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Polyethylene glycol monomethyl ether-polybutadiene-polyethylene glycol monomethyl ether triblock copolymer and preparation method thereof

A technology of polyethylene glycol monomethyl ether and polybutadiene, which is applied in the field of polymer synthesis and modification, can solve the problems of weak molecular polarity, achieve the goal of increasing the polarity level, meeting performance requirements, and mild reaction conditions Effect

Active Publication Date: 2021-09-14
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the above technical problems, the object of the present invention is to provide polyethylene glycol monomethyl ether-polybutadiene-polyethylene glycol monomethyl ether triblock copolymer and preparation method thereof, to overcome polybutadiene product molecular polarity Due to the inherent deficiency of weak property, it is proposed to use polybutadiene with terminal hydroxyl group as the starting material, and insert the poly(ethylene glycol monomethyl ether) segment with a higher polarity level into its two ends to form polyethylene glycol monomethyl ether- Polybutadiene-polyethylene glycol monomethyl ether triblock copolymer

Method used

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  • Polyethylene glycol monomethyl ether-polybutadiene-polyethylene glycol monomethyl ether triblock copolymer and preparation method thereof
  • Polyethylene glycol monomethyl ether-polybutadiene-polyethylene glycol monomethyl ether triblock copolymer and preparation method thereof
  • Polyethylene glycol monomethyl ether-polybutadiene-polyethylene glycol monomethyl ether triblock copolymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) 50g hydroxyl-terminated polybutadiene (M n =2000g / mol, 25mmol) was dissolved in anhydrous tetrahydrofuran, and 11.85g of pyridine (150mmol) was added to the system. After mixing evenly, the system was moved into an ice-water bath, and when the temperature was stabilized, 13.58 g of acryloyl chloride (150 mmol) was slowly added dropwise to the system. After the dropwise addition, react in an ice-water bath for 1 hour, then move to room temperature and continue to react for 7 hours.

[0031] (2) After the reaction, filter with suction and evaporate the solvent to dryness, dissolve the crude product in dichloromethane, and wash with saturated sodium bicarbonate solution and deionized water successively. Use anhydrous magnesium sulfate to dry the organic phase, filter with suction, and evaporate the solvent to obtain an intermediate product of acrylate-based polybutadiene.

[0032] (3) Mix 50g of acrylate-based polybutadiene (25mmol) with 50g of amino polyethylene gly...

Embodiment 2

[0034] (1) 50g hydroxyl-terminated polybutadiene (M n =5000g / mol, 10mmol) was dissolved in anhydrous tetrahydrofuran, and 11.85g of pyridine (150mmol) was added to the system. After mixing evenly, the system was moved into an ice-water bath, and when the temperature was stabilized, 9.05 g of acryloyl chloride (100 mmol) was slowly added dropwise to the system. After the dropwise addition, react in an ice-water bath for 1 hour, then move to room temperature and continue to react for 24 hours.

[0035] (2) After the reaction, filter with suction and evaporate the solvent to dryness, dissolve the crude product in dichloromethane, and wash with saturated sodium bicarbonate solution and deionized water successively. Use anhydrous magnesium sulfate to dry the organic phase, filter with suction, and evaporate the solvent to obtain an intermediate product of acrylate-based polybutadiene.

[0036] (3) Mix 50g acrylate-based polybutadiene (10mmol) with 40g amino polyethylene glycol mo...

Embodiment 3

[0038] (1) 50g hydroxyl-terminated polybutadiene (M n =1000g / mol, 50mmol) was dissolved in anhydrous dichloromethane, and 10.12g triethylamine (100mmol) was added into the system. After mixing evenly, the system was moved into an ice-water bath, and when the temperature was stabilized, 9.05 g of acryloyl chloride (100 mmol) was slowly added dropwise to the system. After the dropwise addition, react in an ice-water bath for 1 hour, then move to room temperature and continue to react for 1 hour.

[0039] (2) After the reaction, filter with suction and evaporate the solvent to dryness, dissolve the crude product in dichloromethane, and wash with saturated sodium bicarbonate solution and deionized water successively. Use anhydrous magnesium sulfate to dry the organic phase, filter with suction, and evaporate the solvent to obtain an intermediate product of acrylate-based polybutadiene.

[0040] (3) Mix 50g acrylate-based polybutadiene (50mmol) with 100g amino polyethylene glycol...

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Abstract

The invention relates to a polyethylene glycol monomethyl ether-polybutadiene-polyethylene glycol monomethyl ether triblock copolymer and a preparation method thereof. This kind of tri-block copolymer is prepared from hydroxyl-terminated polybutadiene through acylation reaction and Michael addition reaction sequentially. First, the terminal hydroxyl groups of hydroxyl-terminated polybutadiene are modified into acrylate groups by acryloyl chloride, and then polyethylene glycol monomethyl ether is prepared by Michael addition reaction between acrylate-based polybutadiene Glycol monomethyl ether-polybutadiene-polyethylene glycol monomethyl ether triblock copolymer. The incorporation of polar polyethylene glycol monomethyl ether segments can effectively increase the molecular polarity of polybutadiene products and improve their application properties. The preparation method proposed by the invention has mild conditions, high reaction efficiency and easy realization of large-scale production.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis and modification, in particular to a polyethylene glycol monomethyl ether-polybutadiene-polyethylene glycol monomethyl ether triblock copolymer and a preparation method thereof. Background technique [0002] Polybutadiene is widely used in rubber products, adhesives, polyurethane soft segments, resin toughening and other fields due to its excellent low temperature performance, mechanical properties and processing characteristics. However, since all polybutadiene structures are non-polar groups, there is an inherent deficiency that the polarity of the main chain of the molecule is weak. In some application fields, polybutadiene resin cannot be effectively compatible with some polar functional components, which eventually leads to a decrease in the performance of the product. Therefore, improving the polarity of polybutadiene molecules through effective chemical means is an important way ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/02C08F8/10C08F136/00
CPCC08F8/10C08G81/025C08F136/06
Inventor 张万斌张光华罗杰王艳蒙
Owner SHAANXI UNIV OF SCI & TECH