Novel method for preparing trisilylamine

A new type of trisilylamine technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of reducing the yield of trisilylamine, and achieve the goal of reducing production cost, improving utilization rate, and increasing production Effect

Active Publication Date: 2022-02-25
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Trisilylamine TSA will produce polysilazane as a by-product during the synthesis process, and when the ammonia gas is excessive, the by-products will be more, reducing the trisilylamine Yield of
Providing a reaction mixture of trisilylamine and monochlorosilane to a reactor under solvent-free conditions, wherein the reaction mixture is at a temperature and pressure sufficient to provide trisilylamine in the liquid phase to produce highly pure TSA, but this method also produces small amounts of polysilazane

Method used

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  • Novel method for preparing trisilylamine
  • Novel method for preparing trisilylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 5g of polysilazane and n-hexane solvent were mixed into a 5wt% mixed solution, transferred to a high-temperature and high-pressure reactor, and the solvent was distilled off under reduced pressure under an inert atmosphere of nitrogen, and then heated to 350°C for pyrolysis, and The pyrolyzed gas was condensed and recovered in the flask, and the collected liquid was heated and distilled to obtain the TSA product, which was detected by gas chromatography. The crude product of TSA was 1.55 g, the product purity was 97.5%, and the product yield was 31%.

Embodiment 2

[0037] 5g of polysilazane and n-hexane solvent were proportioned into a mixed solution of 5wt%, transferred to a high-temperature and high-pressure reactor, and the solvent was distilled off under reduced pressure under an inert atmosphere of nitrogen, and then heated to 400°C for pyrolysis, and The pyrolyzed gas was condensed and recovered in the flask, and the collected liquid was heated and distilled to obtain the TSA product, which was detected by gas chromatography. The crude product of TSA was 1.95 g, the product purity was 97.4%, and the product yield was 34%.

Embodiment 3

[0039] 5g of polysilazane and n-hexane solvent were mixed into a 5wt% mixed solution, transferred to a high-temperature and high-pressure reactor, and the solvent was distilled off under reduced pressure under an inert atmosphere of nitrogen, and then heated to 450°C for pyrolysis, and The pyrolyzed gas was condensed and recovered in the flask, and the collected liquid was heated and distilled to obtain the TSA product, and detected by gas chromatography, the crude product of TSA was 1.70 g, the product purity was 97.7%, and the product yield was 39%.

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Abstract

The invention relates to the technical field of fine chemical engineering, and especially relates to a novel method for preparing trisilylamine. A solid residue ammonium chloride obtained after TSA reaction is washed with normal hexane in a certain proportion and distilled to obtain a byproduct polysilazane, the byproduct polysilazane is dissolved with the solvent containing a synergist and is pyrolyzed to obtain a trisilylamine crude product, so the yield is high, meanwhile, the raw material utilization rate and the product yield are increased, solid ammonium chloride is harmlessly treated, and the production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, especially a novel method for preparing trisilylamine. Background technique [0002] Trisilylamine TSA will produce by-product polysilazane during the synthesis process, and when the ammonia gas is excessive, there will be more by-products, which will reduce the yield of trisilylamine. However, polysilazane residues in solid ammonium chloride are also dangerous and must be disposed of in time. When performed on an industrial scale, the gas-phase reaction produces TSA in high yield and purity while producing large quantities of solid by-products. And it is very time-consuming to remove these solid by-products from the reactor, and it is very likely to prolong the shutdown time of the reactor, thereby affecting the production cost of TSA. [0003] Richard L. Wells and Riley Schaeffer described that after hydrogen chloride and ammonia were heated to room temperature at -196°C, in addition t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/00
CPCC01B33/00
Inventor 徐琴琪熊文辉陈刚李军张广第朱智敏
Owner ZHEJIANG BRITECH CO LTD
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