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Preparation method and system of trimethylsilylamine

A trisilyl amine, preparation system technology, applied in the direction of chloride preparation, chemical instruments and methods, chemical/physical/physicochemical process of energy application, etc., can solve multi-solid by-product ammonium chloride, synthesis process and Problems such as high device complexity and high separation difficulty achieve the effect of being conducive to large-scale industrial production, low product separation difficulty, and simple process

Active Publication Date: 2021-08-06
ASIA SILICON QINGHAI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The above-mentioned process has problems such as high complexity of synthesis process and device, and more solid by-product ammonium chloride will be generated, resulting in difficult separation.

Method used

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  • Preparation method and system of trimethylsilylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 3

[0050] Embodiment 1 Trisilylamine preparation system

[0051] A preparation system for trisilylamine, such as figure 1 Shown, comprise reactor 1, primary cooler 2, secondary cooler 3, absorption tank 4, drier 5, described reactor 1, primary cooler 2, secondary cooler 3, absorption tank 4, The dryers 5 are connected in sequence; the discharge end of the dryer 5 communicates with the feed end of the reactor 1 .

[0052] Wherein, the reactor 1 is a plasma reactor, which may be any plasma reactor commonly used in the art, such as a DBD reactor, an arc discharge plasma reactor, and the like.

Embodiment 2 3

[0053] The preparation of embodiment 2 trisilylamine

[0054] The preparation system of Example 1 is used to prepare trisilylamine, wherein the reactor 1 is a DBD reactor with a conventional coaxial cylindrical structure in the art, and the surface of the electrode in the reactor is provided with an insulating layer, and the electrode is not directly in contact with the reaction gas. . The surface of the insulating layer on the inner wall of the outer electrode is covered with a barium sulfate layer with a roughness of 0.5 μm as a reflective film layer.

[0055] Will N 2 :H 2 : SiCl 2 h 2 N with a molar ratio of 20:20:1 2 :H 2 : SiClH 3 The mixed gas is introduced into the DBD reactor, the pressure formed by the mixed gas in the reactor is 0.05MPa, the working voltage of the DBD reactor is set to 10KV, and the frequency is 50KHz, so that the mixed gas can fully react in the reaction chamber and control the reaction during the reaction process. The temperature of the no...

Embodiment 3 3

[0060] The preparation of embodiment 3 trisilylamine

[0061] The preparation system of Example 1 is used to prepare trisilylamine, wherein the reactor 1 is a DBD reactor with a conventional coaxial cylindrical structure in the art, and the surface of the electrode in the reactor is provided with an insulating layer, and the electrode is not directly in contact with the reaction gas. . The surface of the insulating layer on the inner wall of the outer electrode is covered with a barium sulfate layer with a roughness of 0.5 μm as a reflective film layer.

[0062] Will N 2 :H 2 : SiCl 2 h 2 N with a molar ratio of 20:20:1 2 :H 2 : SiClH 3 The mixed gas is introduced into the DBD reactor, the pressure formed by the mixed gas in the reactor is 0.05MPa, the working voltage of the DBD reactor is set to 50KV, and the frequency is 50KHz, so that the mixed gas can fully react in the reaction chamber and control the reaction during the reaction process. The temperature of the no...

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Abstract

The invention discloses a preparation method and system of trimethylsilylamine, and the method comprises the following steps: carrying out a reaction on a mixed gas of N2, H2 and SiClxH4-x under the action of an electromagnetic field, wherein x is larger than or equal to 0 and smaller than or equal to 2. According to the method, efficient reaction of non-thermal plasma of nitrogen and hydrogen and chlorosilane is achieved, trimethylsilylamine is successfully prepared under the low-temperature and low-pressure conditions, the conditions are mild, and safety is high; and no solid by-product is produced, the product separation difficulty is low, solid waste treatment is not needed, the process is simple, the operability is high, and large-scale industrial production is facilitated.

Description

technical field [0001] The invention relates to the field of trisilylamine production, in particular to a preparation method and system of trisilylamine. Background technique [0002] Trisilylamine is an important synthetic chemical and an important substance in the semiconductor industry. The existing trimethylsilylamine preparation process usually uses monomeric chlorosilane and ammonia as raw materials under conditions of heating, pressurization and the presence of a catalyst to react the raw materials to generate trimethylsilylamine and by-product ammonium chloride. The purer trisilylamine product is separated by means of a multi-stage rectification device, such as patents CN108586515A and CN105731464A. [0003] The above-mentioned process has problems such as high complexity of synthesis process and device, and more solid by-product ammonium chloride will be generated, resulting in difficult separation. Therefore, the existing technology for producing trisilylamine ne...

Claims

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Application Information

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IPC IPC(8): C01B21/088C01B7/03B01J19/08
CPCC01B21/088C01B7/035B01J19/08
Inventor 张宝顺宗冰王体虎
Owner ASIA SILICON QINGHAI
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