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Method for preparing isocyanate-based silane by hydrosilylation reaction

A technology for hydrosilylation reaction and isocyanate, which is applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic chemistry, etc., can solve the problems of slow cracking speed, high energy consumption and low efficiency, etc. Achieve the effect of less impurities, low energy consumption and high reactivity

Inactive Publication Date: 2019-08-16
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This route can effectively avoid the environmental hazards caused by phosgene, and the raw materials are easy to get, no corrosion to equipment, and the conversion rate and yield are high. Carried out at high temperature, high energy consumption, slow cracking speed, low efficiency, and because it is a high-heat environment, the product itself is easy to polymerize, and it is also easy to react with intermediates to form other substances. Therefore, cracking inevitably produces a certain amount of high boiling , its main components are trimer of isocyanate, urea, biuret and a small amount of other oligomers, etc.

Method used

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  • Method for preparing isocyanate-based silane by hydrosilylation reaction
  • Method for preparing isocyanate-based silane by hydrosilylation reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 300 g of allylurea, 1200 g of toluene and 30 g of tetrabutylammonium bromide were put into a 2000 ml four-necked reaction flask equipped with mechanical stirring, a thermometer and a constant pressure dropping funnel. And add 950g of sodium nitrite aqueous solution (42% concentration) and 500g of concentrated hydrochloric acid into the constant pressure dropping funnel, under the condition of ice-water bath, start the mechanical stirring, keep the system temperature at 0°C, after 30 minutes, at the mechanical stirring speed Under the condition of 100-300 revolutions per minute, start to add the aqueous solution of sodium nitrite and concentrated hydrochloric acid dropwise, and the dropping time is controlled at 5h. After the reaction is completed, 3-isocyanatopropylene is obtained through filtration, layering, distillation, etc. The product is 229.3g, the molar yield is 92%, and the content is 99.3%.

[0033]Put 249.3 g of 3-propene isocyanate into a 2000 ml four-necked...

Embodiment 2

[0035] 300 g of allylurea, 1200 g of toluene and 30 g of tetrabutylammonium bromide were put into a 2000 ml four-necked reaction flask equipped with mechanical stirring, a thermometer and a constant pressure dropping funnel. And add 950g of sodium nitrite aqueous solution (42% concentration) and 500g of concentrated hydrochloric acid into the constant pressure dropping funnel, under the condition of ice-water bath, start the mechanical stirring, keep the system temperature at 1°C, after 30 minutes, at the mechanical stirring speed Under the condition of 200 revolutions per minute, the aqueous solution of sodium nitrite and concentrated hydrochloric acid were added dropwise, and the dropping time was controlled at 6 hours. After the reaction was completed, the 3-isocyanate propene product 229.3 was obtained through filtration, layering, distillation, etc. g, the molar yield is 92%, and the content is 99.3%.

[0036] Put 249.3g of 3-propene isocyanate into a 2000ml four-necked r...

Embodiment 3

[0038] 300 g of allylurea, 1200 g of toluene and 30 g of tetrabutylammonium bromide were put into a 2000 ml four-necked reaction flask equipped with mechanical stirring, a thermometer and a constant pressure dropping funnel. And add 950g of sodium nitrite aqueous solution (42% concentration) and 500g of concentrated hydrochloric acid into the constant pressure dropping funnel, under the condition of ice-water bath, start the mechanical stirring, keep the system temperature at 2°C, after 30 minutes, at the mechanical stirring speed Under the condition of 250 revolutions per minute, the aqueous solution of sodium nitrite and concentrated hydrochloric acid were added dropwise, and the dropping time was controlled at 7h. After the reaction was completed, the 3-isocyanate propene product 229.3 was obtained through filtration, layering, distillation, etc. g, the molar yield is 92%, and the content is 99.3%.

[0039] In the 2000ml four-necked reaction flask with mechanical stirring, ...

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Abstract

The invention relates to a synthetic method of an isocyanate-based silane coupling agent and belongs to the field of synthesis of silane coupling agents. The preparation method comprises the followingsteps: taking allyl urea and sodium nitrite as main raw materials, taking toluene as a solvent, and taking tetra-n-butyl ammonium bromide as a catalyst to synthesize allyl isocyanate; then, under theaction of a noble metal catalyst such as platinum or rhodium, carrying out hydrosilylation with silicon-hydrogen bond containing hydrogenalkoxysilanes such as trimethoxy silane, triethoxy silane andthe like for carrying out a reaction to generate an isocyanate-based silane coupling agent crude product; and then carrying out reduced pressure distillation treatment to obtain the isocyanate-based silane coupling agent product. The method has the advantages of simple operation, high reaction conversion rate, high yield, stable quality, safe environment-friendly energy-saving efficient productionprocess, and the like, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to a method for preparing isocyanatosilane by hydrosilylation reaction, belonging to the field of silane coupling agent synthesis. Background technique [0002] Isocyanate-based silane is a kind of silane coupling agent containing two different active groups of isocyanate and alkoxy group in the molecule. The isocyanate group shows the chemical characteristics of typical alkyl isocyanic acid and is very easy to polymerize with organic The active hydrogen in the compound (such as hydroxyl, amino, mercapto, etc.) reacts, and the methoxy group is hydrolyzed and cross-linked to provide good adhesion to the substrate. Utilizing the above characteristics, isocyanate silane can be used for end-capping and modifying the above-mentioned different types of organic polymers, improving the adhesion and water resistance of the resin coating to various substrates, and improving the mechanical, electrical, water resistance and water resistance o...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1876
Inventor 王欣甘俊甘书官陈圣云
Owner JINGZHOU JIANGHAN FINE CHEM
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