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Method for preparing trisilylamine at ultralow temperature

A technology of trisilylamine and ultra-low temperature, applied in the direction of nitrogen and non-metallic compounds, can solve the problems of difficult to complete the reaction, consume a lot of energy, and low yield, and achieve large market value, low cost, and high degree of raw material reaction Effect

Active Publication Date: 2022-01-11
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN103619429A discloses a method for preparing trisilylamine from monochlorosilane and ammonia. The reaction uses MCS directly as a solvent (directly introducing ammonia gas into the liquid of monochlorosilane), and the temperature is -60-40°C. After the reaction is finished, it is also necessary to distill the excess MCS and condense it back to the reactor. The method can be carried out in batches or continuously, and it needs to consume a lot of energy
In actual situations, the solid ammonium chloride produced by the reaction will quickly occupy the entire reactor, making it difficult to carry out the reaction completely, or the yield is very low. The full text does not mention the relevant matters of the yield, and there is no arbitrary ratio of TSA and MCS directly as a reaction solvent

Method used

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  • Method for preparing trisilylamine at ultralow temperature
  • Method for preparing trisilylamine at ultralow temperature
  • Method for preparing trisilylamine at ultralow temperature

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Slowly inject MCS gas into an ultra-low temperature reaction vessel equipped with a mechanical stirrer, then add dropwise liquefied ammonia, liquefied MCS and NH 3 The reaction is carried out at a molar ratio close to 1:1.2, the reaction generates a large amount of ammonium chloride solids, the solids are removed by filtration, the mother liquor is reintroduced into the ultra-low temperature reaction vessel, ammonia gas is added again, filtered again, and the mother liquor is introduced into the reaction vessel again, This cycle is repeated 5 times. When the online GC detects that there is only a small amount of MCS, the metal ion permeation membrane filtration is carried out, and the filtrate is directly introduced into the rectification device for purification.

[0040] The low temperature in the ultra-low temperature reaction is -65°C;

[0041] The amine source is added in the form of gaseous bubbling after mixing and diluting nitrogen (10%) with anhydrous ammonia; ...

Embodiment 2

[0053]The MCS gas is slowly introduced into the ultra-low temperature reaction vessel equipped with a mechanical stirrer, and then the liquefied ammonia gas is added dropwise. The liquefied MCS and NH3 react at a molar ratio close to 1:1.3, and the reaction generates a large amount of ammonium chloride solid. Filter to remove solids, re-introduce the mother liquor into the ultra-low temperature reaction vessel, add ammonia gas again, filter again, and guide the mother liquor into the reaction vessel again, and cycle like this for 5 times. When the online GC detects that there is only a small amount of MCS left, the metal ion is adsorbed. Osmotic membrane filtration, the filtrate is directly introduced into the rectification device for purification.

[0054] The low temperature in the ultra-low temperature reaction is -65°C;

[0055] The amine source is added in the form of gaseous bubbling after mixing and diluting nitrogen (50%) with anhydrous ammonia;

[0056] The membrane ...

Embodiment 3

[0067] The MCS gas is slowly introduced into the ultra-low temperature reaction vessel equipped with a mechanical stirrer, and then the liquefied ammonia gas is added dropwise. The liquefied MCS and NH3 react at a molar ratio close to 1:1.4, and the reaction generates a large amount of ammonium chloride solid. Filter to remove solids, re-introduce the mother liquor into the ultra-low temperature reaction vessel, add ammonia gas again, filter again, and guide the mother liquor into the reaction vessel again, and cycle like this for 5 times. When the online GC detects that there is only a small amount of MCS left, the metal ion is adsorbed. Osmotic membrane filtration, the filtrate is directly introduced into the rectification device for purification.

[0068] The low temperature in the ultra-low temperature reaction is -75°C;

[0069] The added amine source can be mixed and diluted with nitrogen (90%) and anhydrous ammonia in gaseous bubbling form;

[0070] The membrane filtra...

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Abstract

The invention relates to the technical field of trisilylamine preparation, in particular to a method for preparing trisilylamine at an ultralow temperature. According to the method for preparing the trisilylamine at the ultralow temperature without participation of the solvent, by-products generated in the reaction can be easily removed through filtration of a metal ion adsorption permeable membrane, the GC purity of the trisilylamine finally obtained through the reaction reaches 99.5%, the yield reaches 85% or above (based on ammonia gas), and the purity of metal ions contained in the product reaches 6N level; and the device is simple and convenient, the raw material reaction degree is high, the cost is lower, the market value is great, and the industrial production benefit is better.

Description

technical field [0001] The invention relates to the technical field of trisilylamine preparation, in particular to a method for preparing trisilylamine at ultra-low temperature. Background technique [0002] A popular precursor trimethylsilylamine TSA in the field of semiconductor processing, the increasing market demand, urgently needs to find an efficient preparation method in industry. They are currently classified by their reaction modes: currently only gas-gas reaction, gas-liquid reaction or liquid-liquid reaction. [0003] Most of the reactions disclosed in existing patents are usually a single solvent or a mixed solvent system, and now there are also reactions that disclose a solvent-free system, and the reaction purification is easier. The details are as follows: [0004] Patent CN103619429A discloses a method for preparing trisilylamine from monochlorosilane and ammonia. The reaction uses MCS directly as a solvent (directly introducing ammonia gas into the liquid ...

Claims

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Application Information

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IPC IPC(8): C01B21/087
CPCC01B21/087C01P2006/80
Inventor 熊文辉徐琴琪陈刚李军张广第贺辉龙张晓东李平
Owner ZHEJIANG BRITECH CO LTD
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