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Preparation method of three-dynamic cross-linked self-repairing polyurethane and product thereof

A dynamic cross-linking and self-healing technology, applied in the field of polymer materials, can solve the problems of low repair efficiency, low reversible non-covalent bond energy, poor mechanical properties, etc., and achieve the effect of simple and easy preparation method

Active Publication Date: 2020-11-03
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in self-healing polymer materials, a single dynamic reversible non-covalent bond has low bond energy and weak force, which often leads to problems such as polymer repair rate, low repair efficiency, and poor mechanical properties.

Method used

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  • Preparation method of three-dynamic cross-linked self-repairing polyurethane and product thereof
  • Preparation method of three-dynamic cross-linked self-repairing polyurethane and product thereof
  • Preparation method of three-dynamic cross-linked self-repairing polyurethane and product thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] This embodiment provides a preparation method of three dynamically cross-linked self-healing polyurethanes, including:

[0031] (1) Add 3mmol isophorone diisocyanate, 1.5mmol polycarbonate diol 1000, 0.5mmol polytetrahydrofuran diol 2000, 1mmol 2,6-diaminopyridine and 10mL tetrahydrofuran solvent into a device equipped with mechanical stirring and condensing reflux In a three-necked flask, the oil bath was heated to 70°C to react for 6h; then 0.5mmol 1,3-propane sultone was added dropwise to the reaction system, and reacted at 70°C for 3h.

[0032] (2) 0.5mmol ZnCl 2 Add to the above reaction system, react at room temperature for 12 hours, pour into a polytetrafluoroethylene mold, dry at room temperature for 1 day, and then vacuum dry at 40° C. for 1 day to obtain the three-dynamically cross-linked self-healing polyurethane.

Embodiment 2

[0034] This embodiment provides a preparation method of three dynamically cross-linked self-healing polyurethanes, including:

[0035] (1) Add 3mmol of hexamethylene diisocyanate, 1mmol of polycarbonate diol 1000, 1mmol of polytetrahydrofuran diol 1000, 1mmol of 3,5-diaminopyridine and 10mL of tetrahydrofuran solvent into three ports equipped with mechanical stirring and condensing reflux device In the flask, the temperature of the oil bath was raised to 80° C. for 4 h; then 0.25 mmol γ-butyrolactone was added dropwise to the reaction system, and the reaction was carried out at 80° C. for 2 h.

[0036] (2) 0.75mmol Zn(CF 3 SO 3 ) 2 Add it to the above reaction system, react at room temperature for 12 hours, pour into a polytetrafluoroethylene mold, dry at room temperature for 2 days, and then vacuum dry at 40° C. for 2 days to obtain the three-dynamically cross-linked self-healing polyurethane.

Embodiment 3

[0038] This embodiment provides a preparation method of three dynamically cross-linked self-healing polyurethanes, including:

[0039] (1) Add 3mmol dicyclohexylmethane diisocyanate, 0.5mmol polycarbonate diol 2000, 0.5mmol polytetrahydrofuran diol 2000, 2mmol 2,6-diaminopyridine and 10mL tetrahydrofuran solvent into a device equipped with mechanical stirring and condensing reflux In a three-necked flask, the oil bath was heated to 90°C for 3 hours; then 1.5 mmol γ-butyrolactone was added dropwise to the reaction system, and reacted at 90°C for 1 hour.

[0040] (2) 0.5mmol FeCl 3 Added to the above reaction system, reacted at room temperature for 12 hours, poured into a polytetrafluoroethylene mold, dried at room temperature for 3 days, and then dried in vacuum at 40° C. for 3 days to obtain the triple dynamic cross-linked self-healing polyurethane.

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Abstract

The invention discloses a preparation method of three-dynamic cross-linked self-repairing polyurethane and a product thereof. The method comprises the following steps: adding diisocyanate, oligomericdihydric alcohol and diaminopyridine into a reaction system, heating to 70-90 DEG C by taking tetrahydrofuran as a solvent, and reacting for 3-6 hours; dropwise adding sultone or carboxylic acid lactone into the reaction system, and reacting for 1-3 hours at the temperature of 70-90 DEG C; and adding a metal salt into the reaction system, reacting for 6-12 hours at room temperature, pouring into apolytetrafluoroethylene mold, drying for 1-3 days at room temperature, and carrying out vacuum drying for 1-3 days at 40 DEG C to obtain the three-dynamic cross-linked self-repairing polyurethane. According to the preparation method, diaminopyridine respectively reacts with isocyanate groups, sultone or carboxylic acid lactone and metal ions to simultaneously introduce three dynamic reversible bonds including hydrogen bonds, zwitterions and metal coordination bonds into polyurethane to prepare the three-dynamic cross-linking self-repairing polyurethane, the preparation method is simple and easy to implement, and the repair efficiency can reach 98% under the mild condition of room temperature / 12 h or 40 DEG C / 0.5 h.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of three dynamic cross-linked self-repairing polyurethanes and a product thereof. Background technique [0002] Polymer materials are susceptible to comprehensive damage from external factors during processing and use, and microcracks will occur inside. As the cracks expand, the mechanical properties of the material will eventually be reduced and the service life will be shortened. Introducing the self-healing function into polymer materials enables the material to automatically repair damage and avoid further damage, which is beneficial to prolong the service life of the material and improve its safety. [0003] Dynamic reversible non-covalent bonds (such as hydrogen bonds, electrostatic interactions, metal coordination bonds, host-guest interactions, etc.) can achieve self-healing under mild conditions, and have broad application prosp...

Claims

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Application Information

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IPC IPC(8): C08J3/24C08L75/04C08K5/3432C08K5/46C08K5/1535C08K3/16C08K3/30C08G18/75C08G18/73C08G18/44C08G18/48
CPCC08G18/4018C08G18/44C08G18/4825C08G18/73C08G18/755C08G18/758C08J3/243C08J2375/04C08K3/16C08K5/1535C08K5/3432C08K5/46C08K2003/168
Inventor 冒海燕何雪梅朱淼朱青鹏
Owner YANCHENG INST OF TECH
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