Epoxy resin curing accelerator based on cyclotriphosphazene and imidazole compound as well as preparation method and application method thereof

A technology of epoxy resin curing and imidazole compounds, which is applied in the field of epoxy electronic packaging, can solve the problems of long-term storage of single-component systems, shorten the service life of materials, and reduce the curing temperature, etc., so as to improve latent performance and room temperature storage stability The effect of raising and lowering activity

Inactive Publication Date: 2018-12-11
WUXI CHUANGDA ELECTRONICS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for ordinary imidazole, due to the high activity of the two nitrogen atoms on the ring, when imidazole is used as an accelerator, when the curing temperature is lowered, the system tends to initiate crosslinking at room temperature, shortening the The service life of the material prevents it from being stored as a one-component system for a long time, which lacks practicability; in the production process, when the molding system undergoes the screw mixing process, the temperature rise can easily induce unnecessary curing of the system in advance, causing serious production problems; in the transfer molding process, it is necessary to achieve high-efficiency curing reactions under high temperature conditions in order to achieve the purpose of molding and smooth demoulding

Method used

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  • Epoxy resin curing accelerator based on cyclotriphosphazene and imidazole compound as well as preparation method and application method thereof
  • Epoxy resin curing accelerator based on cyclotriphosphazene and imidazole compound as well as preparation method and application method thereof
  • Epoxy resin curing accelerator based on cyclotriphosphazene and imidazole compound as well as preparation method and application method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 14.76 g p-hydroxybenzaldehyde and 20 mL triethylamine, dissolve in 40 mL tetrahydrofuran, 66 o Under C reflux and stirring, the tetrahydrofuran solution of hexachlorocyclotriphosphazene (6.95 g of hexachlorocyclotriphosphazene dissolved in 40 mL of tetrahydrofuran) was added dropwise to it, and the addition was completed within 40 minutes. After the reaction was continued for 8 h, the turbid liquid was suction filtered to obtain a light yellow filtrate. After the solvent was removed by rotary evaporation, washed twice with ethanol, filtered to obtain a white powder, and finally recrystallized in ethyl acetate twice, the precipitate was dried in a vacuum drying oven for 12 h to obtain a pale yellow powder, which is Aldehyde phenoxy) cyclotriphosphazene.

[0025] Weigh 4.31 g of hexa(p-aldehyde phenoxy) cyclotriphosphazene prepared above, 4.33 g 2-naphthol and 2.04 g imidazole, dissolve them in 60 mL isopropanol, adjust the pH of the reaction environment with hydrochlo...

Embodiment 2

[0028] Weigh 14.76 g p-hydroxybenzaldehyde and 20 mL triethylamine, dissolve in 40 mL tetrahydrofuran, 66 o Under C reflux and stirring, the tetrahydrofuran solution of hexachlorocyclotriphosphazene (6.95 g of hexachlorocyclotriphosphazene dissolved in 40 mL of tetrahydrofuran) was added dropwise to it, and the addition was completed within 40 minutes. After the reaction was continued for 8 h, the turbid liquid was suction filtered to obtain a light yellow filtrate. After the solvent was removed by rotary evaporation, washed twice with ethanol, filtered to obtain a white powder, and finally recrystallized in ethyl acetate twice, the precipitate was dried in a vacuum drying oven for 12 h to obtain a pale yellow powder, which is Aldehyde phenoxy) cyclotriphosphazene.

[0029] Weigh 4.31 g of hexa(p-aldehyde phenoxy) cyclotriphosphazene prepared above, 4.33 g 2-naphthol and 2.04 g imidazole, dissolve them in 60 mL isopropanol, adjust the pH of the reaction environment with hydrochlo...

Embodiment 3

[0032] Weigh 14.76 g p-hydroxybenzaldehyde and 20 mL triethylamine, dissolve in 40 mL tetrahydrofuran, 66 o Under C reflux and stirring, the tetrahydrofuran solution of hexachlorocyclotriphosphazene (6.95 g of hexachlorocyclotriphosphazene dissolved in 40 mL of tetrahydrofuran) was added dropwise to it, and the addition was completed within 40 minutes. After the reaction was continued for 8 h, the turbid liquid was suction filtered to obtain a light yellow filtrate. After the solvent was removed by rotary evaporation, washed twice with ethanol, filtered to obtain a white powder, and finally recrystallized in ethyl acetate twice, the precipitate was dried in a vacuum drying oven for 12 h to obtain a pale yellow powder, which is Aldehyde phenoxy) cyclotriphosphazene.

[0033] Weigh 4.31 g of hexa(p-aldehyde phenoxy) cyclotriphosphazene prepared above, 4.33 g 2-naphthol and 2.04 g imidazole, dissolve them in 60 mL isopropanol, adjust the pH of the reaction environment with hydrochlo...

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Abstract

The invention provides an epoxy resin curing accelerator based on cyclotriphosphazene and an imidazole compound as well as a preparation method and an application method thereof. According to the epoxy resin curing accelerator as well as the preparation method and the application method thereof, hexachlorocyclotriphosphazene, p-hydroxy benzaldehyde, naphthol and the imidazole compound are taken asraw materials, and the imidazole derivative based on the cyclotriphosphazene is prepared through two-step reaction; due to the steric effect of a side group and sealing of a pyrrole nitrogen active site, when the product is used as the epoxy resin curing accelerator, the room temperature storage stability of the system is obviously improved, and the curing reaction can be efficiently promoted ata high temperature; and meanwhile, the obtained curing product has good mechanical property and thermal stability, relatively low moisture absorption rate and excellent flame retardancy and can be used as an excellent epoxy resin latent curing accelerator.

Description

Technical field [0001] The invention is mainly used in the field of epoxy electronic packaging, and specifically relates to an epoxy resin curing accelerator based on cyclotriphosphazene and imidazole compounds, and preparation and application methods thereof. Background technique [0002] Due to its excellent electrical insulation, thermal stability, chemical resistance and mechanical properties, epoxy resin has become one of the mainstream electronic packaging materials with the largest consumption today. Generally, epoxy encapsulation systems mainly include potting systems and molding systems. The basic composition includes various additives such as matrix epoxy resin, curing agent, curing accelerator, filler and diluent. The cross-linking reaction between epoxy resin and curing agent such as novolac resin or acid anhydride tends to have higher activation energy, and the curing reaction often requires the presence of an accelerator to proceed smoothly. Due to its low toxicity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/68C08L63/00C08L63/04C07F9/6593
CPCC08G59/688C07F9/65815C08L63/00C08L63/04
Inventor 魏玮唐禹尧李小杰费小马翁根元
Owner WUXI CHUANGDA ELECTRONICS
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