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A kind of synthetic method of trisilylamine

A technology of trisilyl amine and synthesis method, which is applied in the directions of silicon organic compounds, chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, etc. problems such as normal operation to achieve high-purity results

Active Publication Date: 2020-09-11
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] ‍‍Existing patents and literature technologies have shortcomings: or use a tubular reactor, the reaction efficiency is low, and the operation is difficult; or use a tank reactor, the reaction is difficult to control, and the carbon number distribution of the product is too wide; it will cause bed Layer resistance and other shortcomings affect the normal operation of industrial devices

Method used

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  • A kind of synthetic method of trisilylamine

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Embodiment 1

[0024] ‍A synthetic method for trisilylamine, comprising the following steps:

[0025] 1) A method for synthesizing trisilylamine, which is prepared by using a catalytic distillation tower. The catalytic distillation tower is composed of a rectification section, a reaction section, a stripping section and a tower kettle connected in sequence from the top of the tower to the bottom of the tower. Its characteristics The preparation method includes the following steps: purging the catalytic distillation tower with an inert gas in advance, respectively simultaneously adding monochlorosilane and ammonia in gaseous form from the rectification section and the stripping section to the catalytic distillation tower for reaction. The molar ratio of chlorosilane and ammonia is 1:1.8, the space velocity of chlorosilane is 1 / h, the reaction pressure is 0.4MPa, and the reaction temperature of the distillation tower is 370°C. High-purity trisilylamine is obtained by known impurity removal and...

Embodiment 2

[0030] A synthetic method for trisilylamine, comprising the following steps:

[0031]1) A method for synthesizing trisilylamine, which is prepared by using a catalytic distillation tower. The catalytic distillation tower is composed of a rectification section, a reaction section, a stripping section and a tower kettle connected in sequence from the top of the tower to the bottom of the tower. Its characteristics The preparation method includes the following steps: purging the catalytic distillation tower with an inert gas in advance, respectively simultaneously adding monochlorosilane and ammonia in gaseous form from the rectification section and the stripping section to the catalytic distillation tower for reaction. The molar ratio of chlorosilane and ammonia is 1:1.2, the space velocity of chlorosilane is 0.5 / h, the reaction pressure is 0.2MPa, and the reaction temperature of the distillation tower is 350°C. High-purity trisilylamine is obtained by known impurity removal and...

Embodiment 3

[0036] A synthetic method for trisilylamine, comprising the following steps:

[0037] 1) A method for synthesizing trisilylamine, which is prepared by using a catalytic distillation tower. The catalytic distillation tower is composed of a rectification section, a reaction section, a stripping section and a tower kettle connected in sequence from the top of the tower to the bottom of the tower. Its characteristics The preparation method includes the following steps: purging the catalytic distillation tower with an inert gas in advance, respectively simultaneously adding monochlorosilane and ammonia in gaseous form from the rectification section and the stripping section to the catalytic distillation tower for reaction. The molar ratio of chlorosilane and ammonia is 1:3, the space velocity of chlorosilane is 2 / h, the reaction pressure is 1MPa, and the reaction temperature of the distillation tower is 420°C. The reaction product in the tower reactor is continuously drawn out, NH4C...

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Abstract

The invention provides a synthesis method of trimethylsilylamine, which is characterized in that the preparation method includes the following steps: purging a catalytic distillation tower with inert gas in advance, and simultaneously removing monochlorosilane and ammonia from the rectification tower in gaseous form. Section and stripping section are continuously added to the catalytic distillation tower for reaction. The molar ratio of monochlorosilane and ammonia is 1:1.2-3, the space velocity of monochlorosilane is 0.5-2 / h, and the reaction pressure is 0.2-1MPa. The distillation tower The reaction temperature is 350°C-420°C. The reaction product from the tower reactor is continuously taken out, NH4Cl is separated, and then high-purity trimethylsilylamine is obtained through the impurity removal and refining technology known in the industry.

Description

technical field [0001] The invention relates to a synthesis method of silylamine, in particular to a synthesis method of trisilylamine. Background technique [0002] Organoaminosilane precursors can be used in a variety of deposition processes including, but not limited to, atomic layer deposition ("ALD"), chemical vapor deposition ("CVD"), plasma enhanced chemical vapor deposition ("PECVD"), low pressure chemical vapor deposition deposition ("LPCVD") and atmospheric pressure chemical vapor deposition. Several classes of compounds are useful as precursors for silicon-containing films such as, but not limited to, silicon oxide or silicon nitride films. Examples of such compounds suitable for use as precursors include silanes, chlorosilanes, polysilazanes, aminosilanes and azidosilanes. Inert carrier gases or diluents (such as, but not limited to, helium, hydrogen, nitrogen, etc.) are also used to deliver the precursors into the reaction chamber. [0003] Trisilylamine can ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/10C07F7/20B01J23/89B01J35/06B01J37/08
CPCC07F7/10C07F7/20B01J23/892B01J37/086B01J35/58Y02P20/10
Inventor 陈刚李军杨建成叶向荣花永紧张雪刚
Owner ZHEJIANG BRITECH CO LTD
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