Method for synthesizing trimethyl allyl polyoxypropylene ether

A technology of trimethylallyl polyoxypropylene ether and alcohol polyoxypropylene ether, which is applied in the field of preparation of alkyl-terminated polyethers, can solve the problem of highly toxic by-product allyl alcohol, increased side reactions, and capping rate Reduce and other problems, achieve the effect of high end-capping rate, fast reaction speed and high end-capping rate

Inactive Publication Date: 2014-03-12
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 1. The products are mainly polyol allyl ethers with low molecular weight, and the molecules do not contain polyoxyethylene polyoxypropylene ether segments, such as trimethylolpropane allyl ether and trimethylolpropane diallyl ether , Pentaerythritol triallyl ether, etc., are not suitable for methallyl capping of high molecular weight polyethers;
[0008] 2. Phase transfer catalysts, solvents, etc. need to be used in the reaction, and as the reaction progresses, the by-product water produced by the reaction of polyols with sodium hydroxide and potassium hydroxide cannot be removed, side reactions increase, and the end-capping rate decreases, often It is necessary to increase the end-capping agent to increase the end-capping rate, and excessive allyl chloride and sodium (potassium) hydroxide will generate a highly toxic by-product allyl alcohol;
[0009] 3. This method is only suitable for polyols with primary hydroxyl groups at the end, and for molecules containing polyoxypropylene ethers, because the ends are secondary hydroxyl groups with poor reactivity, the secondary hydroxyl groups cannot be polyoxypropylene ethers in this way. Synthesis of products

Method used

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  • Method for synthesizing trimethyl allyl polyoxypropylene ether
  • Method for synthesizing trimethyl allyl polyoxypropylene ether
  • Method for synthesizing trimethyl allyl polyoxypropylene ether

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Add 1000 grams of glycerol polyoxypropylene ether (n=10, molecular weight about 1994) and 97.5 grams of solid sodium methoxide into the 2L reaction kettle. 0.09~-0.1MPa) methanol removal (removal of methanol is accompanied by the whole process of alkoxide reaction, and alkoxide is generated while removing methanol), and alkoxide reaction is carried out for 3 hours; the temperature is lowered to 70~80℃, and 177.0 grams of methyl Allyl chloride was maintained at a pressure of 0.3 MPa, continued to react for 4 hours, and the end-capping reaction was completed; excess methallyl chloride was recovered by distillation under reduced pressure, and the crude product was adsorbed and filtered by a polyether refining adsorbent to obtain a refined product.

Embodiment 2

[0042] Add 1000 grams of glycerol polyoxyethylene ether (n=45, molecular weight about 8084) and 30.1 grams of sodium methoxide into the 2L reaction kettle. After stirring, the temperature is controlled at 110~120℃, under vacuum conditions (pressure-0.09 ~-0.1MPa) methanol removal, alkoxide reaction for 3 hours; cooling to 80 ~ 90 ℃, feeding 53.7 grams of methallyl chloride, maintaining the pressure of 0.3Mpa, continuing the reaction for 5 hours, the end capping reaction is over; decompression Excess methallyl chloride is recovered by distillation, and the crude product is adsorbed and filtered by a polyether refining adsorbent to obtain a refined product.

Embodiment 3

[0044] Add 1000 grams of glycerol polyoxypropylene ether (n=85, molecular weight about 15044), 64.7 grams of liquid sodium methoxide (30% sodium methoxide methanol solution) into the 2L reaction kettle, stir evenly, and control the temperature at 120~130℃ , under vacuum conditions (pressure -0.09~-0.1MPa), methanol was removed, and the alkoxide reaction was carried out for 4 hours; the temperature was lowered to 90~100℃, 34.3 grams of methallyl chloride was introduced, the pressure was maintained at 0.3Mpa, and the reaction was continued for 5 hours , the end-capping reaction ends; the excess methallyl chloride is recovered by distillation under reduced pressure, and the crude product is adsorbed and filtered by a polyether refining adsorbent to obtain a refined product.

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Abstract

The invention relates to a method for synthesizing trimethyl allyl polyoxypropylene ether, belonging to the field of alkyl-terminated polyether preparation technologies. The method comprises an alcohol salinization reaction, a terminating reaction and a refining process, namely adding triol polyoxypropylene ether and an alcohol salinization reagent into a reactor, uniformly stirring, then, controlling the temperature and pressure of alcohol salinization, carrying out the alcohol salinization reaction, removing byproducts after the reaction, then, terminating a remaining product, and refining a terminated crude product so as to remove byproducts, thereby obtaining a final product. By adopting the method disclosed by the invention, the phenomenon of the conventional one-step reaction processes that side reactions are increased due to moisture produced during alcohol salinization reaction is avoided, and the problems that secondary hydroxyl polyether is contained, the reaction activity of high-molecular-weight polyether is poor and the termination rate is low are solved.

Description

technical field [0001] The invention relates to a method for synthesizing trimethylallyl polyoxypropylene ether, and belongs to the technical field of preparation of alkyl-terminated polyether. Background technique [0002] The trimethylallyl polyether molecule is the product generated after the triol polyoxypropylene ether is capped with methallyl, and has the following general formula: [0003] [0004] where R can be etc., n is usually a positive integer ≤ 100, [0005] Since the trimethylallyl polyether molecule contains 3 methylallyl groups with high reactivity, it is an ideal crosslinking agent for polymerization, and its molecular structure has good flexibility, so it is very suitable for modification It can be used to prepare reticulated silicones with different characteristics, so that it can be used in a wider range of applications, so it can be used as a building sealant with excellent comprehensive performance. Trimethylallyl polyether products have broad m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/337C08G65/331
Inventor 郭晓峰金一丰王胜利陈英杰张美军
Owner ZHEJIANG HUANGMA TECH
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