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Prepn process of organic silicone oximino silane

A manufacturing method and technology of silicone oxime, which are applied in the directions of organic chemistry, chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, etc. Health and other issues, to achieve the effect of simple process route, high product yield and high product purity

Inactive Publication Date: 2007-10-10
陈俊光
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Existing methyl or vinyl tributylketoxime silane and tetrabutylketoxime silane are produced by the joint reaction of chlorosilane and alkaline-containing organic matter, and the content (purity) usually obtained is low, and the yield (production Yield) is low, the production process is difficult to operate, the yield and quality are unstable, and the product is colored (slightly yellow, amber and other colors are available)
It cannot meet the needs of customers, the solvents used are harmful to health, and the manufacturing cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 Preparation of methyl tributyl ketoximinosilane

[0016] (1) chlorosilane was added dropwise to butanone oxime containing solvent petroleum ether at 20°C, and the solution was allowed to settle at 25°C, so that the solvent in the upper layer and the crude product and the salt in the lower layer were clearly separated, the lower layer salt was removed, and the recovery Ketoxime raw material; the molar ratio of chlorosilane and butanone oxime is 1:2.04; the amount of solvent is 20% of the total material mass, and the chlorosilane refers to R a SiCl b , R is methyl, a=1, b=3; the ketoxime refers to butanone oxime.

[0017] (2) the ammonia gas after the drying treatment is passed into the solvent and the crude product of the upper layer obtained in step (1), the temperature is controlled at 20 ° C, and the ventilation is stopped when the pH value reaches 7;

[0018] (3) under the protection of dry air, clean the product of step (2) with solvent petroleum ether, ...

Embodiment 2

[0020] Example 2 Preparation of ethylene tributyl ketoximinosilane

[0021] (1) chlorosilane was added dropwise to butanone oxime containing solvent petroleum ether at 50°C, and the solution was allowed to settle at 40°C, so that the solvent in the upper layer and the crude product and the salt in the lower layer were clearly separated, the lower layer salt was removed, and the recovery Ketoxime raw material; the molar ratio of chlorosilane and ketoxime is 1:2.07; the amount of solvent is 60% of the total material mass, and the chlorosilane refers to R a SiCl b , R is a vinyl group, a=1, b=3; the ketoxime refers to butanone oxime.

[0022] (2) the ammonia gas after the drying treatment is passed into the solvent and the crude product of the upper layer obtained in step (1), the temperature is controlled at 52 ° C, and the ventilation is stopped when the pH value reaches 7.5;

[0023] (3) under the protection of dry air, clean the product of step (2) with solvent petroleum et...

Embodiment 3

[0025] Example 3 Preparation of phenyltributanone oximinosilane

[0026] (1) chlorosilane was added dropwise to butanone oxime containing solvent petroleum ether at 30°C, and the solution was allowed to settle at 25°C, so that the solvent in the upper layer and the crude product and the salt in the lower layer were clearly separated, the lower layer salt was removed, and the recovery Ketoxime raw material; the molar ratio of the chlorosilane and the ketoxime is 1:2.05; the amount of petroleum ether is 20% of the total material mass, and the chlorosilane refers to R a SiCl b , R is phenyl, a=1, b=3; the ketoxime refers to butanone oxime.

[0027] (2) the ammonia gas after the drying treatment is passed into the solvent and the crude product of the upper layer obtained in step (1), the temperature is controlled at 30 ° C, and the ventilation is stopped when the pH value reaches 7.3;

[0028] (3) under the protection of dry air, use solvent petroleum ether to clean the product ...

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PUM

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Abstract

The preparation process of organic silicone oximino silane includes the following steps: 1. dropping silane chloride into ketoxime with solvent, depositing to separating solvent and coarse product in the upper layer and salt in the lower layer, eliminating salt and recovering ketoxime material; 2. introducing dry ammonia into the solvent and coarse product in the upper layer until reaching pH 7-7.5; 3. washing the product of the foregoing step with solvent under protection of dry air, and eliminating solvent at 70 deg.c and 50 mmHg vacuum degree to leave coarse product; and 4. adding solvent into the coarse product inside still, dropping silane chloride into the coarse product; repeating the steps 1-3 to obtain colorless transparent liquid product. The product may be used as curing agent and additive for RTV silicone rubber and other organic silicone product, including resin, paint, adhesive, etc.

Description

technical field [0001] The present invention relates to use as organosilicon siloxane type cross-linking agent or coupling agent, or for making RTV silicone rubber and other organosilicon products and resins, coatings, adhesives, plastics, or as curing agent for pharmaceutical raw materials Or additive manufacturing method of organosilicon oximosilane. Background technique [0002] Existing methyl or vinyl tributanone oximo silane and tetrabutanone oximo silane are produced by the co-reaction of chlorosilane and basic organic matter, and the content (purity) obtained is usually low, and the yield (preparation) is low. yield) is low, the production process is difficult to operate, the yield and quality are unstable, and the product is colored (yellowish, amber and other colors). Can not meet the needs of customers, the solvent used is harmful to health, and the manufacturing cost is high. SUMMARY OF THE INVENTION [0003] The purpose of the present invention is to address...

Claims

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Application Information

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IPC IPC(8): C07F7/10
Inventor 陈俊光林博
Owner 陈俊光
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