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A kind of high hardness thermosetting self-healing polyurethane and preparation method thereof

A thermosetting, self-healing technology, applied in the field of self-healing polyurethane materials, to achieve high chemical and physical cross-linking, high repair efficiency, and high self-healing efficiency

Active Publication Date: 2021-08-31
JIANGXI SCI & TECH NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Self-healing thermosetting polyurethane is expected to solve this problem, however, how to prepare a kind of thermosetting polyurethane with exact self-healing ability, there is no prior art that can be used for reference; moreover, how to ensure the hardness, toughness, transparency of self-healing thermosetting polyurethane It has good performance in terms of repair efficiency and repair efficiency, and it has also become a technical problem to be solved urgently.

Method used

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  • A kind of high hardness thermosetting self-healing polyurethane and preparation method thereof
  • A kind of high hardness thermosetting self-healing polyurethane and preparation method thereof
  • A kind of high hardness thermosetting self-healing polyurethane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Take 4.4g of polyvinyl alcohol with a molecular weight of about 1750g / mol and place it in a reaction kettle, dissolve it in 20g of dimethyl sulfoxide at 90°C, add 11.4g of ε-caprolactone and 0.1 g zinc chloride, the reaction system was under the protection of nitrogen, stirred at 25°C for 4h, so that the solution was fully mixed, heated to 140°C for 5h, and a colorless transparent liquid was obtained, and then the obtained liquid was added to the separatory funnel, and the extraction agent 2 was added. Chloromethane, the obtained product is a white polymer. The obtained product is washed with methanol and dried in a vacuum oven at 25°C for 24 hours to obtain a polyvinyl alcohol-grafted polycaprolactone crosslinking agent.

[0048] See attached figure 2 , which is the infrared spectrum of the polyvinyl alcohol grafted polycaprolactone crosslinking agent prepared in Example 1 of the present invention. It can be seen from the figure that the characteristic peak of -C-O-C...

Embodiment 2

[0050] (1) Take 20g of polytetrahydrofuran with a molecular weight of about 1000 in the reaction kettle, pass nitrogen into the reaction kettle for 10 minutes, place the reaction kettle at 120°C for 2 hours in vacuum, completely remove the moisture in the reaction kettle, and put it under the protection of nitrogen , add 10.49g dicyclohexylmethane 4,4'-diisocyanate, 40g solvent N,N-dimethylformamide, 0.04g catalyst dibutyltin dilaurate into the reaction system, react the reaction system at 70°C for 1h, An isocyanate-terminated prepolymer is obtained.

[0051] (2) Add 8.48g of chain extender 2,2'-dithiodiethanol and 15.74g of dicyclohexyl 4,4'-diisocyanate into the reaction system, and react at 70°C for 1.5h under the protection of nitrogen to obtain isocyanate-blocked terminal linear polymer.

[0052] (3) Dissolve 4.74g of polyvinyl alcohol-grafted polycaprolactone in 30g of N,N-dimethylformamide, add the resulting solution into the system, and mix and react at 60°C for 20min...

Embodiment 3

[0061] (1) Take 30g of polytetrahydrofuran with a molecular weight of about 1000 in the reactor, pass nitrogen into the reactor for 10 minutes, place the reactor at 120°C for 2 hours in vacuum, completely remove the moisture in the reactor, and put it under the protection of nitrogen , add 15.74g dicyclohexyl methane 4,4'-diisocyanate, 40g solvent N,N-dimethylformamide, 0.04g catalyst dibutyltin dilaurate to the reaction system, react the reaction system at 70°C for 1h, An isocyanate-terminated prepolymer is obtained.

[0062] (2) Add 8.48g of chain extender 2,2'-dithiodiethanol and 10.49g of dicyclohexyl methane 4,4'-diisocyanate into the reaction system, and react at 70°C for 1.5h under the protection of nitrogen to obtain isocyanate-blocked terminal linear polymer.

[0063] (3) Dissolve 1.58g of polyvinyl alcohol-grafted polycaprolactone in 30g of N,N-dimethylformamide, add the resulting solution into the system, and mix and react at 60°C for 20min under the protection of ...

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Abstract

The invention provides a high-hardness thermosetting self-repairing polyurethane and a preparation method thereof. The technical scheme uses isocyanate-terminated polyurethane containing 2-hydroxyethyl disulfide as a functional group to cross-link and cure polyvinyl alcohol-grafted polycaprolactone to synthesize a thermosetting self-healing material with high self-healing efficiency and high hardness and transparency. Repair polyurethane. The invention realizes the self-healing of the material based on the disulfide bond exchange reaction, and provides a cross-linked network by grafting polycaprolactone with polyvinyl alcohol as a cross-linking agent, and the obtained material has excellent mechanical properties, high Young's modulus, and at the same time The material has good transparency, high self-healing efficiency, shape memory, reprocessing and other properties. In addition, the present invention also discloses a synthesis method of polyvinyl alcohol-grafted polycaprolactone. The polyvinyl alcohol-grafted polycaprolactone prepared by the method has multiple hydroxyl sites, which increases the interaction of hydrogen bonds between molecular chains. role, can provide a higher degree of chemical and physical cross-linking.

Description

technical field [0001] The invention relates to the technical field of self-repairing polyurethane materials, in particular to a high-hardness thermosetting self-repairing polyurethane and a preparation method thereof. Background technique [0002] Self-healing materials are a new class of materials that can achieve self-healing at the molecular level when the material is damaged, and have been extensively studied in recent years. Self-healing materials can prolong the service life of materials, thereby improving the durability of materials. [0003] Self-healing materials can be divided into two types according to their healing mechanism: exogenous self-healing and intrinsic self-healing. The external aid self-healing system relies on cross-linking agents, initiators and functional molecules wrapped in microcapsules, microspheres, microvessels and other structures as therapeutic agents. When the material is damaged, these microstructures release the internal therapeutic age...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/66C08G18/48C08G18/42C08G18/32C08G63/08C08G63/78
CPCC08G18/3855C08G18/4277C08G18/4854C08G18/66C08G63/08C08G63/78C08G2280/00
Inventor 钟江柳茂陈荣金闯申亮
Owner JIANGXI SCI & TECH NORMAL UNIV
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