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A kind of reversible hydrogen bond self-healing polymer and its preparation method

A self-healing, polymer technology, applied in the preparation of organic compounds, preparation of urea derivatives, chemical instruments and methods, etc., can solve the problems of difficult to realize industrial production, high production cost, complex synthesis operation of UPy linking unit, etc., to achieve The post-processing is simple and easy to operate, the production cost is low, and the effect of industrialized operation is realized

Active Publication Date: 2020-08-04
广州市润奥化工材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis operation of UPy linker unit is complicated and the production cost is high, making it difficult to realize industrial production.

Method used

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  • A kind of reversible hydrogen bond self-healing polymer and its preparation method
  • A kind of reversible hydrogen bond self-healing polymer and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) At room temperature, add 0.3mol isophorone diisocyanate (IPDI), 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl p-cresol into a dry reaction flask, Add 0.3mol hydroxyethyl acrylate (HEA) dropwise under stirring, raise the temperature to 40-50°C after the dropwise addition, and stir the reaction until the measured -NCO value reaches half of that at the beginning of the reaction, that is, the semi-blocked isocyanate IPDI is prepared -HEA monomer;

[0023] (2) Keep the temperature of the reaction system, add 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl p-cresol to the reaction flask of step (1), batch by batch under stirring Add 0.15 mol of urea, then raise the temperature to 60-70°C, and stir the reaction until the measured isocyanate group (-NCO) value reaches the theoretical value, that is, the reversible hydrogen bond self-healing polymer is prepared.

[0024] Synthetic route such as figure 1 As shown, the infrared spectrum of the obtained self-h...

Embodiment 2

[0026] (1) At room temperature, add 0.2mol hexamethylene diisocyanate (HDI), 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl p-cresol into a dry reaction flask, Add 0.2mol polycaprolactone acrylate (CA) dropwise under stirring, raise the temperature to 40-50°C after the dropwise addition, and stir the reaction until the measured -NCO value reaches half of that at the beginning of the reaction, that is, the half-capped Isocyanate HDI-CA monomer;

[0027] (2) Keep the temperature of the reaction system, add 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl p-cresol to the reaction flask of step (1), batch by batch under stirring Add 0.1 mol of urea, then raise the temperature to 60-70°C, and stir the reaction until the measured isocyanate group (-NCO) value reaches the theoretical value, that is, the reversible hydrogen bond self-healing polymer is prepared.

Embodiment 3

[0029] (1) At room temperature, add 0.21mol diphenylmethane diisocyanate (MDI), 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl p-cresol into a dry reaction flask, Add 0.21mol hydroxyethyl methacrylate (HEMA) dropwise under stirring, raise the temperature to 40-50°C after the dropwise addition, and stir the reaction until the measured -NCO value reaches half of that at the beginning of the reaction, that is, the semi-blocked Isocyanate MDI-HEMA monomer;

[0030] (2) Keep the temperature of the reaction system, add 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl p-cresol to the reaction flask of step (1), batch by batch under stirring Add 0.1 mol of urea, then raise the temperature to 60-70°C, and stir the reaction until the measured isocyanate group (-NCO) value reaches the theoretical value, that is, the reversible hydrogen bond self-healing polymer is prepared.

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Abstract

The invention discloses a preparation method of a reversible hydrogen bond self-healing polymer. The preparation method comprises the following steps: (1) at room temperature, adding diisocyanate, a catalyst and a polymerization inhibitor into a reaction flask, dropwise adding hydroxy-terminated acrylate in a stirring state, then heating up to 40-50 DEG C, and stirring for reacting until the measured NCO value is half of the NCO value when reaction is started, so that a semi-terminated isocyante monomer is obtained; and (2) maintaining the temperature of the reaction system, replenishing the catalyst and the polymerization inhibitor into the reaction flask in the step (1), adding metered urea in batches in a stirring state, after the catalyst and the polymerization inhibitor are completely added, heating up to 60-70 DEG C, and stirring for reacting until the measured NCO value reaches a theoretical value, so that the reversible hydrogen bond self-healing polymer is obtained. The preparation method disclosed by the invention has the advantages that the operation is simple, the production cost is low, reaction conditions are mild, industrial production can be realized, and the obtained polymer contains a large number of N-H and C=O and has a self-healing capability.

Description

technical field [0001] The invention relates to the field of self-healing materials, in particular to a reversible hydrogen bond self-healing polymer and a preparation method thereof. Background technique [0002] Due to the advantages of excellent physical and chemical properties, high designability, low price and easy processing, polymer materials have a wide range of applications. However, polymer materials are easily affected by external thermal energy, mechanical action and chemical factors, and cracks or microcracks will occur inside. These cracks generally do not immediately lead to structural damage, and are difficult to be discovered or detected in time. If these micro-damages are not repaired in time, the structure and performance of the material will be reduced, leading to the deterioration of the function of the material, and it may also cause macroscopic cracks and brittle fractures, which will lead to serious catastrophic accidents. Therefore, the research on...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/79C08G18/09C08G18/32C08G18/68C08G18/67C07C273/18C07C275/18C07C275/14C07C275/40
CPCC07C273/1881C08G18/09C08G18/3829C08G18/672C08G18/68C08G18/79C08G2115/00C07C275/18C07C275/14C07C275/40
Inventor 杜鹏王贵富张弢余立挺张绳延
Owner 广州市润奥化工材料有限公司
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