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A kind of epoxy resin curing agent microcapsule with polyurethane as shell material and preparation method thereof

An epoxy resin curing and microcapsule technology, which is applied in the direction of microcapsule preparation and microsphere preparation, can solve the problems of incomplete microcapsules, non-environmental protection of microcapsules, and affecting storage stability, etc., and achieve fast curing speed, Clear and controllable structure, good sealing effect

Active Publication Date: 2022-04-26
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of material either has organic solvent volatilization during the preparation process, or the microcapsules are not environmentally friendly due to the presence of formaldehyde and other toxic substances, or the storage stability is affected by the incomplete microcapsules

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preparation of polyurethane prepolymer

[0034] 1.5g (0.0334mol) of 1,4-butanediol, 1.5g (0.0030mol) of polyether diol (N210), 3.4g (0.0034mol) of polyethylene glycol monomethyl ether (MPEG1000), polyether three Add 0.34g (0.0102mol) of polyhydric alcohol (N303) into the reaction vessel, vacuum dehydrate, after cooling down to 70°C, add 10g (0.09mol) of isophorone diisocyanate (IPDI), 10g of butanone, and react at 90°C for 5 hours to obtain polyurethane prepolymer.

[0035] (2) Preparation of curing agent prepolymer aqueous dispersion

[0036] After the temperature of the prepolymer drops below 50°C, add 4.25g of 2-ethyl-4-methylimidazole into the prepolymer to disperse evenly. Slowly add the curing agent prepolymer into 85 g of distilled water, and disperse to obtain the aqueous dispersion of the curing agent prepolymer.

[0037] (3) Preparation of epoxy resin curing agent microcapsules with polyurethane as shell material

[0038] 1.44 g (0.048 mol) of ethylene...

Embodiment 2

[0040] (1) Preparation of polyurethane prepolymer

[0041] Diethylene glycol (DEG) 1.8g (0.034mol), polyether glycol (N210) 1.8g (0.004mol), polyethylene glycol monomethyl ether (MPEG1000) 4.6g (0.0045mol), poly Add 0.45 g (0.0135 mol) of ether trihydric alcohol (N303) into the reaction vessel, melt MPEG at 110° C., vacuumize and dehydrate. When the temperature was lowered to 70° C., 10 g (0.115 mol) of toluene diisocyanate (TDI) and 15 g of N-methylpyrrolidone were added, and reacted at 90° C. for 5 hours to obtain a polyurethane prepolymer.

[0042] (2) Preparation of curing agent prepolymer dispersion

[0043] After the temperature of the prepolymer drops below 50°C, 2.25g of 2-ethyl-4-methylimidazole and 2.25g of polythiol are added to the prepolymer to disperse evenly. Slowly add the curing agent prepolymer into 90 g of distilled water, and disperse to obtain the curing agent prepolymer dispersion.

[0044] (3) Preparation of curing agent microcapsules with polyurethan...

Embodiment 3

[0047] (1) Preparation of polyurethane prepolymer

[0048] Add 1.8g (0.021mol) of menthylene glycol, 3g (0.003mol) of polyethylene glycol monomethyl ether (MPEG1000), and 0.3g (0.009mol) of polyether trihydric alcohol (N303) into the reaction vessel, and heat it at 110°C. The MPEG is melted, vacuumed, and dehydrated. When the temperature was lowered to 70°C, 5 g (0.059 mol) of 1,6-hexyl diisocyanate (HDI) and 20 g of butanone were added, and reacted at 90° C. for 5 hours to obtain a polyurethane prepolymer.

[0049] (2) Preparation of curing agent prepolymer dispersion

[0050] After the temperature of the prepolymer drops below 50° C., 3.0 g of isophorone diisocyanate and 2.5 g of IPDI-modified 2-ethyl-4-methylimidazole are added to the prepolymer to disperse evenly. Add 50 g of distilled water dropwise to the curing agent prepolymer, and disperse to obtain a curing agent prepolymer dispersion.

[0051] (3) Preparation of curing agent microcapsules with polyurethane as she...

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Abstract

The invention belongs to the field of chemical materials, and in particular relates to an epoxy resin curing agent microcapsule with polyurethane as a shell material and a preparation method thereof. First react diisocyanate monomer with small molecule diol, macromolecule polyol and hydrophilic polyol to synthesize polyurethane prepolymer terminated with isocyanate, then disperse epoxy resin curing agent in the prepolymer and add water to make it The aqueous dispersion of polyurethane prepolymer containing curing agent is finally prepared by interfacial polymerization with water-soluble amine to form epoxy resin curing agent microcapsules with polyurethane as shell material. The method for preparing polyurethane epoxy resin curing agent microcapsules provided by the invention has the advantages of simple preparation method and environmental friendliness; the obtained epoxy resin curing agent microcapsules have the advantages of good storage stability, fast curing speed and the like.

Description

technical field [0001] The invention belongs to the field of chemical materials, and in particular relates to an epoxy resin curing agent microcapsule with polyurethane as a shell material and a preparation method thereof. Background technique [0002] Due to its good thermal stability, chemical stability, dimensional stability, mechanical properties, insulation, adhesion and molding processability, epoxy resin is widely used in aerospace materials, electronic component bonding materials, coatings and composite materials. materials etc. However, the epoxy resin and curing agent are two-component curing systems, and they will start to cure in a short time after mixing, which is greatly limited in the process of transportation and use, and is easy to cause waste. Therefore, the development of latent curing agent has been paid more and more attention. [0003] The so-called latent resin curing agent refers to a one-component system composed of a curing agent added to an epoxy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/50C08G18/66C08G18/48C08G18/42C08G18/40C08G18/32C08G18/12B01J13/16
CPCC08G59/5073C08G18/6674C08G18/6607C08G18/4825C08G18/4829C08G18/4238C08G18/4018C08G18/3206C08G18/283C08G18/12C08G18/3228B01J13/16
Inventor 李坚张怡菲任强汪称意
Owner CHANGZHOU UNIV