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A kind of room temperature curing epoxy curing agent microcapsule based on water-insoluble amine and preparation method thereof

An epoxy curing agent and room temperature curing technology, which is applied in the direction of microcapsule preparation, microsphere preparation, etc., can solve the problems of adverse effects on material properties, failure to meet basic requirements, unstable storage of curing agent, etc., and achieve a simple and easy preparation method , short reaction time, good stability

Active Publication Date: 2018-12-07
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this way, if the amount of curing agent or catalyst used is large, it will have an adverse effect on the performance of the material itself. If the amount used is small, there will be less catalyst or curing agent on the crack plane, and self-healing cannot be fully performed.
[0004] Chinese published patent CN101116806A prepares polythiol into a capsule-type curing agent, which solves the above problems, but the capsule core material is prone to cross-linking reaction with the wall material during the microencapsulation process and is consumed, and the storage of the curing agent in the capsule is unstable. The problem
Chinese patent CN104193965A discloses a microcapsule of imidazole epoxy curing agent and its preparation method, but heat curing is required in the repair process
However, the wall material of the former is prone to bacterial degradation, while the wall thickness of the latter exceeds 100 μm and requires special processing equipment, which cannot meet the basic requirements for self-healing composite materials and other fields.

Method used

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  • A kind of room temperature curing epoxy curing agent microcapsule based on water-insoluble amine and preparation method thereof
  • A kind of room temperature curing epoxy curing agent microcapsule based on water-insoluble amine and preparation method thereof
  • A kind of room temperature curing epoxy curing agent microcapsule based on water-insoluble amine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 16g of urea and 32.43g of 37wt% formaldehyde into a 250ml three-necked \reaction flask equipped with mechanical stirring. After the urea is completely dissolved, slowly adjust the pH value of the solution to 8 with sodium hydroxide solution, and then rapidly raise the temperature to 50°C , and stirred and refluxed for 0.5h to obtain a viscous and transparent prepolymer of urea formaldehyde, which was naturally cooled to room temperature. Mix 240g of 4,4'-diaminobicyclohexylmethane, 2g of toluene and 0.6g of n-hexanol evenly, slowly add to the above solution, stir and emulsify at 300r / min for 20-30min, then slowly drop in hydrochloric acid solution to adjust the reaction system When the pH value reaches 2, after the microcapsules are completely formed, raise the temperature to 50° C., cure for 2 hours, and the reaction ends. After filtering, washing and drying, white curing agent microcapsules are obtained. The average particle size of the synthesized curing agent m...

Embodiment 2- Embodiment 7

[0044] The preparation method of the microcapsules is basically the same as that in Example 1. The formula table and reaction conditions are shown in Table 1, and the coating ratio and other parameters of the prepared microcapsules are shown in Table 3.

Embodiment 8

[0046] Take 100 parts of epoxy resin E51 and 22 parts of IPDA, add the theoretical ratio of epoxy resin microcapsules and the curing agent microcapsules prepared in Example 1, mix evenly, remove air bubbles under reduced pressure, pour into a silicone mold and cure at room temperature for 24 hours , placed in an oven at a constant temperature of 80°C for 1.5 hours to cure. After natural cooling, the silicone mold was removed to obtain the fracture toughness test piece, and the INSTRON 3344 universal tensile testing machine was used for the fracture toughness test. Under room temperature, the tensile speed was set at 1mm / min, and the initial sample was stretched to failure. The fracture toughness is K 0 , remove the load, slowly close the crack surface, place it at room temperature for 3 hours, repeat the test, and obtain the repaired fracture toughness K 1 , η=K 0 / K 1 =70% is the repair efficiency under the conditions of the epoxy resin agent microcapsules and curing agent...

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Abstract

The invention discloses a water-insoluble type amine based epoxy hardener microcapsule solidified at room temperature and a preparation method thereof. The epoxy hardener microcapsule employs water-insoluble type amine or water-insoluble type amine and a water-insoluble type diluent and (or) a water-insoluble type promoter mixture as a capsule core, urea-formaldehyde resin is used as a capsule wall, and micro encapsulation is carried out in water for preparing the epoxy hardener microcapsule. The preparation method has the advantages of simple process and low cost, and the epoxy hardener microcapsule has the advantages of high covering rate and stable storage. The usage amounts of the diluent and the promoter can be controlled in order to adjust releasing speed and reaction speed, and the epoxy hardener microcapsule and an epoxy resin microcapsule can be compounded and applied to self-repairing of high-molecular materials at room temperature.

Description

technical field [0001] The invention belongs to the technical field of rapid curing epoxy curing agent at room temperature, and in particular relates to a water-insoluble amine-based room temperature curing epoxy curing agent microcapsule and a preparation method thereof. Background technique [0002] When polymer materials are subjected to external forces during use, local damage such as cracks will inevitably occur, resulting in deterioration of material properties. Self-healing materials can sense this damage in time, repair cracks, etc., eliminate hidden dangers and prolong the service life of materials. [0003] In recent years, the application of microcapsules in the self-healing of polymer materials has become a new focus. By dispersing encapsulated epoxy resin in the resin matrix, when the material is damaged, the microcapsules are broken under the action of crack stress to release epoxy resin. , contact with the catalyst or curing agent in the resin matrix to under...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/50C08G12/12B01J13/04B01J13/08B01J13/14
CPCB01J13/043B01J13/08B01J13/14C08G12/12C08G59/5026C08G59/5033
Inventor 张春刘赵兴周萌牟昌盛陈浩邵仁龙倪自林
Owner WANHUA CHEM GRP CO LTD