Preparation method of butyl-terminated allyl polyether

A technology of allyl polyether and butyl polyether, which is applied in the field of preparation of butyl-terminated allyl polyether, can solve the problems of by-products, low butyl-terminated rate, poor reactivity, etc. The effect of fast speed, high end capping rate and high reactivity

Inactive Publication Date: 2012-02-22
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solve the problem of poor reactivity of halogenated butyl to secondary hydroxyl-containing polyethers, especially high molecular weight polyethers, and low butyl end-capping rate
The selection of a new type of 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

Method used

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  • Preparation method of butyl-terminated allyl polyether
  • Preparation method of butyl-terminated allyl polyether
  • Preparation method of butyl-terminated allyl polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 1000 grams of butanol polyoxypropylene ether (m=0, n=80, molecular weight about 4700) and 16.1 grams of solid sodium methoxide into a 2L reactor, and stir vigorously. The temperature is 100-110°C, under vacuum conditions (pressure -0.09--0.1MPa) and demethanol is reacted at the same time, and the reaction is 3 hours. Cool down to 60-70°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.

Embodiment 2

[0026] Add 1,000 grams of butanol block polyether (m=40, n=40, polyether propylene oxide end, molecular weight about 4150), 18.2 grams of sodium methoxide into a 2L reactor, and stir vigorously. The temperature is 100-110°C, the reaction is under vacuum conditions (pressure -0.09--0.1MPa) and the methanol is released at the same time, and the reaction is 3 hours. The temperature was lowered to 60-70° C., and 27.7 g of allyl chloride was slowly added dropwise under normal pressure, and the reaction was continued 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.

Embodiment 3

[0028] Add 1000 grams of butanol random polyether (m=20, n=20, molecular weight about 2120) and 30.6 grams of solid sodium methoxide into a 2L reactor, and stir vigorously. The temperature is 100-110°C, under vacuum conditions (pressure -0.09--0.1MPa) and demethanol is reacted at the same time, and the reaction is 2 hours. The temperature was lowered to 60-70° C., and 46.9 g of allyl chloride was slowly added dropwise under normal pressure, and the reaction was continued 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.

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Abstract

The invention discloses a preparation method of butyl-terminated allyl polyether. The method is characterized in that: butyl polyether and halogenated propylene are employed as the raw materials for reaction, and the butyl polyether has the following general formula (1), wherein, m+n is less than 80; the prepared alkyl-terminated polyether has the following general formula (2), wherein, m+n is less than 80; an alkoxidation reagent is added into the butyl polyether for reaction, with the butyl polyether and the alkoxidation reagent in a feeding mole ratio of 1:1-1.5; then allyl chloride is introduced for reaction continuously so as to obtain butyl-terminated allyl polyether, with the butyl polyether and allyl chloride in a feeding ratio of 1:1-1.5. The method of the invention can prepare butyl-terminated allyl polyether products of high termination efficiency which is higher than that of butyl-terminiated polyether prepared by existing preparation methods.

Description

technical field [0001] The invention relates to a preparation method of butyl-terminated allyl polyether. Background technique [0002] Butyl-terminated allyl polyether is a silicone modifier with excellent performance. Since the hydroxyl group in the molecular chain is replaced by butyl, it is oil-soluble and high-temperature-resistant compared with allyl polyether containing hydroxyl groups. , acid and alkali resistance, foam suppression and other abilities have been improved, with unique functions. The silicone modified by butyl-terminated allyl polyether can be used in the oil agent for high-speed spinning of chemical fibers; it can also be used as an additive in high-temperature-resistant lubricating oil or heat-conducting oil; it can also be used in strong alkali In detergent formulations; in addition, it is an excellent cell opener and foam stabilizer in the polyurethane industry. [0003] At present, the preparation method of butyl-terminated allyl polyether is usu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/329
Inventor 郭晓锋金一丰王胜利王月芬余建新
Owner ZHEJIANG HUANGMA TECH
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