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A kind of preparation method of high molecular weight diallyl capped polyether

A bisallyl capping and high molecular weight technology is applied in the field of preparation of high molecular weight bisallyl capping polyether, which can solve the problems of reducing the recovery cost of end capping agent, low end capping rate of high molecular weight polyether, etc. The effect of improving the reaction conversion rate, reducing the usage and reducing the cost

Active Publication Date: 2017-05-10
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to provide a preparation method of high molecular weight diallyl capped polyether (molecular weight 6000-10000), which solves the problem of low capping rate of high molecular weight polyether and greatly reduces the recovery of capping agent. cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Add 1000g of allyl alcohol polyoxyethylene ether (m=68, n=0, molecular weight about 3050) and 23.0g of solid potassium methoxide into a 2L reactor, slowly raise the temperature to 70°C, under vacuum conditions (control pressure is - 0.095 ~ -0.1MPa) to remove the methanol generated by the reaction, and the reaction time is 1h to generate allyl alcohol polyoxyethylene ether potassium salt.

[0027] 2) Lower the temperature of step 1) to 60°C, add 32.4 g of 1,2-dichloroethane dropwise to the reaction kettle, after the dropwise addition, control the pressure to 0.0MPa, and the temperature to 60°C, and continue the reaction for 1 hour to obtain diene Propyl-terminated polyoxyethylene ether, the by-product is potassium chloride.

Embodiment 2

[0029] 1) Add 1,000 g of allyl alcohol polyoxypropylene ether (m=0, n=52, molecular weight about 3074) and 45.5 g of solid potassium methoxide into a 2L reactor, slowly raise the temperature to 120°C, and under vacuum conditions (control pressure is -0.095 ~ -0.1MPa), remove the methanol generated by the reaction, the reaction time is 3h, and generate allyl alcohol polyoxypropylene ether potassium salt.

[0030] 2) Lower the temperature of step 1) to 90°C, add 64.4g of 1,2-dichloroethane dropwise to the reactor, after the dropwise addition, control the pressure to 0.4MPa, then raise the temperature to 120°C, and the reaction time is 4h. Diallyl-terminated polyoxypropylene ether is obtained, and the by-product is potassium chloride.

Embodiment 3

[0032] 1) Add 1000 g of allyl alcohol polyoxyethylene polyoxypropylene atactic polyether (m=30, n=30, molecular weight about 3118) and 33.7 g of solid potassium methoxide into a 2L reactor, slowly heat up to 95°C, vacuum Under the conditions (control pressure is -0.095 ~ -0.1MPa), the methanol generated by the reaction is removed, and the reaction time is 2h, and the potassium salt of allyl alcohol polyoxyethylene polyoxypropylene ether is generated.

[0033] 2) Lower the temperature of step 1) to 75°C, add 47.7g of 1,2-dichloroethane dropwise to the reactor, after the dropwise addition, control the pressure to 0.2MPa, then raise the temperature to 90°C, and the reaction time is 2h. Diallyl alcohol polyoxyethylene polyoxypropylene ether is obtained, and the by-product is potassium chloride.

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Abstract

The invention relates to a preparation method for high-molecular weight diallyl-terminated polyether and belongs to the technical field of organic synthesis. Allyl alcohol polyether with the molecular weight of 2986-4986 is taken as a raw material, an alkoxidation reagent is added for reaction, vacuum pumping is performed for removing gas or moisture generated by the reaction, then 1,2-dichloroethane is added for reaction, and the diallyl-terminated polyether with the doubled molecular weight is obtained. The preparation method used for the synthesis of the high-molecular weight diallyl-terminated polyether has the advantages of being simple in production technology, high in yield of termination, low in cost, free of pollution, stable in quality and the like.

Description

technical field [0001] The invention relates to a preparation method of a high-molecular-weight diallyl-terminated polyether, which belongs to the technical field of organic synthesis. Background technique [0002] The middle part of the molecular chain of high molecular weight diallyl-terminated polyether is polyoxyethylene polyoxypropylene ether, and the two ends of the molecular chain are allyl groups. It has the following general formula: [0003] ; For random polyether, the general formula can be simplified as: , wherein: m and n are arbitrary, but must satisfy that the molecular weight range of the bisallyl-terminated polyether is 6000-10000. [0004] Due to the highly reactive allyl groups at both ends of the molecule, it is an ideal crosslinking agent for polymerization reactions. Polyether modified silicone sealant contains both polyether as the main chain and silyl group as the curing functional group. It has many advantages of silicone sealant and polyurethan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/00C08G65/337
CPCY02P20/582
Inventor 陈荧杰金一丰张美军颜吉校
Owner ZHEJIANG HUANGMA TECH
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