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Epoxy resin microcapsule coated by tetraethyl orthosilicate, and preparation method of the epoxy resin microcapsule

A technology of tetraethyl orthosilicate and epoxy resin coating, applied in the field of tetraethyl orthosilicate coating epoxy resin microcapsules and its preparation, to achieve excellent thermal stability and storage stability

Inactive Publication Date: 2013-10-02
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the existing research adopts two methods of chemical copolymerization and physical blending to introduce silicone-modified epoxy resin, and the introduction of silicone into epoxy resin system and toughening modification through microcapsule technology has not been reported yet.

Method used

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  • Epoxy resin microcapsule coated by tetraethyl orthosilicate, and preparation method of the epoxy resin microcapsule
  • Epoxy resin microcapsule coated by tetraethyl orthosilicate, and preparation method of the epoxy resin microcapsule
  • Epoxy resin microcapsule coated by tetraethyl orthosilicate, and preparation method of the epoxy resin microcapsule

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Add 15 g of terpene-based epoxy resin and 3 g of terpene-based epoxy resin-polyethylene glycol 4000 nonionic surfactant into a four-neck flask equipped with a thermometer, agitator, and condenser tube, Heat to 60°C and stir evenly at 600 rpm. Slowly add 150 g of distilled water dropwise and continue stirring for 40 min to obtain an oil-in-water (O / W) emulsion.

[0038](2) Add 15 g tetraethyl orthosilicate (TEOS) and 30 g distilled water to the Erlenmeyer flask, add dropwise 2 mol / L acetic acid aqueous solution, adjust the pH value to 2.2, and place it in a water bath at 60 °C for 50 min for hydrolysis , to obtain a uniform and transparent hydrolyzate.

[0039] (3) Slowly add the prehydrolyzate in (2) to the O / W emulsion in (1), control the temperature at 55 ℃, and stir at 450 rpm. After the dropwise addition, the pH value was adjusted to 2.5±0.1, and the reaction was continued for 3 h. Cool to room temperature, wash with distilled water, suction filter and dry to...

Embodiment 2

[0041] (1) Add 15 g of terpene-based epoxy resin and 3 g of terpene-based epoxy resin-polyethylene glycol 4000 nonionic surfactant into a four-neck flask equipped with a thermometer, agitator, and condenser tube, Heat to 60°C and stir evenly at 600 rpm. Slowly add 150 g of distilled water dropwise and continue stirring for 40 min to obtain an oil-in-water (O / W) emulsion.

[0042] (2) Add 30 g tetraethyl orthosilicate (TEOS) and 60 g distilled water to the Erlenmeyer flask, add dropwise 2 mol / L acetic acid aqueous solution, adjust the pH value to 2.2, and place it in a water bath at 60 °C for 50 min for hydrolysis , to obtain a uniform and transparent hydrolyzate.

[0043] (3) Slowly add the prehydrolyzate in (2) to the O / W emulsion in (1), control the temperature at 55 ℃, and stir at 450 rpm. After the dropwise addition, the pH value was adjusted to 2.5±0.1, and the reaction was continued for 4 h. Cool to room temperature, wash with distilled water, suction filter and dry t...

Embodiment 3

[0045] (1) Add 15 g of rosin-based epoxy resin and 3 g of rosin-based epoxy resin-polyethylene glycol 4000 nonionic surfactant into a four-neck flask equipped with a thermometer, agitator, and condenser, and heat to 80°C, stirring evenly at 600 rpm. Slowly add 150 g of distilled water dropwise and continue stirring for 40 min to obtain an oil-in-water (O / W) emulsion.

[0046] (2) Add 15 g tetraethyl orthosilicate (TEOS) and 30 g distilled water to the Erlenmeyer flask, add dropwise 2 mol / L HCl aqueous solution, adjust the pH value to 2.2, and place it in a water bath at 60 °C for 50 min for hydrolysis , to obtain a uniform and transparent hydrolyzate.

[0047] (3) Slowly add the prehydrolyzate in (2) to the O / W emulsion in (1), control the temperature at 55 ℃, and stir at 450 rpm. After the dropwise addition, the pH value was adjusted to 2.5±0.1, and the reaction was continued for 4 h. Cool to room temperature, wash with distilled water, suction filter and dry to obtain pow...

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Abstract

The invention discloses an epoxy resin microcapsule coated by tetraethyl orthosilicate, and a preparation method of the epoxy resin microcapsule. Epoxy resin is taken as a core material; and a wall material is formed by hydrolysis polycondensation reaction of the tetraethyl orthosilicate under an acid condition to coat the epoxy resin, so as to obtain the epoxy resin microcapsule; the core of the epoxy resin microcapsule is any one of bisphenol A epoxy resin, rosin epoxy resin and terpenyl epoxy resin; and the dosage of the tetraethyl orthosilicate is 0.5-2 times of mass of the epoxy resin. The epoxy resin microcapsule prepared by the method disclosed by the invention has the performances of organic and inorganic materials, and has excellent thermal stability and storage stability; the tetraethyl orthosilicate is free of poison or harm; the formed wall material of the epoxy resin microcapsule is friendly to the environment; and meanwhile, an organic silicon wall material of the epoxy resin microcapsule cracks in a curing process and is evenly distributed inside an epoxy resin system. Therefore, the toughness of cured epoxy resin can be improved.

Description

technical field [0001] The invention relates to an epoxy resin microcapsule and a preparation method thereof, in particular to a tetraethyl orthosilicate-coated epoxy resin microcapsule and a preparation method thereof. Background technique [0002] Microcapsules are micro-containers with a core-shell structure formed by coating the core material with film-forming substances. It isolates the core material from the outside world to protect, control release, improve stability, shield odor and reduce toxicity. Therefore, it is widely used in food, medicine, adhesives, coatings, dyes, photosensitive materials, phase change materials and other industries. In recent years, microcapsule technology has been applied in resin and its composite materials, and has become a new direction of high-performance materials research. [0003] The microencapsulation of epoxy resin refers to coating a layer of uniform solid capsule wall material on the surface of epoxy resin, so as to achieve th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/14C08G77/00C08L63/00C08L83/00
Inventor 孔振武林广沅吴国民
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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