Method for preparing glycidol ether terminated propenol polyoxyethylene ether

A technology of terminal allyl alcohol polyoxyethylene ether and terminal allyl polyoxyethylene ether, which is applied in the field of preparation of end-capped polyether, and can solve the problem of many intermediate by-products, affecting product yield, and epoxy group ring-opening. Addition side reactions and other problems, to achieve the effect of high reactivity, convenient and fast purification, and low cost

Active Publication Date: 2010-12-29
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the reported patents, there is almost no glycidyl ether for synthesizing long chains, and there are also problems such as the above-mentioned easy ring-opening addition of epoxy groups to produce side reactions, resulting in more intermediate by-products, which ultimately affect the yield of the product. Rate

Method used

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  • Method for preparing glycidol ether terminated propenol polyoxyethylene ether
  • Method for preparing glycidol ether terminated propenol polyoxyethylene ether
  • Method for preparing glycidol ether terminated propenol polyoxyethylene ether

Examples

Experimental program
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Effect test

Embodiment 1

[0046] In thermometers, condensers, stirrers, N 2 Add 454.8 g of allyl polyoxyethylene ether (produced by Zhejiang Huangma Chemical Group Co., Ltd., molecular weight 454) into the 1000 mL dry four-neck flask at the entrance, vacuum dehydrate at 100 ° C for 30 min, and when the temperature drops to 80 ° C, add the catalyst NaH1. 6g. Add 101.8 g of epichlorohydrin dropwise with a constant pressure dropping funnel for 2 hours. After the addition, continue the reaction for 2 hours. Control the reaction temperature at 80° C. and remove excess epichlorohydrin under reduced pressure. Weigh 40.2g of NaOH and dissolve it in deionized water to form a 40% aqueous solution, add it dropwise to the intermediate of allyl polyoxyethylene chlorohydrin ether, and add it for 2 hours. The reaction was continued for 2 hours. After the reaction was finished, impurities were removed by post-processing such as vacuum distillation and filtration to obtain a capped polyether product. The measured epo...

Embodiment 2

[0048] In thermometers, condensers, stirrers, N 2Add 430.8 g of allyl polyoxyethylene ether (produced by Zhejiang Huangma Chemical Group Co., Ltd., molecular weight 718) into the 1000 mL dry four-neck flask at the entrance, vacuum dehydrate at 100 ° C for 30 min, and when the temperature drops to 70 ° C, add the catalyst NaH2. 0g. Add 66.6 g of epichlorohydrin dropwise with a constant-pressure dropping funnel for 1 hour, and continue the reaction for 3 hours after the addition is complete. Control the reaction temperature at 70° C., and remove excess epichlorohydrin under reduced pressure. Weigh 28.8g of NaOH and dissolve it in deionized water to form a 30% aqueous solution, add it dropwise to the intermediate of allyl polyoxyethylene chlorohydrin ether, the time of adding is 1 hour, control the reaction temperature at 30°C, and the addition is completed The reaction was continued for 3 hours, and after the reaction was completed, after the reaction, the impurities were remov...

Embodiment 3

[0050] In thermometers, condensers, stirrers, N 2 Add allyl polyoxyethylene ether (produced by Zhejiang Huangma Chemical Group Co., Ltd., molecular weight 1158) 463.2g into the 1000mL dry four-necked flask at the entrance, vacuum dehydrate at 100°C for 30min, and when the temperature drops to 55°C, add the catalyst NaH2. 5g. Add 48.1 g of epichlorohydrin dropwise with a constant pressure dropping funnel for 3 hours. After the addition, continue the reaction for 1 hour. Control the reaction temperature at 55° C. and remove excess epichlorohydrin under reduced pressure. Weigh 30.2g of KOH and dissolve it in deionized water to form a 40% aqueous solution, and add it dropwise to the intermediate of allyl polyoxyethylene chlorohydrin ether. The dropping time is 3 hours, and the reaction temperature is controlled at 45°C. The reaction was continued for 1 hour. After the reaction was finished, impurities were removed by post-processing such as vacuum distillation and filtration to ...

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Abstract

The invention discloses a method for preparing glycidol ether terminated propenol polyoxyethylene ether, which comprises the following steps of: mixing commercial allyl polyoxyethylene ether and epoxy chloropropane serving as raw materials, performing ring opening reaction on the mixture by adopting NaH as a catalyst to generate an allyl polyoxyethylene chlorohydrine ether intermediate, then removing redundant epoxy chloropropane with reduced pressure, adding inorganic alkali into the allyl polyoxyethylene chlorohydrine ether intermediate, and performing ring closing reaction to prepare the glycidol ether terminated propenol polyoxyethylene ether. The method has the characteristics of high reaction speed and high termination efficiency.

Description

technical field [0001] The invention relates to a preparation method of glycidyl ether group-capped allyl alcohol polyoxyethylene ether, which belongs to the technical field of capped polyether preparation. Background technique [0002] The structural formula of glycidyl ether group-terminated allyl alcohol polyoxyethylene ether is: [0003] [0004] Glycidyl ether-terminated allyl alcohol polyoxyethylene ether is an epoxy compound with a flexible chain segment. Because the molecule contains active unsaturated double bonds and epoxy groups, it has good reactivity and activity. The polyether chain segment contained has the characteristics of low viscosity and good flexibility. Therefore, glycidyl ether-blocked allyl alcohol polyoxyethylene ether is widely used in epoxy reactive diluents, crosslinking agents and chain transfer agents, chloride stabilizers, fabric finishing agents, modified silicone oils, etc. A multipurpose fine chemical product. [0005] At present, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/00C07D303/24C07D301/26
Inventor 王伟松金一丰郭晓锋王新荣陶彭均
Owner ZHEJIANG HUANGMA TECH
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