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A kind of two (diethylamino) silane synthetic method

A diethylamino and synthesis method technology, applied in the field of bis(diethylamino)silane synthesis, can solve the problems of reduced volume efficiency, low reaction yield, loss and waste of alkyl metal reagents, etc., to achieve increased yield, easy separation effect

Active Publication Date: 2020-09-15
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] ‍‍Existing patents and literature technology react a large amount of dialkylamine hydrochloride by-product, the alkyl metal reagent is easy to lose and waste, and the reaction yield is low. Therefore, in order to obtain dialkylaminosilane, it needs Decreased volumetric efficiency, or solid-liquid separation operations such as filtration or decantation

Method used

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  • A kind of two (diethylamino) silane synthetic method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] ‍A method for synthesizing bis(diethylamino)silane, comprising the following steps:

[0021] ‍1) Using Cu(NO 3 ) 2 Dissolved in water, the Cu(NO 3 ) 2 The solution is used as a pillar liquid for subsequent use;

[0022] 2) Add clay to the water so that the weight ratio of clay to water is 1:2, stir until the clay is dispersed in water, add 4-fluorobenzamide oxime accounting for 0.03% of the clay mass, and tetraphenylboronic acid accounting for 0.003% of the clay mass Tris(1,2-dimethoxyethane)lithium adduct, ethylenebis(tetrahydroindenyl)titanium dichloride 0.002% by mass of clay, 2-ethylhexyl 3% by mass of clay Zinc acid, continue to stir to obtain clay solution;

[0023] 3) the pillar liquid obtained in step 1) is mixed with the clay solution obtained in step 2) to make Cu(NO 3 ) 2 Accounting for 5% of the mass of clay, heat up to 98°C and stir for 60 hours, then granulate and dry to obtain a clay catalyst.

[0024] 4) In parts by weight, add 100 parts of dichl...

Embodiment 2

[0026] A kind of two (diethylamino) silane synthetic method, comprises the following steps:

[0027] ‍1) Using Cu(NO 3 ) 2 Dissolved in water to obtain Cu(NO 3 ) 2 The solution is used as a pillar liquid for subsequent use;

[0028] 2) Add clay to the water so that the weight ratio of clay to water is 1:1, stir until the clay is dispersed in water, add 4-fluorobenzamide oxime accounting for 0.01% of the clay mass, and tetraphenylboronic acid accounting for 0.001% of the clay mass Tris(1,2-dimethoxyethane) lithium adduct, ethylenebis(tetrahydroindenyl)titanium dichloride 0.001% by mass of clay, 2-ethylhexyl 1% by mass of clay Zinc acid, continue to stir to obtain clay solution;

[0029] 3) the pillar liquid obtained in step 1) is mixed with the clay solution obtained in step 2) to make Cu(NO 3 ) 2 Accounting for 3% of the mass of clay, heat up to 90°C and stir for 80 hours, then granulate and dry to obtain a clay catalyst.

[0030] 4) According to parts by weight, add 1...

Embodiment 3

[0032] A kind of two (diethylamino) silane synthetic method, comprises the following steps:

[0033] ‍1) Dissolve Cu(NO3)2 in water to obtain a Cu(NO3)2 solution with a mass percentage concentration of 40% as a pillar liquid, and set aside;

[0034] 2) Add clay to the water so that the weight ratio of clay to water is 1:3, stir until the clay is dispersed in water, add 4-fluorobenzamide oxime accounting for 0.05% of the clay mass, and tetraphenylboronic acid accounting for 0.005% of the clay mass Tris(1,2-dimethoxyethane)lithium adduct, ethylenebis(tetrahydroindenyl)titanium dichloride, 0.005% by mass of clay, 2-ethylhexyl, 5% by mass of clay Zinc acid, continue to stir to obtain clay solution;

[0035] 3) Mix the pillar liquid obtained in step 1) with the clay solution obtained in step 2), so that Cu(NO3)2 accounts for 10% of the clay mass, heat up to 120°C and stir for 50h, then granulate and dry to obtain clay catalyst.

[0036] 4) In parts by weight, add 100 parts of di...

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Abstract

The invention provides a synthesis method of bis(diethylamino)silane. The method is characterized by comprising the following steps of adding 100 parts of dichlorosilane, 1000 to 2000 parts of hexaneand 5 to 20 parts of white clay catalysts into a reactor in parts by weight; introducing nitrogen gas; dripping 300 to 600 parts of diethylamine under the stirring condition for reaction; maintainingthe temperature of the reaction system at 40 to 60 DEG C; after the dripping completion, performing heat insulation for 5 to 10 hours; then, obtaining the bis(diethylamino)silane by the existing impurity removal technology in industry.

Description

technical field [0001] The invention relates to a method for preparing silane, in particular to a method for synthesizing bis(diethylamino)silane. 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 Phase 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] JPWO2016152...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/02B01J31/28
CPCB01J31/28C07F7/025
Inventor 陈刚李军张广第付铁柱赵丹张雪刚
Owner ZHEJIANG BRITECH CO LTD