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Epoxy resin self-repairing microcapsule and preparation method thereof

A self-healing microcapsule, epoxy resin technology, applied in the field of composite materials, can solve the problems of unevenness, weakened catalytic efficiency, large size, etc., and achieves simple process, excellent stability and tightness, and little influence on the mechanical properties of the matrix. Effect

Inactive Publication Date: 2015-05-20
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned self-healing system with DCPD microcapsules as the key component has the following disadvantages: the price of Grubbs catalyst is high; it is unstable and easy to decompose when it is higher than 120 ° C, and it is susceptible to epoxy resin curing agent amines during the synthesis process. The influence of DCPD weakens the catalytic efficiency; although DCPD microcapsules have achieved good results in the repair of polymer matrix composites formed at room temperature, there are two isomers of α and β in DCPD (condensation points are 19.5 ° C and 33 ° C, respectively ℃), so DCPD is not suitable for self-healing of composite materials used at low temperatures; the mechanical properties of DCPD polymerization reaction products are low; in the traditional process of preparing urea-formaldehyde resin wall materials, the main raw material is formaldehyde, and the teratogenicity of the latter Sexuality and toxicity have been confirmed, so it is necessary to prepare low-formaldehyde or formaldehyde-free phase-change microcapsules
However, the size of the hollow capsule is large (2-35mm) and uneven, which is not conducive to the combination of the capsule and the matrix, which has a great impact on the mechanical strength of the matrix.

Method used

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  • Epoxy resin self-repairing microcapsule and preparation method thereof
  • Epoxy resin self-repairing microcapsule and preparation method thereof
  • Epoxy resin self-repairing microcapsule and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add 0.5 g of hectorite particles (purchased from Rockwood, with an average particle size of 105 nm, a maximum particle size of 500 nm, and a minimum particle size of 20 nm) into 100 g of water to obtain a dispersion as the water phase. Mix 1.0g of bisphenol A type epoxy resin E51 (purchased from Bluestar New Material Company), 0.5g of oil-soluble monomer styrene (St), 0.5g of oil-soluble crosslinking agent divinylbenzene (DVB), 0.5g Styrene and 0.002 g of initiator azobisisobutyronitrile (AIBN) were mixed, and the mixed liquid was used as an oil phase. Put the water phase and the oil phase into a 70°C oven to heat for 20 minutes and 3 minutes respectively for preheating, and stir to mix the components of the oil phase evenly (the total mass of epoxy resin E51 and monomer and crosslinking agent The mass ratio is 1:1, the mass ratio of divinylbenzene to styrene is 1:1). The water phase and the oil phase are mixed, and a stable oil-in-water emulsion is obtained by high-sp...

Embodiment 2

[0050] An aqueous solution of 0.5 g of silicon carbide particles (purchased from Sinopharm Chemical Reagent Co., Ltd., with an average particle size of 80 nm, a minimum particle size of 5 nm, and a maximum particle size of 230 nm) and 0.2 g of potassium persulfate (1% KPS) was added to 100 g In water, a dispersion was obtained as an aqueous phase. Mix 0.1g oil-soluble crosslinking agent ethylene glycol di(methacrylate) ester (EGDMA), 0.1g oil-soluble monomer methyl methacrylate (MMA), and 1.0g bisphenol A epoxy resin E51, This mixed solution was used as the oil phase. Put the water phase and the oil phase into a 70°C oven to heat for 20 minutes and 3 minutes respectively for preheating, and stir to mix the components of the oil phase evenly (the total mass of epoxy resin E51 and monomer and crosslinking agent The mass ratio is 5:1, and the mass ratio of methyl methacrylate to ethylene glycol di(methacrylate) ester is 1:1). The water phase and the oil phase are mixed, and a s...

Embodiment 3

[0055] Add 0.5 g of lithium diatomaceous earth particles (purchased from Rockwood (Rockwood) company, with an average particle size of 105 nm, a maximum particle size of 500 nm, and a minimum particle size of 20 nm) and 0.2 g of initiator azobisisobutyronitrile (AIBN) into the 100 g of water to obtain a dispersion as an aqueous phase. Mix 1.0g bisphenol A type epoxy resin F44 (purchased from Blue Star New Material Company) from Shanghai Resin Factory, 0.1g oil-soluble crosslinking agent divinylbenzene (DVB) and 0.1g styrene (St), This mixed solution was used as an oil phase. Put the water phase and the oil phase into a 70°C oven to heat for 20 minutes and 5 minutes respectively for preheating, and stir to mix the components of the oil phase evenly (wherein the mass ratio of epoxy resin F44 to the total mass of monomers is 5: 1. The mass ratio of divinylbenzene to styrene is 1:1). The water phase and oil phase prepared above were mixed, and the temperature was raised to 70° C...

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Abstract

The invention provides an epoxy resin self-repairing microcapsule and a preparation method thereof. The method comprises the following steps: mixing a water phase containing inorganic nanoparticles and water with an oil phase containing epoxy resin, monoolefin monomer, a polyene cross-linking agent and an initiator to form a stable oil-in-water emulsion; and heating the emulsion to realize emulsion polymerization in order to form the epoxy resin self-repairing microcapsule. The epoxy resin self-repairing microcapsule is prepared by adopting the inorganic nanoparticles as an emulsifier through an emulsion polymerization process via the method; and compared with methods adopting molecular emulsifiers, the method provided by the invention has the advantages of no need of subsequent emulsifier removal, simple process, and no pollution to environment. The epoxy resin self-repairing microcapsule prepared in the invention has the advantages of excellent stability, excellent leakproofness and high cladding rate.

Description

technical field [0001] The invention relates to the technical field of composite materials with self-healing function, more specifically, the invention relates to epoxy resin self-healing microcapsules synthesized by emulsion polymerization and a preparation method thereof. Background technique [0002] The concept of self-healing composite materials was first proposed by the US military in the mid-1980s. The earliest self-healing system was a simple simulation of the animal vascular network. Hollow glass fibers were embedded in concrete, and acetal polymer solution was injected into the fibers as an adhesive. Due to the difficulties in the manufacturing method of the hollow fiber network system, this technology is difficult to realize automatic preparation, so it is difficult to enter into industrial application. [0003] At present, the most researched self-healing microcapsules at home and abroad are microcapsule systems synthesized by coating DCPD (dicyclopentadiene) mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/14
CPCB01J13/14
Inventor 孙怡菁杨振忠张成亮
Owner INST OF CHEM CHINESE ACAD OF SCI
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