Vinyl trimethoxysilane oligomer preparation method

A vinyltrimethoxysilane and oligomer technology is applied in the field of preparation of vinyltrimethoxysilane oligomers and can solve the problems of vinyltrimethoxysilane with low boiling point and flash point, safety and hidden dangers. , to achieve the effect of good safety and operability, easy implementation and simple process

Active Publication Date: 2007-10-17
南京市化学工业研究设计院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The problem to be solved by the present invention is that the boiling point and flash point of vinyltrimethoxysilane are relatively low, and there are potential safety hazards in the application process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 300g of vinyltrimethoxysilane into a 500ml three-necked flask equipped with a stirrer, thermometer, and discharge tube, add hydrochloric acid dropwise while stirring until the pH value is 5, then add 0.03g of copper hydroxide, stir for 10min to make it fully mix. Add 31 grams of deionized water dropwise at a constant speed, and the dropwise addition is completed within 15 minutes. The generated methanol was distilled off at -0.1MPa at 120°C. Then add 20 g of anhydrous calcium carbonate to neutralize the residual acid, stir thoroughly for 30 min, then filter with suction, collect the filtrate to obtain the product, which is a slightly yellowish transparent liquid with a yield of 92%.

Embodiment 2

[0018] Add 300g of vinyltrimethoxysilane into a 500ml three-necked flask equipped with a stirrer, thermometer, and discharge tube, add glacial acetic acid dropwise while stirring until the pH value is 4, then add 0.03g of aluminum trichloride, and stir for 10min to make Mix it well. 43g of deionized water was added dropwise at a constant speed, and the dropwise addition was completed within 15 minutes. The generated methanol was distilled off at -0.1MPa at 110°C. Then add 20 g of anhydrous calcium carbonate to neutralize the residual acid, stir thoroughly for 30 min, then filter with suction, collect the filtrate to obtain the product, which is a colorless transparent liquid with a yield of 96%.

Embodiment 3

[0020] Add 300g of vinyltrimethoxysilane into a 500ml three-necked flask equipped with a stirrer, thermometer and discharge tube, add sulfuric acid dropwise while stirring until the pH value is 6, then add 0.03g of iron oxide, stir for 10min to make it fully mixed . Under nitrogen protection, 44 g of distilled water was added dropwise at a constant speed, and the dropwise addition was completed within 15 minutes. The generated methanol was distilled off at -0.1MPa at 110°C. Then add 30 g of anhydrous calcium carbonate to neutralize the residual acid, stir thoroughly for 30 min, then filter with suction, collect the filtrate to obtain the product, which is a slightly yellow transparent liquid with a yield of 86%.

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Abstract

The invention relates the method for preparation of ethenyl trimethoxy silane low-molecular polymer, comprising the following steps: 1 adding the ethenyl trimethoxy silane into the reactor, adjusting the PH at 4-7 by adding the acid; 2 adding the metallic catalyst, the dosage of which is 10-1000ppm, stirring; 3 at 60-160 DEG C, making them hydrolytic polycondensation reaction for 6-12 hours by adding water, the weight ratio of water and ethenyl trimethoxy silane being 0.05-0.15; 4 distilling and removing the by-product carbinol; 5 neutralizing the acid by adding the alkali, using the suction and getting the product. The invention possesses the characters of simple technology and easy accomplishment. Because the boiling point and flash point of the said ethenyl trimethoxy silane low-molecular polymer are high, the security and operability is better. The alcohol of releasing by using the method is less, so it is more propitious to environmental protection.

Description

technical field [0001] The invention relates to a preparation method of vinyltrimethoxysilane oligomer. Background technique [0002] Vinyltrimethoxysilane, United States Union Carbide brand A-171, is a widely used silane coupling agent. Mainly used for polyethylene crosslinking agent, glass fiber surface treatment of glass fiber reinforced plastics, synthesis of special coatings, surface moisture-proof treatment of electronic components, surface treatment of inorganic silicon-containing fillers, etc. However, since vinyltrimethoxysilane is a single-chain substance, its boiling point (about 110°C) and flash point (about 22°C) are relatively low, so it is used in polyethylene crosslinking agents and glass fiber reinforced plastics. There are safety hazards in surface treatment. Contents of the invention [0003] What the present invention aims to solve is the problem that vinyltrimethoxysilane has a relatively low boiling point and flash point and has potential safety haz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/32C07F7/02
Inventor 陶再山李钟宝祁拥军
Owner 南京市化学工业研究设计院有限公司
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