Preparation method of siloxane modified polyaspartic acid ester

An aspartate and siloxane modification technology, which is applied in the field of chemical product synthesis, can solve the problems of low double bond activity, less double bond steric hindrance, and increased resin viscosity, and achieves low production cost and single composition. , the effect of simple operation

Active Publication Date: 2015-07-01
广东坚派新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the silane coupling agents described in the above-mentioned patent documents all have highly active primary amino groups and short-chain alkyl groups, and the reaction speed with isocyanates in organic polymers is too fast, and the short-chain alkyl groups are compatible with the polymer substrate. Therefore, in the actual application process, there will be a reaction that will lead to poor compatibility and uniformity of the system, and the viscosity of the resin will rise rapidly, which will eventually affect the binding ability of the silane coupling agent and the organic polymer.
[0004] There is also a patent CN200610124089.8 that uses acrylate to modify γ-aminopropyltrialkoxysilane, but the double bond activity of acrylate is low and the double bond is less hindered, so the modified silane coupling agent has primary amines , secondary amines and tertiary amines, although they can effectively improve their compatibility with polymer substrates, but due to the high activity of primary amines, tertiary amines have a catalytic effect, so the modified γ-aminopropyltrialkoxy The reaction speed between silane and isocyanate in organic polymers is still fast, resulting in a rapid rise in resin viscosity after mixing, poor system compatibility and uniformity, and the binding ability of silane coupling agent and organic polymers is also unsatisfactory

Method used

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  • Preparation method of siloxane modified polyaspartic acid ester

Examples

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Comparison scheme
Effect test

example 1

[0023] Mix 3.5g of 3A molecular sieve with 110g of diethyl maleate, keep the temperature at 90°C, stir at 500°C, keep warm for 70 minutes, heat up to 120°C, turn on the vacuum pump and adjust the vacuum degree to 300Pa to start vacuum rectification, rectification Carry out after 60min, after temperature rises to 150 ℃, promptly there is no rectification product, stop rectification, obtain the diethyl maleate that water content is 400ppm; Add 110g gamma-aminopropyltriethoxy in the reaction kettle Silane and pass nitrogen gas for 10 minutes, raise the temperature to 40°C, start stirring and maintain the stirring speed at 500r / min, and start to drop 86g of diethyl maleate that has been dehydrated, and control the dropping speed to 1 drop / S, with the reaction Exothermic, control the temperature not to exceed 80°C, dropwise is completed in about 50-80 minutes, that is, maintain the temperature and the reaction temperature at 80°C and continue the reaction for 24 hours to obtain the ...

example 2

[0025]Mix 6.0g of 3A molecular sieve with 160g of diisobutyl maleate, keep the temperature at 90°C, stir at 500°C, keep warm for 70 minutes, raise the temperature to 140°C, turn on the vacuum pump and adjust the vacuum degree to 300Pa to start rectification under reduced pressure. After distillation for 60min, when the temperature rises to 180°C, there is no rectification product, stop the rectification, and obtain a maleic acid ester with a water content of 200ppm; add 110g of γ-aminopropyltriethoxysilane to the reaction kettle And pass through nitrogen for 8 minutes, heat up to 40°C, start stirring and maintain the stirring speed at 500r / min, and start to drop 114g of diisobutyl maleate after dehydration, control the dropping speed to 2 drops / S, with the reaction Exothermic, control the temperature not to exceed 80°C, the dropwise addition is completed in about 50-80 minutes, that is, maintain the temperature and the reaction temperature at 80°C and continue the reaction for ...

example 3

[0027] Mix 6.0g of 3A molecular sieve with 160g of dipropyl maleate, keep the temperature at 90°C, stir at 500°C, keep warm for 70 minutes, raise the temperature to 120°C, turn on the vacuum pump and adjust the vacuum degree to 300Pa to start vacuum rectification, rectification After 60 minutes, when the temperature rises to 160°C, there is no rectification product, stop the rectification to obtain dipropyl maleate with a water content of 200ppm; add 90g of γ-aminopropyltrimethoxysilane to the reaction kettle And feed nitrogen gas for 8 minutes, heat up to 40°C, start stirring and maintain the stirring speed at 500r / min, and start to drop 102g of dipropyl maleate after dehydration, control the dropping speed to 1-2 drops / S, with The reaction is exothermic, and the temperature is controlled not to exceed 80°C. The dropwise addition is completed in about 50-80 minutes, that is, the temperature is maintained at 80°C and the reaction is continued for 24 hours to obtain the crude pr...

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Abstract

The invention discloses a preparation method of siloxane modified polyaspartic acid ester. The method comprises the step of adding primary amine in gamma-aminopropyl trialkoyl saline to a carbon-carbon double-bond in a maleate monomer to generate the siloxane modified polyaspartic acid ester. The method specifically comprises the following steps: dropwise adding maleate to the gamma-aminopropyl trialkoyl saline at 30-80 DEG C for 50-80 minutes; and then insulating and reacting for 12-24 hours at 60-100 DEG C to obtain the siloxane modified polyaspartic acid ester. The preparation method disclosed by the invention is free of side reactions, simple to operate and low in production cost, and the product has the advantages of being single in component, good in stability, low in viscosity, high in purity (the purity can reach over 99.5%) and the like. The prepared siloxane modified polyaspartic acid ester can be applied to any filed of gamma-aminopropyl trialkoyl saline, and particularly, the siloxane modified polyaspartic acid ester has a relatively remarkable application performance in polyurethane waterproof field.

Description

technical field [0001] The invention belongs to the field of synthesis of chemical products, and relates to a method for preparing a siloxane-modified polyaspartic acid ester through an organic chemical reaction of double bond addition, in particular to a maleate-modified γ-ammonia A method for preparing siloxane-modified polyaspartate from propyltrialkoxysilane. Background technique [0002] The silane coupling agent itself acts as a "molecular bridge" to form a firm and stable bond between two weakly bonded interfaces, which can obviously connect two substances with different properties. The mechanism of action of the silane coupling agent is that under certain conditions, small molecule alcohols (methanol, ethanol) are hydrolyzed to form silane polycondensed alkoxysilanes, which are mainly coupled with inorganic substrates, while the organic functional groups at one end of the silane coupling agent It has a certain compatibility with organic polymers, and the two can be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/00
Inventor 李世伯
Owner 广东坚派新材料有限公司
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