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A self-healing elastomer with high cross-linking topology and its preparation method and application

An elastic body and self-healing technology, applied in the direction of insulators, plastic/resin/wax insulators, organic insulators, etc., can solve the problem of not being able to improve mechanical strength and stretchability at the same time

Active Publication Date: 2021-09-10
GUANGDONG POWER GRID CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The invention provides a self-healing elastic body with a high cross-linking topological structure and its preparation method and application, which solves the problem that the existing elastic body cannot improve mechanical strength and stretchability at the same time

Method used

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  • A self-healing elastomer with high cross-linking topology and its preparation method and application
  • A self-healing elastomer with high cross-linking topology and its preparation method and application
  • A self-healing elastomer with high cross-linking topology and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] This embodiment is the preparation of self-healing elastomer, specifically as follows:

[0044] (1) Synthesis of triynes: 1,3,5-benzenetricarboxylic acid (15.0g, 72mmol) was dissolved in thionyl chloride (45ml, 0.63mol, excess), and a few drops of DMF were added dropwise, and the reaction mixture was refluxed 8h, converted to 1,3,5-benzenetricarboxylic acid chloride (pale yellow liquid); then at 0°C, the obtained trichloride (1.06g, 4.0mol) was dissolved in CH 2 Cl 2 , and triethylamine (2.8ml, 20mmol, catalyst) was added, then the mixture was added dropwise to propargylamine (0.8ml, 12.6mmol) in CH 2 Cl 2 solution, after stirring at room temperature for 24 h, the resulting mixture was concentrated, dissolved in ethyl acetate (200-300 ml), and successively washed with 1M H 2 SO 4 , water, saturated NaHCO 3 Wash the organic layer with anhydrous Na 2 SO 4 Dry, filter and spin dry to obtain the tripyne compound.

[0045] (2) Synthesis of azide monosubstituted β-cyc...

Embodiment 2

[0055] This embodiment is the preparation of self-healing elastomer, specifically as follows:

[0056] (1) Preparation of Alkyne-Modified Mono(6-ethylenediamino)-β-cyclodextrin (Alkyne-Modified EDA-β-CD)

[0057] Synthesis of 4-oxo-4-(prop-2-ynyloxy)butanoic acid: propargyl alcohol (4.76g, 0.085mol), succinic anhydride (10.6g, 0.116mol), pyridine (9.18g, 0.116mol ) and TEA (8.46 g, 0.116 mol) were dissolved in 100 mL of anhydrous 1,4-dioxane. The mixture was stirred at room temperature for 24 hours, then evaporated under vacuum. Dissolve the crude product in CH 2 Cl 2 and washed with cold 1M HCl. The organic phase was washed with MgSO 4 Dry, filter and evaporate. The product was isolated as a brown solid.

[0058] Take 5g of Tos-β-CD in 30ml of ethylenediamine, and heat the reaction at 100°C for 12h. After the reaction is complete, cool to room temperature, add excess acetone to precipitate, and filter to obtain a light yellow solid. Then, the obtained light yellow so...

Embodiment 3

[0064] This embodiment is the preparation of self-healing elastomer, specifically as follows:

[0065] (1) Modification of guest molecules: cholic acid has multiple functional groups that can be modified, and can be easily introduced into the main chain polymer. The head and the tail of cholic acid are respectively modified with amino functional groups to obtain water-soluble cholic acid derivatives (cholic acid diamine). First, cholic acid is modified into 3-aminomethyl cholate with higher activity, and then After dissolving in dry ethylenediamine and refluxing at 120° C. for 5 h, the reaction mixture was cooled to room temperature and stirred for 18 h, and the residual solvent was removed by distillation under reduced pressure. The final product obtained was purified by flash column chromatography (methanol / triethylamine=50:1 as eluent) to obtain cholic acid diamine.

[0066] (2) The preparation method of the clathrate is the same as step (3) of Example 2, wherein the main ...

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Abstract

The invention relates to the technical field of elastic materials, in particular to a self-healing elastic body with high crosslinking degree topological structure and its preparation method and application. The present invention provides a self-healing elastomer, wherein, the guest molecule in the clathrate and the comonomer are polymerized to form a long polymer chain, forming a rotaxane-like structure in which cyclodextrin is sheathed on the polymer main chain structure; and because the cyclodextrins are multimer structures, the polymeric long chains are cross-linked with each other through the cyclodextrins, forming an ultra-high cross-linking topology structure, and this ultra-high cross-linking degree increases the strength of the material. The cyclodextrin molecules on the long polymer chain can slip on the polymer molecular chain segment, so that when an external force is applied, energy can be dissipated through slipping, so that the material has better deformation ability and reversible recovery characteristics. At the same time, the strong reversible interaction between the copolymerized units of the polymer enables the self-healing of the material, which can be achieved at room temperature without external stimuli.

Description

technical field [0001] The invention relates to the technical field of elastic materials, in particular to a self-healing elastic body with high crosslinking degree topological structure and its preparation method and application. Background technique [0002] Elastomer materials have reversible deformation ability and superelasticity. This excellent mechanical property makes elastomer materials considered as one of the most useful materials for soft robots, cable sheath insulation materials, automobiles, and airplanes. Elastomer materials with a certain self-healing ability can greatly meet the intelligent needs of future products. In principle, the polymer material used as an elastomer must be soft, that is, the mobility of the molecular chain is better. Therefore, adding plasticizers to crosslinked rigid polymers or directly preparing polymers with lower glass transition temperatures are typical methods for preparing elastomers. However, these approaches usually fail to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F251/00C08F222/38C08F220/20C08B37/16C08G81/00H01B3/30
CPCC08B37/0015C08F251/00C08G81/00H01B3/307C08F222/385C08F220/20C08F222/38
Inventor 林木松李丽侯君波张晟付强
Owner GUANGDONG POWER GRID CO LTD
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