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Preparation method of glycidol ether base allyl alcohol polyoxyethylene ether

A technology of allyl alcohol polyoxyethylene ether and allyl alcohol polyoxyethylene ether, which is applied in the field of preparation of glycidyl ether-based allyl alcohol polyoxyethylene ether, can solve the problem of low reaction efficiency, many by-products, and low yield Low-level problems, to achieve the effect of high reaction efficiency, less side reactions, and high yield

Inactive Publication Date: 2011-05-18
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The purpose of the present invention is to provide a novel preparation method of glycidyl ether-based allyl alcohol polyoxyethylene ether to solve the problems of more by-products, lower yield and low reaction efficiency

Method used

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  • Preparation method of glycidol ether base allyl alcohol polyoxyethylene ether
  • Preparation method of glycidol ether base allyl alcohol polyoxyethylene ether
  • Preparation method of glycidol ether base allyl alcohol polyoxyethylene ether

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Add 1,000 g of allyl alcohol polyoxyethylene ether (molecular weight: 410, n=8), 178 g of solid potassium hydroxide, and 250 g of benzene into a 2L reactor, and stir. Raise the temperature to 80-90°C, remove the water through the water separator, reflux the benzene, and react for 2 hours. After the reaction, the benzene is recovered by distillation under reduced pressure. Cool down to 40-50°C, slowly add 294g of epichlorohydrin dropwise, and react for 3 hours after the dropwise addition. The unreacted epichlorohydrin is removed under reduced pressure, and the glycidyl ether-based allyl alcohol polyoxyethylene ether product is obtained after filtering to remove solid impurities.

Embodiment 2

[0046]Add 1,000 g of allyl polyoxyethylene ether (molecular weight: 1158, n=25), 78 g of solid sodium hydroxide, and 100 g of toluene into a 2L reactor, and stir. Raise the temperature to 100-110°C, remove the water through the water separator, reflux the benzene, and react for 3 hours. After the reaction is completed, the benzene is recovered by distillation under reduced pressure. Cool down to 60-70°C, slowly add 128g of epichlorohydrin dropwise, and react for 5 hours after the dropwise addition. The unreacted epichlorohydrin is removed under reduced pressure, and the glycidyl ether-based allyl alcohol polyoxyethylene ether product is obtained after filtering to remove solid impurities.

Embodiment 3

[0048] Add 1000 g of allyl polyoxyethylene ether (molecular weight 2038, n=45), 55 g of a mixture of solid potassium hydroxide and solid sodium hydroxide, and 50 g of a mixture of benzene and toluene into a 2L reactor, and stir. Raise the temperature to 120-130°C, remove the water through the water separator, reflux the benzene, and react for 5 hours. After the reaction is completed, the benzene is recovered by distillation under reduced pressure. Cool down to 80-90°C, slowly add 91 g of epichlorohydrin dropwise, and react for 8 hours after the dropwise addition. The unreacted epichlorohydrin is removed under reduced pressure, and the glycidyl ether-based allyl alcohol polyoxyethylene ether product is obtained after filtering to remove solid impurities.

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Abstract

The invention discloses a preparation method of glycidol ether base allyl alcohol polyoxyethylene ether. In the method, 1 mole of allyl alcohol polyoxyethylene ether and 1.3-2.0 moles of epichlorohydrin as raw materials, and the method comprises the following steps: A) adding solid base and water-carrying agent into the allyl alcohol polyoxyethylene ether, carrying out backflow reaction for 2-5 hours at the temperature of 80-130DEG C, and obtaining an intermediate A after azeotropic dehydration; B) at the temperature of 80-130 DEG C and the pressure of minus 0.09-minus 0.01 MPa, carrying out reduced pressure distillation to recover the water-carrying agent in the intermediate A, dipping the epichlorohydrin, and reacting for 3-8 hours at the temperature of 40-90DEG C to obtain an intermediate B; and C) refining the product: firstly, removing the excessive epichlorohydrin in the intermediate B by distillation, and filtering to obtain the glycidol ether base allyl alcohol polyoxyethylene ether. The reaction system in the preparation method has the characteristics of no moisture, less side reaction, high reaction efficiency, high yield and the like.

Description

technical field [0001] The invention relates to a preparation method of glycidyl ether allyl alcohol polyoxyethylene ether. The invention belongs to the technical field of polyether modification. Background technique [0002] The structural formula of glycidyl ether allyl alcohol polyoxyethylene ether is: [0003] [0004] Glycidyl ether-based allyl alcohol polyoxyethylene ether molecule contains two active groups, allyl group and epoxy group, which have good reactivity. The polyether segment contained in the molecule makes it have low viscosity and good flexibility. features. Silicone surfactant widely used in fine chemical industry, its good water solubility and surface activity is obtained by grafting glycidyl ether allyl alcohol polyoxyethylene ether on hydrogen-silicon bond; in epoxy resin, chemical fiber , Plastic and rubber production are also widely used as additives, solvents, catalysts, crosslinking agents and chain transfer agents; it has important uses in o...

Claims

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Application Information

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IPC IPC(8): C08G65/337C07D303/24C07D301/00
Inventor 王伟松金一丰郭晓锋王新荣张晨辉
Owner ZHEJIANG HUANGMA TECH
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