Preparation method of unsaturated polyether

A technology of unsaturated polyether, applied in the field of preparation of unsaturated polyether, can solve the problem of high by-products of unsaturated polyether, achieve the effect of low by-products, high purity, and eliminate the formation of by-products

Active Publication Date: 2017-04-26
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Aiming at the above-mentioned defects in the existing polyether synthesis, this application provides a method for preparing unsaturated polyether with reasonable process, safe operation and good performance, especially to solve the problem of high by-products in unsaturated polyether question

Method used

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  • Preparation method of unsaturated polyether

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Embodiment 1: the synthesis of allyl alcohol polyoxyethylene ether 500

[0037] Add 168 parts of allyl alcohol and 0.45 parts of potassium hydroxide into the reaction kettle, raise the temperature to 88°C for azeotropic distillation and dehydration until the water content reaches 120ppm and stop dehydration. Start stirring and heat up to the reaction temperature of 95-100°C, add 1332 parts of ethylene oxide dropwise, control the reaction pressure at 0.05-0.20Mpa, after the dropwise addition of ethylene oxide is complete, continue the reaction for 1 hour, cool down to 70°C and inject for post-treatment kettle, add phosphoric acid to neutralize, polyether adsorbent treatment, and filter to obtain the product.

Embodiment 2

[0041] (1) Synthesis of allyl alcohol polyoxyethylene polyoxypropylene ether oligomer 400:

[0042] Add 200 parts of allyl alcohol and 0.72 parts of sodium hydroxide into the reaction kettle, raise the temperature to 88°C for azeotropic distillation and dehydration until the water content reaches 110ppm and stop dehydration. Start stirring and heat up to the reaction temperature of 100-105°C, add 662 parts of ethylene oxide and 444 parts of propylene oxide dropwise, control the reaction pressure at 0.20-0.30Mpa, complete the dropwise addition of ethylene oxide and propylene oxide, and continue the reaction for 2 Hours, the temperature was lowered to 70°C.

[0043] (2) Synthesis of allyl alcohol polyoxyethylene polyoxypropylene ether 1500:

[0044] Add 3.00 parts of sodium hydroxide and 400 parts of allyl alcohol polyoxyethylene polyoxypropylene oligomer 400 synthesized in step (1) in the reactor, seal the reactor, first use nitrogen to blow and replace, then vacuumize, repeat...

Embodiment 3

[0048] (1) Synthesis of methallyl alcohol polyoxyethylene polyoxypropylene ether oligomer 400: add 200 parts of methallyl alcohol and 0.72 part of sodium hydroxide in the reaction kettle, heat up to 91°C for azeotropic rectification dehydration, Stop dehydration until the moisture reaches 110ppm. Start stirring and heat up to the reaction temperature of 100-105°C, add 860 parts of ethylene oxide and 369 parts of propylene oxide dropwise, control the reaction pressure at 0.20-0.30Mpa, complete the dropwise addition of ethylene oxide and propylene oxide, and continue the reaction for 2 Hours, the temperature was lowered to 70°C.

[0049] (2) Synthesis of methallyl alcohol polyoxyethylene polyoxypropylene ether 3000: add 3.80 parts of sodium hydroxide and 200 parts of methallyl alcohol polyoxyethylene polyoxypropylene low in the reaction kettle synthesized in step (1) Polymer 400, seal the reactor, first use nitrogen to blow and replace, then vacuumize, repeat the replacement tw...

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Abstract

The invention relates to a preparation method of unsaturated polyether and belongs to the technical field of polymer synthesis. The preparation method comprises: using an unsaturated alcohol as an initiator, adding first catalyst, subjecting the unsaturated alcohol to azeotropic dewatering with water generated by reaction, and adding ethylene oxide, propylene oxide or their mixture to carry out ring-opening copolymerization to obtain unsaturated polyether intermediate oligomer having molecular weight of 300-500; adding second catalyst, subjecting the intermediate oligomer to polycondensation with ethylene oxide and propylene oxide to form the finished unsaturated polyether having molecular weight of 300-500. The application is applied to the synthesis of unsaturated polyether, and the preparation method has the advantages of high purity, low byproduct content and the like.

Description

technical field [0001] The invention relates to a preparation method of unsaturated polyether, which belongs to the technical field of high polymer synthesis. Background technique [0002] The polyether obtained by reacting the alcohol containing unsaturated double bond as the initiator with epoxy monomer such as ethylene oxide (EO) and propylene oxide (PO) is an unsaturated polyether. Alcohols containing unsaturated double bonds include allyl alcohol, methallyl alcohol, and the like. [0003] The main use of unsaturated polyether is to use its unsaturated double bond to react with hydrogen-containing silicone oil to prepare polyether-modified silicone surfactant: [0004] [0005] The polyether structures used in the hydrosilylation reaction are different, and polyether-modified silicones with different molecular structures are obtained. At present, allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene atactic polyether and methallyl alcohol polyoxyethyle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/2696
Inventor 万庆梅金一丰余渊荣王月芬刘佳
Owner ZHEJIANG HUANGMA TECH
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