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A kind of polyurethane with pH response and self-healing properties and preparation method thereof

A self-healing, polyurethane material technology, applied in the field of polymer materials to achieve the effect of improving damage recovery and improving mechanical properties

Active Publication Date: 2022-08-09
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, polymer materials that can take into account multiple responsiveness and self-healing properties have not been reported, especially pH-responsive temperature-sensitive self-healing polyurethanes that integrate shape memory effects, inter-chain hydrogen bonds, and intra-chain dynamic bonds.

Method used

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  • A kind of polyurethane with pH response and self-healing properties and preparation method thereof
  • A kind of polyurethane with pH response and self-healing properties and preparation method thereof
  • A kind of polyurethane with pH response and self-healing properties and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The present embodiment adopts the following raw materials:

[0041] 20g polycaprolactone diol (Mn~2000)

[0042] 160mL Tetrahydrofuran (THF)

[0043] 0.04g Dibutyltin dilaurate (DBTDL)

[0044] 0.856g Bis(2-hydroxyethyl)disulfide (SS)

[0045] 0.7408g 2,2-Dimethylolbutyric acid (DMBA)

[0046] 3.383g hexamethylene diisocyanate (HDI)

[0047] The preparation method of the present embodiment is:

[0048]In a three-necked flask equipped with an electric stirrer, a condenser tube and a vacuum tailpiece, polycaprolactone diol was added, and after vacuum dehydration at 110-120 °C for 2 hours, the temperature was lowered to about 60 °C, and HDI and an appropriate amount of tetrahydrofuran were added. Under nitrogen protection, the reaction was stirred at 60° C. for 1 hour to obtain a prepolymer. Add 0.856g bis(2-hydroxyethyl) disulfide (SS) and 0.7408g 2,2-dimethylolbutyric acid (DMBA) to the prepolymer to continue the reaction until the isocyanate is consumed completely...

Embodiment 2

[0073] The present embodiment adopts the following raw materials:

[0074] 10g polycaprolactone diol (Mn~1000)

[0075] 160mL N,N-Dimethylformamide (DMF)

[0076] 0.04g Dibutyltin dilaurate (DBTDL)

[0077] 0.8569g Bis(2-hydroxyethyl)disulfide (SS)

[0078] 0.7408g 2,2-Dimethylolbutyric acid (DMBA)

[0079] 3.3837g hexamethylene diisocyanate (HDI)

[0080] The preparation method of the present embodiment is:

[0081] In a three-necked flask equipped with an electric stirrer, a condenser tube and a vacuum tailpiece, polycaprolactone diol was added, and after vacuum dehydration at 110-120°C for 2 hours, the temperature was lowered to about 60°C, and HDI and an appropriate amount of N,N were added. -Dimethylformamide, stirred and reacted at 60°C for 1 hour under nitrogen protection to obtain a prepolymer. Add 0.856g bis(2-hydroxyethyl) disulfide (SS) and 0.7408g 2,2-dimethylolbutyric acid (DMBA) to the prepolymer to continue the reaction until the isocyanate is completely c...

Embodiment 3

[0097] The present embodiment adopts the following raw materials:

[0098] 10.6g polycaprolactone diol (Mn~530)

[0099] 160mL N,N-Dimethylformamide (DMF)

[0100] 0.04g Dibutyltin dilaurate (DBTDL)

[0101] 1.7138g Bis(2-hydroxyethyl)disulfide (SS)

[0102] 1.4966g 2,2-Dimethylolbutyric acid (DMBA)

[0103] 6.9654g hexamethylene diisocyanate (HDI)

[0104] The preparation method of the present embodiment is:

[0105] In a three-necked flask equipped with an electric stirrer, a condenser tube and a vacuum tailpiece, polycaprolactone diol was added, and after vacuum dehydration at 110-120°C for 2 hours, the temperature was lowered to about 60°C, and HDI and an appropriate amount of N,N were added. - Dimethylformamide, stirred and reacted at 60° C. for 1 hour under nitrogen protection to obtain a prepolymer. Add 0.856g bis(2-hydroxyethyl) disulfide (SS) and 0.7408g 2,2-dimethylolbutyric acid (DMBA) to the prepolymer to continue the reaction until the isocyanate is complete...

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Abstract

The invention discloses a preparation method of a polyurethane material with pH response and self-healing properties. The polyurethane material contains hydrogen bonds between molecular chains, and dynamic disulfide bonds and carboxylic acid functional groups in the molecular chains to form a microphase separation structure. . The polyurethane material is formed by polymerizing macromolecular diol, diisocyanate and chain extender in a nitrogen atmosphere in the presence of a catalyst and an organic solvent; the chain extender is a chain extender containing carboxylic acid and a chain extender containing carboxylic acid. As a chain extender for dynamic disulfide bonds, the ratio of the two substances is 1:1. Under the synergistic action of various functional groups and multi-level structures, the polyurethane material prepared by the invention has both pH and temperature responsiveness, can be effectively thermally healed under various dynamic actions, has good thermal stability, good hydrophilicity, and has good thermal stability. Potential for mass production and application.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to an intelligent responsive polyurethane material which simultaneously reflects pH responsiveness, temperature sensitivity and self-healing properties and a preparation method thereof. Background technique [0002] When the physicochemical characteristics of a macromolecule respond or change suddenly with the change of the environment, the macromolecule can be called a smart responsive material. Smart responsive polymer materials with pH responsiveness and temperature sensitivity have important applications in membrane separation, sustained drug release, target recognition, and smart coatings. [0003] The polymers containing -COOH on the polymer chain show pH-responsive characteristics due to the difference in protonation or ionization of carboxylic acid functional groups under different conditions. Polycaprolactone diol (PCL) is an environmentally friendly and degrad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/10C08G18/66C08G18/42C08G18/32C08G18/34
CPCC08G18/10C08G18/6659C08G18/4277C08G18/3855C08G18/348
Inventor 王化屈琦琪田兴友刘研研
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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