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Latent light-sensitive microcapsule epoxy curing agent and preparation method thereof

An epoxy curing agent and microcapsule technology, which is applied in the direction of microcapsule preparation, microsphere preparation, adhesives, etc., can solve the problems of incomplete rupture of microcapsules, long time required, insufficient rapid curing, etc.

Inactive Publication Date: 2019-02-15
CHANGCHUN YONGGU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, in the curing reaction of epoxy resin using microcapsule latent curing agent, due to incomplete rupture of microcapsules during curing, insufficient release of curing agent after capsule rupture, etc., the time required for system reaction is long and rapid curing Sexual insufficiency and other issues

Method used

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  • Latent light-sensitive microcapsule epoxy curing agent and preparation method thereof
  • Latent light-sensitive microcapsule epoxy curing agent and preparation method thereof
  • Latent light-sensitive microcapsule epoxy curing agent and preparation method thereof

Examples

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preparation example Construction

[0067] combine figure 1 Illustrate that the present invention also provides a kind of preparation method of latent photosensitive microcapsule epoxy curing agent, comprises the following steps:

[0068] Step 1, the preparation of polymers whose general structure is a3, b3 or c3

[0069] Step 1-1, dissolve 3-hydroxymethyl-2 nitrobenzyl alcohol a1 or 4-hydroxymethyl-2 nitrobenzyl alcohol b1 or 5-hydroxymethyl-2 nitrobenzyl alcohol c1 in dry Dichloromethane or chloroform solvent is used to make a solution with a mass fraction of 0.1-10%. The solution is added to a three-necked flask equipped with a stirrer, and then the 4-dimethylaminopyridine catalyst is added. After stirring evenly, triethyl After amine, add 2-bromo-2-methyl-propionyl bromide dropwise, stir at room temperature, react for 20-30 hours, quench the reaction with methanol, dilute the reaction solution with tetrahydrofuran solvent, use 200-500 mesh basic silica gel or alkali Filter the triethylamine hydrochloride b...

Embodiment 1

[0094] The structure of the microcapsule wall material is shown in the figure below.

[0095]

[0096] Preparation of polymer a-1

[0097] In a three-neck flask equipped with a stirrer, dissolve 183 mg of 3-hydroxymethyl-2-nitrobenzyl alcohol (a1) in 90 mL of dry dichloromethane, and then add 1.83 mg of 4-dimethylaminopyridine. After stirring evenly, after adding 3 mg of triethylamine, 459.8 mg of 2-bromo-2-methyl-propionyl bromide was added dropwise, stirred at room temperature, reacted for 20 hours, and quenched the reaction with 18 mL of methanol. Add 10 mL of tetrahydrofuran solvent to the reaction solution, filter triethylamine hydrochloride with 200 mesh basic aluminum oxide, drop the filtrate into diethyl ether, precipitate precipitate, filter with Buchner funnel, and wash with deionized water several times, After vacuum drying at 110°C for 10 h, 394 mg of intermediate a2 was obtained, with a yield of 82%.

[0098] Mass spectrometry, [M+H] + : 479.96; elemental anal...

Embodiment 2

[0106] microcapsule wall material

[0107]

[0108] Preparation of polymer a-2

[0109] In a three-neck flask equipped with a stirrer, dissolve 183 mg of 3-hydroxymethyl-2-nitrobenzyl alcohol (a1) in 90 mL of dry dichloromethane, and then add 1.83 mg of 4-dimethylaminopyridine. After stirring evenly, after adding 3 mg of triethylamine, 459.8 mg of 2-bromo-2-methyl-propionyl bromide was added dropwise, stirred at room temperature, reacted for 20 hours, and quenched the reaction with 18 mL of methanol. Add 10 mL of tetrahydrofuran solvent to the reaction solution, filter triethylamine hydrochloride with 200 mesh basic aluminum oxide, drop the filtrate into diethyl ether, precipitate precipitate, filter with Buchner funnel, and wash with deionized water several times, After vacuum drying at 110°C for 10 h, 394 mg of intermediate a2 was obtained, with a yield of 82%.

[0110] Mass spectrometry, [M+H] + : 479.96; elemental analysis, C 39.93H 3.97Br 33.20N 2.90O19.94. Infrare...

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Abstract

The invention relates to the technical field of adhesives, in particular to a latent light-sensitive microcapsule epoxy curing agent and a preparation method thereof. The microcapsule epoxy curing agent takes a degradable polymer of a novel structure as a microcapsule wall material and an epoxy curing agent as a core material. The microcapsule wall material of the microcapsule epoxy curing agent can be degraded at a wavelength of 200-400 nm, and further the epoxy curing agent is released to cure epoxy resin; the problems that a system reaction takes a relatively long time, the rapid curing isnot sufficient and the like caused by reasons such as incomplete rupture of a microcapsule during curing, inadequate release of the curing agent after capsule rupture and the like in the curing reaction of epoxy resin performed by utilizing the microcapsule latent curing agent are solved; by means of an emulsion-solvent evaporation technology, the polymer or a mixture of other polymer materials doped with the polymer is used as the microcapsule wall material to encapsulate the epoxy resin curing agent, and the round microcapsule curing agent with a particle size of 1-100 mu m is prepared.

Description

technical field [0001] The invention relates to the technical field of adhesives, in particular to a latent photosensitive microcapsule epoxy curing agent and a preparation method thereof. Background technique [0002] Epoxy resin generally refers to low molecular weight organic compounds containing two or more epoxy groups in the molecule. It will not cure under normal temperature and general heating conditions. Because its molecular structure contains active epoxy groups, The epoxy curing agent can be used to open the ring to form an insoluble polymer with a network structure. The cured epoxy resin has good physical and chemical properties, such as its strong adhesion to various materials, small curing shrinkage, good electrical insulation, and strong chemical corrosion resistance. It is widely used in coatings , Adhesives, FRP, laminates, electronic casting, potting, encapsulation and other fields. [0003] In epoxy resin adhesive applications, the adhesive is usually p...

Claims

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Application Information

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IPC IPC(8): C08G59/40C08G59/50C09J163/00B01J13/04
CPCB01J13/043C08G59/40C08G59/5006C09J163/00
Inventor 张强王群郑岩刘姝李宇
Owner CHANGCHUN YONGGU TECH
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