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Ultraviolet self-healing polyamide material, and preparation method and self-healing method thereof

A technology of combining polyamide and ultraviolet light, which is applied in the field of ultraviolet light self-healing polyamide materials and its preparation, can solve the problems of limiting the development of metal ligand self-healing materials and the lack of research on self-healing systems. Achieve high healing efficiency, low healing temperature and good repeatability

Active Publication Date: 2019-12-17
SOUTHWEST PETROLEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few kinds of ligands that can be used in metal ligand self-healing systems, which limits the further development of metal ligand self-healing materials.
[0004] In addition, the self-healing materials of this kind of metal coordination system generally realize the self-healing of the material by heating, and there are few studies on the self-healing system induced by light.

Method used

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  • Ultraviolet self-healing polyamide material, and preparation method and self-healing method thereof
  • Ultraviolet self-healing polyamide material, and preparation method and self-healing method thereof
  • Ultraviolet self-healing polyamide material, and preparation method and self-healing method thereof

Examples

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Embodiment 1

[0033] A preparation method of ultraviolet light self-healing polyamide material, the steps are as follows:

[0034] (1) Preparation of ligand polyamide: take 2g of azopyridinecarboxylic acid in a 100ml round bottom flask, add 30ml of thionyl chloride therein, and reflux overnight to obtain a deep red transparent solution. After the solvent is evaporated to dryness, use two Methyl chloride was dissolved and filtered, repeated three times, and evaporated to dryness to obtain azobispyridyl chloride.

[0035] Add 16ml of polysiloxane diamine (Mn=5000g / mol), 25ml of dichloromethane, and 3.0ml of triethylamine into a 100ml round-bottomed flask, place it in a water bath at 0°C and stir for 2 hours to make it fully mixed, Under the protection of an inert gas at this temperature, 1 g of azopyridine chloride in dichloromethane was added dropwise to the round bottom flask. After the addition was complete, the reaction was continued at this temperature for 2 h, and then placed at room te...

Embodiment 2

[0043] A kind of preparation method of ultraviolet light self-healing polyamide material, step (1) is the same as embodiment 1, in step (2), in the step (2), zinc trifluoromethanesulfonate consumption 36mg, the azobispyridine unit and zinc ion in the polyamide The molar ratio is 2:1 for coordination, and other operations are the same as step (2) of Example 1.

[0044] Figure 6 It is the ultraviolet absorption spectrum of polyamide and polyamide after coordination with zinc ions. When there is no coordination with metal ions, the absorption peak of polyamide at 329nm is the trans absorption peak of the azopyridine structure, and the absorption peak at 470nm is the cis absorption peak of the azopyridine structure. After adding metal ions to coordinate with azopyridine, a new absorption peak appeared at 439nm, which proved that metal ions and azopyridine were successfully coordinated.

[0045] Figure 7 It is a self-healing material under UV light after 2:1 coordination of po...

Embodiment 3

[0047] A kind of preparation method of ultraviolet light self-healing polyamide material, step (1) is the same as embodiment 1, and step (2) is: take 1g above-mentioned polyamide and dissolve in 10ml dichloromethane, dissolve 16mg ferric trichloride in methanol (the molar ratio of the azobispyridine unit in the polyamide to the iron ion is 2:1 for coordination), the methanol solution of ferric chloride is added dropwise to the dichloromethane solution of the polyamide, and stirred at room temperature for 24h , evaporate the solvent to about 3ml, pour it into a polytetrafluoroethylene mold, place it at room temperature for 24 hours, and then dry it at 70°C for 12 hours to prepare a 15*6*1mm sample.

[0048] Figure 8 It is a UV self-healing material after 2:1 coordination of polyamide and iron ions, and the tensile curve before and after healing. The results showed that the self-healing efficiency of the material is close to 100%.

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Abstract

The invention discloses an ultraviolet self-healing polyamide material. The ultraviolet self-healing polyamide material is formed by compounding metal ions with a ligand polyamide through coordinationbonds, wherein the polyamide contains an azodipyridine structure; and a molar ratio of azodipyridine units in the polyamide to the metal ions is 1:(0.1-1). A preparation method of the ultraviolet self-healing polyamide material comprises the following steps: reacting azodipyridinecarboxylic acid with thionyl chloride under a 80 DEG C refluxing condition to synthesize azodipyridyl acyl chloride; synthesizing polyamide from the azodipyridinecarboxylic acid and long-chain diamine at room temperature under the catalysis of triethylamine with dichloromethane as a solvent; and stirring mixed solution of the obtained dichloromethane solution of the polyamide containing the azodipyridine structure and a methanol solution of a metal salt at room temperature for 24 h, and then heating the obtainedsolution to remove the organic solvent in order to obtain the ultraviolet self-healing polyamide material. The self-healing polyamide material can be rapidly self-healed through the reversible metal coordination bonds under the irradiation of ultraviolet light, and the healing efficiency is close to 100%.

Description

technical field [0001] The invention relates to the technical field of self-healing materials, in particular to an ultraviolet self-healing polyamide material based on an azopyridine structure, a preparation method thereof, and a self-healing method. Background technique [0002] Polymer composite materials are easily affected by chemical substances, external forces, light, heat and other factors during use, resulting in microcracks in the material. The appearance and diffusion of microcracks will degrade the structure and performance of the material, affecting its safety and life. Therefore, in view of the potential threat of microcracks to the safety of material structures, it is undoubtedly an important and practical issue to detect and repair microcracks as soon as possible. However, the microcracks of polymers are usually hidden deep inside, and due to technical limitations, small damages such as microcracks on many substrates are usually not easy to detect. If the da...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42C08G69/40C08G69/48C08J3/28C08L77/06
CPCC08G69/40C08G69/42C08G69/48C08J3/28C08J2377/06
Inventor 李云涛李辉彭博武赵春霞曾凯龙赐杰
Owner SOUTHWEST PETROLEUM UNIV
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