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A kind of synthetic method of hyperbranched polytetrahydrofuran

A technology of tetrahydrofuran and hyperbranched polymerization, which is applied in the field of new rare earth metal catalysts, can solve the problems such as the synthesis report of hyperbranched polytetrahydrofuran that has not yet been reported, and achieves the effects of improving toughness, high tensile properties and high catalytic activity.

Active Publication Date: 2018-05-22
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] There is no report on the synthesis of hyperbranched polytetrahydrofuran

Method used

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  • A kind of synthetic method of hyperbranched polytetrahydrofuran
  • A kind of synthetic method of hyperbranched polytetrahydrofuran
  • A kind of synthetic method of hyperbranched polytetrahydrofuran

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] At room temperature, Lu(OTf) 3 (0.0647g, 0.104mmol), 1.5ml THF (1.312g, 18.2mmol) were successively added to a 20ml long-necked tube, and 0.1ml initiator ethylene glycol diglycidyl ether (0.0894g, 0.513mmol) and 3.5ml THF (3.086g, 42.791mmol) was added to another 20ml long-necked tube, and the reagents in the two long-necked bottles were shaken to fully dissolve. Use a syringe to extract 0.2ml of the solution from the long-necked tube containing the initiator and add it to the long-necked tube containing the catalyst. tube. The molar ratio of catalyst, initiator and THF is 1:0.3:200. Seal the long-necked tube with a flame, and place it at a constant temperature of 25°C for reaction. After 2 hours, cut the mouth of the long-necked tube to terminate the reaction, add an appropriate amount of THF to the polymerization system to dilute the polymer, precipitate it in cold n-hexane, pour out the supernatant after fully standing, and dry it in a vacuum drying oven to constan...

Embodiment 2

[0052] Other polymerization conditions are the same as in Example 1, except that vinyl dioxide cyclohexene is used as an initiator to initiate the ring-opening polymerization of THF, and the molar ratio of catalyst, initiator and THF is 1:0.1:2000. Constant temperature at 80°C After reacting in the tank for 1 h, the yield of polytetrahydrofuran obtained was 72%. The molecular weight is 355KDa.

Embodiment 3

[0054] Other polymerization conditions are the same as in Example 1, except that polyethylene glycol dioxirane methyl ether is used as an initiator to initiate the ring-opening polymerization of THF, and the mol ratio of catalyst, initiator and THF is 1:0.3: 200. Reacted in a constant temperature bath at 0°C for 2 hours, the yield of polytetrahydrofuran obtained was 64%, and the molecular weight was 232KDa.

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Abstract

The invention discloses a method for synthesizing hyperbranched polytetrahydrofuran through catalysis of rare earth catalysts. Hydroboration, alkoxy rare earth, aryloxy rare earth, trifluoromethanesulfonic acid rare earth, substituted benzoic acid rare earth, carboxylic acid rare earth and halogenation rare earth are adopted as catalysts, a compound containing poly epoxy groups is adopted as an initiator for catalyzing tetrahydrofuran for ring opening polymerization, under the temperature of 30-80 DEG C, a reaction is performed for 5 min to 5 d, and hyperbranched polytetrahydrofuran is prepared. The adopted rare earth catalysts are wide in application range, the price is low, preparation is easy, the high catalytic activity is achieved, the molecular weight of the obtained polytetrahydrofuran can reach up to hundreds of thousands, the degree of polymerization can reach up to thousands to tens of thousands, and the degree of branching is controllable.

Description

technical field [0001] The present invention relates to seven types of new rare earth metal catalysts: borohydride rare earth catalysts, alkoxy rare earth catalysts, aryloxy rare earth catalysts, trifluoromethanesulfonic acid rare earths, substituted benzoic acid rare earths, carboxylic acid rare earths and halogenated rare earths, involving fifteen types Polyepoxy compound initiator, and the synthetic method of hyperbranched polytetrahydrofuran. Background technique [0002] Polytetrahydrofuran is a product produced by cationic ring-opening polymerization of tetrahydrofuran, and its structural formula is HO(CH 2 CH 2 CH 2 CH 2 O) n H, its chain body is mainly composed of carbon chain and ether chain, has hydrolysis resistance, and its products have excellent physical and mechanical properties. The glass transition temperature of polytetrahydrofuran is low, which is -76 ° C. Its physical properties are mainly determined by molecular weight. At room temperature, polytetr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/20
CPCC08G65/20C08G2650/24
Inventor 凌君李瑶白天闻李逸凡黄雁鑫
Owner ZHEJIANG UNIV