation columns into a subsequent second distillation column of said at least three distillation columns to recover trisilylamine (G) and also with a line for transferring bottoms (F) from the second distillation column of said at least three distillation columns into a subsequent third distillation column of said at least three distillation columns to recover solvent (H) and also export bottoms (I);
wherein said solvent is toluene;
wherein a solvent-to-monochlorosilane ratio between the volumes of the liquids is in the range from 30:1 to 1:1;
wherein the monochlorosilane is present in a molar stoichiometric excess to the ammonia;
wherein the trisilylamine is formed at a temperature of −60 to +40° C.

Assignees

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

Inventors

• Hoppe Carl-Friedrich
• Rauleder Hartwig
• Goetz Christian

Classifications

• B01J2219/00002

  Chemical plants · CPC title

• C01B21/087 Primary

  containing one or more hydrogen atoms · CPC title

• C01B33/00

  Silicon; Compounds thereof ({C01B6/00,} C01B21/00, C01B23/00 take precedence; persilicates C01B15/14; carbides C01B32/956) · CPC title

• B01D3/143

  by two or more of a fractionation, separation or rectification step · CPC title

• B01D3/009

  in combination with chemical reactions · CPC title