Method for preparing 3-isocyanatopropyltrimethoxysilane

A technology of esteryl propyltrimethoxysilane and trimethoxysilane, which is applied in the field of preparation of 3-isocyanatopropyltrimethoxysilane, and can solve problems such as difficult control of by-products, harsh reaction conditions, and long reaction time , to achieve the effects of safe production, easy control, good product quality and high conversion rate

Inactive Publication Date: 2019-01-18
大连鼎燕医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 2. Thermal cracking method, using silane-based carbamate compounds, the reaction needs to be cracked at high temperature (200-260°C) with the help of alkali metal organic salt as a catalyst to prepare isocyanate alkoxysilane, the reaction conditions are harsh, and the by-products difficult to control
[0008] 3. In the isocyanate alkali metal salt method, the raw material sodium isocyanate or potassium isocyanate is a highly toxic compound, which has low safety and pollutes the environment
The reaction time is long and the yield is low

Method used

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  • Method for preparing 3-isocyanatopropyltrimethoxysilane
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  • Method for preparing 3-isocyanatopropyltrimethoxysilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 126 g of methyl [3-(trimethoxysilane)propyl] carbamate, 59 g of triethylamine and 400 ml of toluene into a 1 L reaction kettle, and stir. Under nitrogen protection, add 45g of methyltrichlorosilane dropwise at 20-40°C, after the dropwise addition, slowly raise the temperature to 95-100°C, react for 1h, take samples for analysis, [3-(trimethoxysilane)propyl]carbamic acid When the GC content of methyl ester is less than 1%, the heating can be stopped. Cool down to 20-30°C and filter, and wash the filter cake twice with 100ml of toluene. The filtrates were combined, toluene was concentrated, and 107 g of the product was evaporated under reduced pressure, with a yield of 96% and a content of 98%.

Embodiment 2

[0035] Put 150 g of [3-(trimethoxysilyl)propyl]methyl carbamate, 96 g of triethylamine and 400 ml of toluene into a 1L reaction flask, and stir. Under nitrogen protection, add 75g of methyltrichlorosilane dropwise at 20-40°C, after the dropwise addition, slowly raise the temperature to 95-100°C, react for 1h, take samples for analysis, [3-(trimethoxysilane)propyl]carbamic acid When the GC content of methyl ester is less than 1%, the heating can be stopped. Cool down and filter, and the filter cake is washed twice with 150ml of toluene. The filtrates were combined, the solvent was evaporated, and 127 g of the product was evaporated under reduced pressure, with a yield of 95.8% and a content of 98%.

Embodiment 3

[0037] Add 169 g of [3-(trimethoxysilane)propyl] methyl carbamate, 111 g of triethylamine and 400 ml of toluene into a 1 L reaction kettle, and stir. Under nitrogen protection, add 106g of methyltrichlorosilane dropwise at 20-40°C, after the addition is complete, slowly raise the temperature to 95-100°C, react for 1h, take samples for analysis, [3-(trimethoxysilane)propyl]carbamic acid When the GC content of methyl ester is less than 1%, the heating can be stopped. Cool down and filter, and the filter cake is washed twice with 150ml of toluene. The filtrates were combined, the solvent was concentrated, and 142 g of the product was evaporated under reduced pressure, with a yield of 95.3% and a content of 97.7%.

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Abstract

The invention relates to a method for preparing 3-isocyanatopropyltrimethoxysilane. The method is characterized in that [3-(trimethoxysilane)propyl]methyl carbamate is used as a raw material to reactwith methyl trichlorosilane, and thus 3-isocyanatopropyltrimethoxysilane is synthesized by one step. The preparation method provided by the invention is simple, the production process is safe, the reaction temperature is easy to control, production equipment is simple, and thus the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of an isocyanate compound, in particular to a preparation method of 3-isocyanatopropyltrimethoxysilane. Background technique [0002] 3-Isocyanatopropyltrimethoxysilane is an isocyanate-functional silane used as a crosslinker and adhesion promoter in adhesives and sealants. Its outstanding wet adhesion can adhere to glass, metal and other inorganic substrates; it can also adhere well to difficult-to-adhere substrates, such as nylon and other plastic products. It can be rapidly hydrolyzed in the presence of atmospheric humidity, and has very good thermal stability, chemical stability and UV stability. Suitable polymers: acrylics, silicones (Si), PU-prepolymers, etc. [0003] The synthetic method of existing isocyanate alkoxysilane mainly contains following several kinds at present: [0004] 1. The phosgene method is suitable for industrial production, but the raw material phosgene is highly toxic, and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
CPCC07F7/1888
Inventor 蔡鲁伯王洋吕永智董志军刘岩
Owner 大连鼎燕医药化工有限公司
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