Hyperbranched polythioether preparation method

A technology of polysulfide and thiol, which is applied in the field of preparation of hyperbranched polysulfide, can solve the problems of few types of monomers, prone to cross-linking, poor selectivity, etc. Highly controllable effect

Active Publication Date: 2018-02-27
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But AB 2 There are fewer types of monomers of type A, and most of them require complex organic synthesis processes; while A 2 +B 3 The polymerization system is prone to cross-linking due to poor selectivity during the reaction

Method used

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  • Hyperbranched polythioether preparation method
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  • Hyperbranched polythioether preparation method

Examples

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Effect test

Embodiment example 1

[0023] 9.965g (25mmol) 2-ethylglycerol trimercaptopropionate, 75mL tetrahydrofuran and 5.355g (25mmol) 3-(acryloyloxy)-methacrylic acid-2-hydroxypropyl ester and 0.1265g (1.25 mmol) triethylamine was added to the reactor at one time, and N at 40°C 2 Protect the reaction for 48 hours; after the reaction, the reaction solution was concentrated by rotary evaporation, redissolved in chloroform and precipitated in anhydrous ether, and the dissolution-precipitation operation was repeated 3 times, and the precipitate was vacuum-dried to obtain a colorless viscous liquid product hyperbranched polysulfide (12.68 g, 82.8% yield).

[0024] figure 2 It is the infrared absorption spectrogram of the hyperbranched polysulfide prepared in Example 1, wherein the 3505cm-1 place is the stretching vibration absorption peak of OH, the 2540cm-1 place is the characteristic absorption peak of thiol, and the double bond characteristic at 1600cm-1 place The peaks disappeared completely, proving the ...

Embodiment example 2

[0028] 9.965g (25mmol) 2-ethylglycerol trimercapto propionate, 75mL dioxane and 5.355g (25mmol) 3-(acryloyloxy)-methacrylic acid-2-hydroxypropyl ester and 0.1265 g (1.25mmol) triethylamine was added to the reactor at one time, and N at 40°C 2 Protect the reaction for 48 hours; after the reaction, the reaction solution was concentrated by rotary evaporation, redissolved in chloroform and precipitated in anhydrous ether, and the dissolution-precipitation operation was repeated 3 times, and the precipitate was vacuum-dried to obtain a colorless viscous liquid product hyperbranched polysulfide (12.44 g, 81.2% yield).

Embodiment example 3

[0030] 10.961g (27.5mmol) 2-ethylglycerol trimercaptopropionate, 75mL tetrahydrofuran and 5.355g (25mmol) 3-(acryloyloxy)-methacrylic acid-2-hydroxypropyl ester and 0.1265g ( 1.25mmol) triethylamine is added in the reactor at one time, and under 40 ℃, N 2 Protect the reaction for 24 hours; after the reaction, the reaction solution was concentrated by rotary evaporation, redissolved in chloroform and precipitated in anhydrous ether, and the dissolution-precipitation operation was repeated 3 times, and the precipitate was vacuum-dried to obtain a colorless viscous liquid product hyperbranched polysulfide (11.13 g, 68.2% yield).

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Abstract

The invention relates to a hyperbranched polythioether preparation method. According to the preparation method disclosed by the invention, a bi-functionality asymmetric alkene compound and tri-functionality sulfur alcohol are utilized as raw materials, thiol-ene is utilized to perform unequal-reactivity addition reaction, and hyperbranched polythioether is synthesized by a one-pot method. The preparation method disclosed by the invention has the advantages that the raw materials are easy to obtain, and the steps are simple; a terminal group of the prepared hyperbranched polythioether is sulfydryl; functional modification can be further performed; thus, the hyperbranched polythioether with specific performance can be prepared.

Description

【Technical field】 [0001] The invention relates to a preparation method of hyperbranched polysulfide, belonging to the field of organic polymers. 【Background technique】 [0002] The hyperbranched polymer molecule has a three-dimensional ellipsoidal structure, has a cavity inside the molecule, and has a large number of reactive groups at the end. Compared with the dendritic polymer, the hyperbranched polymer has simple synthesis steps and has a good industrial application prospect. [0003] At present, hyperbranched polysulfide mainly has AB 2 and A 2 +B 3 Two preparation methods. Chinese patent (CN2016105865276) uses lipoic acid as a raw material to synthesize AB containing both sulfhydryl and double bonds through multi-step reactions 2 Monomers, and lipoic acid-based hyperbranched polythioethers were prepared by mercapto-ene click chemistry. But AB 2 There are fewer types of monomers of type A, and most of them require complex organic synthesis processes; while A 2 +B...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/045
CPCC08G75/045
Inventor 李小杰朱钦富胡可珍魏玮刘仁陈明清
Owner JIANGNAN UNIV
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