Method for synthesizing polymer of terminal hydroxy ethylene liquid

A technology of liquid polymer and hydroxy-terminated ethylene, applied in the field of liquid polymer synthesis, can solve problems affecting product polymerization, side reactions, etc., and achieve the effects of good repeatability, low cost and simple polymerization process

Inactive Publication Date: 2003-07-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In 1978, there was a second report in Puyou that the reaction between maleic anhydride and carboxyl-terminated liquid polybutadiene was used to prepare hydroxyl-terminated vinyl liquid polybutadiene, but the conversion rate of the terminal group was only 85%. It may be because the unsaturated bonds in polybutadiene are prone to side reactions with maleic anhydride, which will seriously affect the further polymerization of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve 10.0g potassium hexacyanocobaltate in 200ml deionized water to obtain 0.16mol / l potassium hexacyanocobaltate solution; dissolve 20.0g zinc chloride in 40ml deionized water to obtain 3.67mol / l zinc chloride solution; uniformly mix zinc chloride solution and potassium hexacyanocobaltate solution under vigorous stirring to obtain zinc hexacyanocobaltate precipitate. After the precipitation is separated, it is washed 3 times with deionized water, 200ml each time, and the washed precipitate is dried to constant weight under vacuum; the dried precipitate is placed in a closed container filled with ethylene glycol diethyl ether gas, and the precipitate Stand until constant weight to obtain zinc hexacyanocobaltate ethylene glycol diethyl ether double metal complex catalyst.

[0019] Add 100g of hydroxyl-terminated tetrahydrofuran-propylene oxide liquid copolyether (hydroxyl value 129), 40g of maleic anhydride and 0.03g of zinc hexacyanocobaltate ethylene glycol diethyl...

Embodiment 2

[0021] In a dry 1-liter autoclave, add 100 g of hydroxyl-terminated epichlorohydrin liquid polyether (hydroxyl value 160), 85 g of maleic anhydride and 0.035 g of zinc hexacyanocobaltate ethylene glycol diethyl ether double metal complex catalyst , after nitrogen replacement, adjust the temperature of the kettle to 120°C, start electromagnetic stirring, inject 20g propylene oxide and 40g ethylene oxide after 2 hours, react for 6 hours, remove unreacted monomers and condensation products under reduced pressure, and discharge Then record the weight of the obtained polymer. A polyether ester diol with a hydroxyl value of 57 was obtained with a yield of 100%.

Embodiment 3

[0023] In dry 1-liter autoclave, add 100g polypropylene oxide ether glycol (hydroxyl value 160), 60g maleic anhydride and 0.04g zinc hexacyanocobaltate ethylene glycol diethyl ether double metal complex catalyst, After nitrogen replacement, adjust the temperature of the kettle to 160°C, start electromagnetic stirring, inject 71g of butylene oxide and 71g of epichlorohydrin after 2 hours, react for 3 hours, remove unreacted monomers and condensation products under reduced pressure, and discharge Then record the weight of the obtained polymer. The polyether ester diol with a hydroxyl value of 55 can be prepared with a yield of 100%.

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PUM

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Abstract

A process for synthesizing hydroxy-terminated vinyl polymer liquid includes such steps as proportionally adding liquid hydroxy-terminal polyether, maleic acid anhydride and catalyst to high-pressure reactor, vacuumizing, filling N2, heating to 50-200 deg.c, adding epoxy compound, and polymerizing for 2-50 hr. Its advantage is high transform rate (100%).

Description

Technical field: [0001] The invention belongs to a method for synthesizing liquid polymers with different types of functional groups at the end, in particular to a method for synthesizing a hydroxyl-terminated vinyl liquid polymer. technical background: [0002] Vinyl liquid polymers are widely used because of their high activity and easy curing characteristics. If there are not only vinyl groups in the molecular chain, but also functional groups at the end groups, you can use vinyl groups, end groups or both. Further reaction with terminal groups to prepare various types of heterophasic copolymers, such as multi-block polymers, graft copolymers, telechelic copolymers, star copolymers, grate copolymers, semi-interpenetrating network copolymers, Graft-type interpenetrating network copolymers, block-type interpenetrating network copolymers, etc. This liquid polymer is therefore a suitable intermediate for the preparation of various heterophasic copolymers. [0003] In 1978, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48
Inventor 王心葵亢茂青王东贤瞿波
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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