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Method for synthetizing diallyl polyether

The technology of a bisallyl polyether and its synthesis method is applied in the field of synthesis of bisallyl polyether, which can solve the problems of low capping rate and poor reactivity, and achieve high capping rate, low cost and excellent production process. simple effect

Inactive Publication Date: 2012-06-20
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It solves the problem of poor reactivity and low capping rate of polyethers containing secondary hydroxyl groups, especially high molecular weight polyethers
The choice of alkoxide reagent not only solves the problem of the by-product of allyl alcohol, which is a highly toxic drug, in the conventional allylation process, but also makes the product have a higher end-capping rate

Method used

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  • Method for synthetizing diallyl polyether
  • Method for synthetizing diallyl polyether
  • Method for synthetizing diallyl polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 1,000 grams of allyl alcohol polyoxyethylene ether (m=20, n=0, molecular weight about 940) and 63.2 grams of solid sodium methoxide into a 2L reactor, and stir vigorously. The temperature is 90~100℃, under vacuum condition (pressure -0.09~-0.1MPa) to remove methanol, and react for 3 hours. Cool down to 60-70°C, slowly introduce 97.7 g of allyl chloride, maintain the pressure at 0.3 MPa, and continue the reaction for 4 hours. Excess allyl chloride is recovered by distillation under reduced pressure, and the end-capped polyether product is obtained after filtering to remove solid impurities. This embodiment solves the problems of poor reactivity and low end capping rate of high molecular weight polyether. The selection of the alkoxide reagent not only solves the problem of the by-product of the highly toxic allyl alcohol in the conventional allylation process, but also makes the product have a higher end-capping rate.

Embodiment 2

[0036] Add 1,000 grams of allyl alcohol polyoxyethylene ether (m=40, n=0, molecular weight about 1820) and 35.6 grams of sodium methoxide into a 2L reactor, and stir vigorously. The temperature is 100~110℃, under vacuum conditions (pressure -0.09~-0.1MPa) to remove methanol, and react for 3 hours. Cool down to 60-70°C, slowly introduce 54.6 g of allyl chloride, maintain the pressure at 0.3 Mpa, and continue the reaction for 4 hours. Excess allyl chloride is recovered by distillation under reduced pressure, and the end-capped polyether product is obtained after filtering to remove solid impurities. This embodiment solves the problems of poor reactivity and low end capping rate of high molecular weight polyether. The selection of the alkoxide reagent not only solves the problem of the by-product of the highly toxic allyl alcohol in the conventional allylation process, but also makes the product have a higher end-capping rate.

Embodiment 3

[0038] Add 1,000 grams of allyl alcohol polyoxypropylene ether (m=0, n=80, molecular weight about 4700), 16.1 grams of solid sodium methoxide into a 2L reactor, and stir vigorously. The temperature is 110~120℃, under vacuum condition (pressure -0.09~-0.1MPa) to remove methanol, and react for 3 hours. Cool down to 80-90°C, slowly introduce 24.4 g of allyl chloride, maintain the pressure at 0.3 Mpa, and continue the reaction for 5 hours. Excess allyl chloride is recovered by distillation under reduced pressure, and the end-capped polyether product is obtained after filtering to remove solid impurities. This embodiment solves the problems of poor reactivity and low end capping rate of polyethers containing secondary hydroxyl groups, especially high molecular weight polyethers. The selection of the alkoxide reagent not only solves the problem of the by-product of the highly toxic allyl alcohol in the conventional allylation process, but also makes the product have a higher end-ca...

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Abstract

The invention discloses a method for synthetizing diallyl polyether. A polymerization product which is prepared from ethylene oxide and propylene oxide by using allyl alcohol as a starting agent is polyether with the following general formula (I). The method is carried out according to the following process steps of: 1, adding an alkoxidation reagent into the polyether to perform alkoxidation reaction and removing methanol generated during the reaction; 2, then filling allyl chloride into a reaction kettle to continuously perform the reaction, wherein the charging molar ratio of the polyether to the allyl chloride is 1: (1.0-2.0) and a by-product is sodium chloride or potassium chloride; and 3, refining the product, i.e. firstly, distilling and recovering the unreacted allyl chloride and then filtering a crude product to obtain the refined product. The problems of poor reaction activity and low yield of termination of polyether containing a secondary hydroxyl group, particularly high molecular weight polyether are solved. Due to the selection of the alkoxidation reagent, not only is the problem of generating a highly toxic allyl alcohol by-product in the conventional allylation process solved, but also the product has high yield of termination.

Description

technical field [0001] The invention relates to a method for synthesizing bisallyl polyether. It belongs to the technical field of preparation of alkyl-terminated polyether. Background technique [0002] The middle part of the molecular chain of bisallyl polyether is polyoxyethylene polyoxypropylene ether, and the two ends of the molecular chain are allyl groups. It has the following general formula: [0003] m+n≤200 [0004] Due to the highly reactive allyl groups at both ends of the molecule, it is an ideal crosslinking agent for polymerization reactions. When m=0, it is bisallyl polyoxypropylene ether, and the molecule has good flexibility. It is especially suitable for modifying network-shaped water-based silicone with different characteristics. It can be used in building sealants with excellent comprehensive performance. There are two technical routes of silicon-modified polyether and silicon-modified polyurethane for the preparation of adhesives and sealants by ...

Claims

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Application Information

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IPC IPC(8): C08G65/337C08G65/331C08G65/28
Inventor 金一丰郭晓锋王胜利马定连谢专
Owner ZHEJIANG HUANGMA TECH
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