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Latent microcapsule curing agent initiating thermosetting epoxy resin curing at medium temperature and preparation method of adhesive thereof

A technology of epoxy resin curing and microcapsule curing agent, applied in microcapsule preparation, microsphere preparation and other directions, can solve the problems of high material preparation cost, slow polymerization reaction speed, complicated reaction equipment, etc., and achieve tensile shear strength. The effect of improved performance, narrow particle size distribution and high content

Inactive Publication Date: 2012-04-25
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] At present, the preparation methods of microcapsules at home and abroad are mainly concentrated on in-situ polymerization and interfacial polymerization. There are problems such as long reaction time and slow polymerization reaction caused by chemical processes. At the same time, there are complex reaction equipment and required materials. Disadvantages such as high preparation cost

Method used

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  • Latent microcapsule curing agent initiating thermosetting epoxy resin curing at medium temperature and preparation method of adhesive thereof
  • Latent microcapsule curing agent initiating thermosetting epoxy resin curing at medium temperature and preparation method of adhesive thereof
  • Latent microcapsule curing agent initiating thermosetting epoxy resin curing at medium temperature and preparation method of adhesive thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1: Take gelatin as a dispersant, sodium dodecylbenzenesulfonate as an emulsifier, and dichloromethane as a solvent

[0053] In a fume hood, directly add 50mL of 0.5wt% gelatin aqueous solution and 100mL of 0.2wt% sodium dodecylbenzenesulfonate aqueous solution into a 500ml three-necked flask equipped with an electric stirrer, a condenser tube and a thermometer. Stir and disperse for 30 minutes to obtain a stable and uniform water phase; respectively add 1 g of diaminodiphenylmethane and 1 g of polymethyl methacrylate to two beakers filled with 20 mL of dichloromethane, and disperse evenly in an ultrasonic instrument until they dissolve The oily phase was obtained, and the oily phase was gradually added dropwise to the three-necked flask within 5 minutes. Stir for about 30 minutes to make the oil phase and water phase form a uniform and stable emulsion. Slowly raise the reaction temperature to 30°C and stir for 3 hours, then raise the temperature to 38°C and ...

Embodiment 2

[0055] Embodiment 2: Take polyvinyl alcohol as a dispersant, sodium dodecylbenzenesulfonate as an emulsifier, and dichloromethane as a solvent

[0056] In a fume hood, directly add 40mL of 0.2wt% polyvinyl alcohol aqueous solution and 80mL of 0.2wt% sodium dodecylbenzenesulfonate aqueous solution into a 500ml three-necked flask equipped with an electric stirrer, a condenser tube and a thermometer. Disperse under mechanical stirring for 30min to obtain a stable and uniform aqueous phase; add 1g N-aminoethylpiperazine and 2g polystyrene to two beakers containing 20mL of dichloromethane respectively, and disperse evenly in an ultrasonic instrument until the The oil phase was obtained by dissolving, and the oil phase was gradually added dropwise into the three-necked flask within 5 minutes. Stir for about 30 minutes to make the oil phase and water phase form a uniform and stable emulsion. Slowly raise the reaction temperature to 30°C and stir for 3 hours, then raise the temperatu...

Embodiment 3

[0058] Embodiment 3: Take gelatin as dispersant, Tween and Span as emulsifier, and dichloromethane as solvent

[0059] In a fume hood, directly add 50mL of 0.3wt% gelatin aqueous solution, 90mL of 0.1wt% Tween and Sipan (1:1) aqueous solution into a 500ml three-necked flask equipped with an electric stirrer, a condenser tube and a thermometer, at 700r / min disperse under mechanical stirring for 30min to obtain a stable and uniform aqueous phase; add 2g m-phenylenediamine and 1g styrene-methyl methacrylate copolymer to two beakers containing 20mL dichloromethane respectively, and Disperse until it dissolves to obtain an oil phase, and gradually add the oil phase to the three-necked flask within 5 minutes. Stir for about 30 minutes to make the oil phase and water phase form a uniform and stable emulsion. Slowly raise the reaction temperature to 30°C and stir for 3 hours, then raise the temperature to 40°C and stir for more than 3 hours until the dichloromethane volatilizes compl...

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Abstract

The invention relates to a latent microcapsule curing agent initiating thermosetting epoxy resin curing at medium temperature and a preparation method of an adhesive thereof. The latent microcapsule curing agent is technically characterized in that the high-activity medium temperature curing agent is taken as a core material, thermoplastic high polymer microspheres are taken as a wall material, the solvent evaporation technology is adopted for preparing the latent microcapsule curing agent with better curing performance and latent performance, and the latent microcapsule curing agent can be applied to an epoxy resin system for preparing the single-component medium temperature curing epoxy resin adhesive. Microcapsules prepared by the method are high in capsule core content, smooth in surfaces, narrow in particle size distribution and good in compatibility with matrix epoxy resin and can be better dispersed in the epoxy resin; and the prepared single component adhesive can realize curing at the medium temperature, the storage period at room temperature is longer and the tensile shear strength performance can be further improved.

Description

technical field [0001] The invention relates to a latent microcapsule curing agent for initiating curing of thermosetting epoxy resins, which can be used to prepare cured products with excellent physical properties, low viscosity and excellent processability. Background technique [0002] Epoxy resins are excellent in adhesion, corrosion resistance, mechanical properties, thermal properties, and electrical properties, and are widely and widely used as adhesives, coatings, inks, laminates, castings, molds, etc. Plastic products and electronic insulation materials, etc. Epoxy adhesives used in these areas can be one-component or two-component systems. [0003] The most widely used epoxy adhesive is a two-component system, which consists of epoxy resin and curing agent, which are stored separately. Therefore, two-component adhesives not only need to be packaged, stored and transported separately, which brings many operational and environmental problems, but also measurement e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/20
Inventor 张秋禹史有强马爱洁顾军渭耿旺昌
Owner NORTHWESTERN POLYTECHNICAL UNIV
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