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Epoxy resin, process for producing the same, epoxy resin composition containing the same, and cured object

A technology of epoxy resin and hydroxide, which is applied in the field of epoxy resin, its manufacture, epoxy resin composition using the epoxy resin and cured products, can solve the problem of low hygroscopicity, unsatisfactory adhesion, low Viscosity and other issues

Active Publication Date: 2006-08-09
NIPPON STEEL CHEMICALL &MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These epoxy resins have excellent characteristics such as excellent low viscosity and high filling rate of fillers. On the other hand, because they are low-viscosity, it is easy to cause sintering of the powder in the state of epoxy resin composition, and in the resistance There is a problem with agglomeration
In addition, even the obtained cured product is not ideal in terms of low hygroscopicity and adhesiveness.
[0004] From the viewpoint of improving blocking resistance, low hygroscopicity, and adhesion to metal materials, Japanese Patent Application Laid-Open No. 6-145300 proposes diphenyl sulfide having a glycidyl ether group with a t-butyl group in the ortho position. Structural epoxy resins, however, are not ideal in terms of curing, low viscosity, anti-blocking and heat resistance

Method used

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  • Epoxy resin, process for producing the same, epoxy resin composition containing the same, and cured object
  • Epoxy resin, process for producing the same, epoxy resin composition containing the same, and cured object
  • Epoxy resin, process for producing the same, epoxy resin composition containing the same, and cured object

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 240g of DHS was dissolved in 240g of DEGME and 1480g of epichlorohydrin, and reflux was performed under reduced pressure, while 108.4g of 48% sodium hydroxide aqueous solution was added dropwise at 45°C for 4 hours. During this process, generated water was removed from the system by azeotroping with epichlorohydrin, and distilled epichlorohydrin was condensed and returned to the system. After the dropwise addition, the reaction was continued for 1 hour. After that, the generated salt was removed by filtration, and after washing with water, DEGME and epichlorohydrin were distilled off to obtain 302 g of a colorless, transparent, liquid crude epoxy resin. The epoxy equivalent is 248, and the hydrolyzable chlorine is 2100ppm. The purity of DGS (epoxy monomer) in the resin was 91.0 wt%, and the content of the epoxy dimer containing two bisphenol compound units was 5.7 wt%. In addition, the content of the above-mentioned monoepoxide was 3.3 wt%.

[0049] 100 g of the obta...

Embodiment 2

[0052] Methanol was used to recrystallize 100 g of the epoxy resin obtained in Example 1 to obtain 88 g of white crystalline epoxy resin (epoxy resin B). The epoxy equivalent was 236, the hydrolyzable chlorine was 90 ppm, the purity of DGS in the resin was 98.2 wt%, and the content of epoxy dimer was 1.5 wt%. In addition, the content of the monoepoxide was 0.3 wt%. The temperature of the melting point peak in the DSC measurement of the obtained crystal was 122.2°C, the endothermic heat was 77.2 J / g, and the half width of the endothermic peak was 5.6°C.

Embodiment 3

[0054] Using 240g of DHS, 240g of DEGDME, 900g of epichlorohydrin, and 107.0g of 48% sodium hydroxide aqueous solution, it reacted similarly to Example 1, and obtained 298g of liquid crude epoxy resins. The epoxy equivalent is 253, and the hydrolyzable chlorine is 4600ppm. The purity of DGS in the resin is 88.5wt%, and the content of epoxy dimer is 8.4wt%. In addition, the content of the monoepoxide was 3.1 wt%.

[0055] 100 g of the obtained crude epoxy resin was dissolved in 800 g of MIBK, and 10.3 g of a 10% NaOH aqueous solution was added at 80° C., and reacted for 2 hours. After the reaction, filtration and water washing were performed, and MIBK was distilled off to obtain 94 g of a pure yellow liquid epoxy resin. The epoxy equivalent of the obtained epoxy resin was 242, the hydrolyzable chlorine was 240 ppm, the purity of DGS in the resin was 92.6 wt%, and the dimer content of the bisphenol compound was 6.2 wt%. In addition, the content of the monoepoxide was 1.4 wt%....

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Abstract

An epoxy resin having excellent curability and high crystallizability; an epoxy resin composition having excellent blocking resistance; and a cured epoxy resin excellent in heat resistance, moisture resistance, and adhesion. The epoxy resin is one obtained by reacting a 4,4'-dihydroxydiphenyl sulfide compound with epichlorohydrin, wherein the content of molecules in which the number of repetitions, n, is 0 is 90 wt.% or higher and the content of monoepoxy molecules is 2 wt.% or lower. For example, the epoxy resin is obtained by reacting 2,2'-dimethyl-5,5'-di-tert-butyl-4,4'-dihydroxydiphenyl sulfide with excess epichlorohydrin in the presence of an alkali metal hydroxide.

Description

technical field [0001] The present invention relates to a cured product that provides cured products that are excellent in handling properties such as low viscosity, curing reactivity, and anti-blocking properties, and that are excellent in low moisture absorption and adhesion to metal materials, and can be used in electronic devices such as semiconductor elements. / Crystalline epoxy resins for sealing electronic components, powder coatings, laminates, composite materials, etc., methods for producing the same, epoxy resin compositions using the epoxy resins, and cured products thereof. Background technique [0002] Epoxy resins have been widely used in industry for a long time. In recent years, the requirements for their performance are getting higher and higher. For example, in the representative field of resin compositions with epoxy resin as the main agent, there is a semiconductor sealant. In recent years, with the improvement of the integration of s...

Claims

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Application Information

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IPC IPC(8): C08G59/04C08G59/06
CPCC08G59/063C08G59/04
Inventor 梶正史大神浩一郎中原和彦
Owner NIPPON STEEL CHEMICALL &MATERIAL CO LTD
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