A kind of synthesis technique of alkoxysilane containing amide group

The technology of aminoalkylalkoxysilane and alkoxysilane is applied in the field of synthesis technology of alkoxysilane, and can solve problems such as hydrolysis equipment and corrosion, and achieve the effects of improving reaction activity, avoiding corrosion, and being easy to separate and remove.

Active Publication Date: 2016-02-24
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to solve the problem of hydrolysis of easily hydrolyzed alkoxysilane groups contained in the structure or equipment corrosion caused by the production of by-product water or HCl when synthesizing amide-containing alkoxysilanes in the prior art, Provide a synthesis process of alkoxysilane containing amide group, this synthesis process only produces by-product alcohol, has no effect on the reaction and the main product of the reaction, and is relatively easy to separate and remove

Method used

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  • A kind of synthesis technique of alkoxysilane containing amide group
  • A kind of synthesis technique of alkoxysilane containing amide group
  • A kind of synthesis technique of alkoxysilane containing amide group

Examples

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Effect test

Embodiment 1

[0029] In a 500ml three-neck flask equipped with nitrogen conduit, tail gas liquid seal, stirrer, thermometer, reflux condenser and heating device, add 52.8g of dimethyl malonate, γ-aminopropylmethyldiethoxysilane 160.4g. Stir and heat to reflux at 90°C. After 7 hours of reaction, change the reflux device to a distillation device, and then heat at 90°C to distill the by-product methanol under normal pressure, and then distill the excess raw materials at 140°C under reduced pressure to obtain a light yellow liquid The product N,N'-bis[3-(diethoxymethylsilyl)propyl]malonamide 165.6g. The yield is 92%.

Embodiment 2

[0031] In a 1000ml four-neck flask equipped with a nitrogen conduit, tail gas liquid seal, dropping funnel, stirrer, thermometer, reflux condenser and heating device, add 194g of dimethyl terephthalate, γ-aminopropylmethyl Diethoxysilane 382g, sodium methoxide 1g. Stir and heat to reflux at 90-95°C, stop heating after 5 hours of reaction and cool the material to room temperature, start stirring again while adding 1.3g of dimethyldichlorosilane to neutralize the catalyst sodium methoxide through the dropping funnel, and then heat for 90 Atmospheric pressure distillation at ℃ to separate by-product methanol, dimethyldimethoxysilane, etc., and then distill off excess raw materials at 120 ℃ under reduced pressure. After cooling, the light yellow solid product N,N'-bis[3-( Diethoxymethylsilyl)propyl]terephthalamide 474g. Yield 92.6%.

Embodiment 3

[0033] Add 52.8 g of dimethyl malonate and 186 g of γ-aminopropyltriethoxysilane into a 500 ml three-neck flask equipped with a nitrogen conduit, tail gas liquid seal, stirrer, thermometer, reflux condenser and heating device. Stir and heat to reflux at 100°C. After 7 hours of reaction, change the reflux device to a distillation device, heat and distill the by-product methanol at 70°C under normal pressure, and then distill the excess raw materials at 130°C under reduced pressure to obtain a light yellow liquid product N,N'-bis[3-(triethoxysilyl)propyl]malonamide 181.6 g. Yield 89%.

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Abstract

The invention provides a process for synthesizing amidoalkylalkoxysilane. Carboxylate and aminoalkylalkoxysilane are used as raw materials for heating and reflux reaction. If necessary, sodium alkoxide can be added as a catalyst to make amidation reaction between ester and amino group to generate amidoalkylalkoxysilane target product and by-products alcohol. After the reaction is completed, use a small amount of chlorosilane to neutralize the sodium alkoxide catalyst, then distill under normal pressure to remove alcohols and other low boilers, and then distill under reduced pressure to remove unreacted high boiling point raw materials. The conversion rate of the target product can reach more than 90%, and the by-product alcohol in the process will not hydrolyze the alkoxy silicon groups in the raw materials and products. The target product can also be further purified by rectification, and can be used as a coupling agent, a crosslinking agent, or a monomer for synthesizing silicone resin.

Description

technical field [0001] The invention relates to a synthesis process of alkoxysilane, more specifically, the invention relates to a synthesis process of amide group-containing alkoxysilane, which belongs to the technical field of organosilicon compounds. Background technique [0002] Alkoxysilane generally refers to a silane compound with two or more alkoxy groups (such as methoxy, ethoxy, etc.) attached to a silicon atom. Other organic groups, such as methyl, vinyl, aminopropyl, etc. It is mainly used as a silane coupling agent, a monomer for synthesizing silicone resin or a crosslinking agent for room temperature vulcanized silicone rubber, etc. It has been widely used as a large class of organosilicon compounds. However, there are few reports on the synthesis and application of alkoxysilanes containing amide groups. [0003] Most alkoxysilanes are generally obtained by alcoholysis of corresponding chlorosilanes, such as methyltriethoxysilane, tetraethylorthosilicate, etc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 朱良波唐小斗钟云竹
Owner CHINA BLUESTAR CHENGRAND CO LTD
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