Thermal-reversible self-repair polyurethane membrane and preparation method therefor

A polyurethane film and self-healing technology, which is applied in the field of self-healing polymer-based composite materials and its preparation, can solve the problems of low hardness and low heat-resistant temperature, and achieve high self-healing ability, good manufacturability, and good environmental protection characteristics Effect

Active Publication Date: 2015-12-23
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The invention aims at the deficiencies of the existing reversible self-healing polyurethane materials, such as low heat-resistant temperature and low hardness, and provides an initial thermal decomposition temperature Tdi The thermally reversible self-healing polyurethane film with a temperature not lower than 300°C has high heat resistance, and the hardness is not lower than Shore A70-80. At the same time, it has a wide source of raw materials, a simple preparation method, a short cycle, and strong practicability. Preparation

Method used

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  • Thermal-reversible self-repair polyurethane membrane and preparation method therefor
  • Thermal-reversible self-repair polyurethane membrane and preparation method therefor
  • Thermal-reversible self-repair polyurethane membrane and preparation method therefor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Preparation of hyperbranched polysiloxane with maleimide group

[0036] in N 2 Under protection and magnetic stirring conditions, in a 250mL three-necked flask, 2.24g N-carbamoylmaleimide and 100mL toluene were fully mixed; then 3.584g γ-(2,3-epoxypropylene oxy)propyltrimethoxysilane. After the dropwise addition, the temperature of the three-neck flask was raised to 50° C. and the reaction was carried out at constant temperature for 6 hours. After the reaction was over, the solvent was distilled off under reduced pressure, and vacuum-dried at room temperature to obtain silanized N-carbamoylmaleimide. For its hydrogen nuclear magnetic resonance spectrum, refer to the attached figure 1 .

[0037] Add 0.2688g of deionized water, 80mL of ethanol and 0.009g of tetramethylammonium hydroxide to the silylated N-carbamoylmaleimide, and mix thoroughly under the condition of magnetic stirring. Raise the temperature to 50°C and react at a constant temperature for 3 hours; ...

Embodiment 2

[0054] (1) Preparation of hyperbranched polysiloxane with maleimide group

[0055] in N 2Under protection and stirring conditions, in a 250mL three-necked flask, 2.24g N-carbamoylmaleimide and 80mL toluene were fully mixed; then 4.256g γ-(2,3-glycidyloxypropoxy ) Propyltrimethoxysilane. After the dropwise addition was completed, the temperature of the three-neck flask was raised to 55° C. and the reaction was carried out at constant temperature for 7 hours. After the reaction was completed, the solvent was distilled off under reduced pressure, and vacuum-dried at room temperature to obtain silylated N-carbamoylmaleimide.

[0056] To silylated N-carbamoylmaleimide, add 0.448g deionized water, 90mL ethanol, methanol, propanol, n-butanol mixture and 0.009g tetramethylammonium hydroxide, and under the condition of mechanical stirring , mix well. Raise the temperature to 50° C. and react at a constant temperature for 5 hours; after the reaction, the solvent was distilled off un...

Embodiment 3

[0063] (1) Preparation of hyperbranched polysiloxane with maleimide group

[0064] in N 2 Under protection and stirring conditions, in a 250mL three-necked flask, 2.24g N-carbamoylmaleimide and 90mL toluene were fully mixed; then 3.607g γ-(2,3-glycidyloxypropoxy ) Propyltrimethoxysilane. After the dropwise addition, the temperature of the three-neck flask was raised to 60° C. and the reaction was carried out at constant temperature for 6 hours. After the reaction was completed, the solvent was distilled off under reduced pressure, and vacuum-dried at 45° C. to obtain silylated N-carbamoylmaleimide.

[0065] Add 0.2748g of deionized water, 80mL of ethanol and 0.0091g ​​of tetramethylammonium hydroxide and tetraethylammonium hydroxide mixture to the silylated N-carbamoylmaleimide, and under magnetic stirring conditions, fully mix. Raise the temperature to 55° C. and react at a constant temperature for 4 hours; after the reaction, the solvent was distilled off under reduced p...

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Abstract

The invention discloses a thermal-reversible self-repair polyurethane membrane and a preparation method therefor. Under protection of inert gases, 4,4-diphenylmethane diisocyanate, polycaprolactone glycol and N,N-dimethyl formamide are mixed uniformly, a reaction is carried out at a temperature of 50-60 DEG C, then the solution is cooled to a temperature of less than 5DEG C, 2-furan methylamine is added in the solution, the temperature is risen to 95-105 DEG C, the reaction is carried out for 10-11h, then hyperbranched polysiloxane with maleimide groups is added, the pre-finishing product prepared after the reaction is finished is poured into a die and dried, and a thermal-reversible self-repair polyurethane membrane is obtained. By utilization of the Diels-Alder (DA) reaction, thermal-reversible self-repair of a polyurethane membrane is achieved, the prepared polyurethane membrane has advantages of excellent thermal stability and high hardness, and raw materials have wide sources. The preparation method has characteristics of simple technology, strong practicality, wide applicability and the like.

Description

technical field [0001] The invention relates to a self-healing polymer-based composite material and a preparation method thereof, in particular to a thermally reversible self-healing polyurethane film and a preparation method thereof. Background technique [0002] Self-healing materials are a class of smart materials with structural self-healing ability. They have broad development prospects and important application values ​​in the fields of automobiles, construction, electronics, and biomedicine. They are currently a hot spot in the research and development of functional materials. [0003] Common self-healing methods include microcapsules, hollow fibers, and microvessels. The problem with these methods is that the number of repairs is low, and once the curing agent is used up, the material will no longer have the ability to self-heal. In addition, it has disadvantages such as complex preparation process, high cost, and long repair time. In order to overcome these proble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L75/06C08L83/08C08G18/42C08G77/26
Inventor 梁国正付高辉顾嫒娟袁莉
Owner SUZHOU UNIV
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