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Preparation method of high purity electronic stage tetraphenolic ethane tetraglycidel ether epoxy resin

A technology of tetraglycidyl ether and tetraphenolic ethane, applied in the field of high-purity electronic grade 1, can solve the problems of low epoxy value, high hydrolyzed chlorine content, many by-products, etc., and achieves high epoxy value and purity, The synthesis process is stable and reliable, and the effect of low hydrolyzable chlorine content

Inactive Publication Date: 2007-10-03
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of carrying out ring-opening addition etherification and ring-closing epoxidation dechlorination under the same strong alkaline condition is that the reaction process is carried out in one step and the process is simple; the disadvantage is that under such strong alkaline conditions, the raw material epichlorohydrin is prone to occur Hydrolysis side reaction, the formed resin product tetraphenol ethane tetraglycidyl ether is also easy to undergo polymerization side reactions with the raw material tetraphenol ethane, etc., there are many by-products, the product has a high hydrolyzable chlorine content and a low epoxy value

Method used

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  • Preparation method of high purity electronic stage tetraphenolic ethane tetraglycidel ether epoxy resin

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Introduce nitrogen into a 1L four-neck flask equipped with a stirring, thermometer and condensing reflux device to replace the air, add 245g of epichlorohydrin, 50g of tetraphenol ethane and 45g of isopropanol, stir, raise the temperature to 85°C, add Tetraethylammonium bromide 4.2g, ring-opening addition etherification reaction for 4h; then control the reaction temperature to 70°C, add 40% NaOH solution 20g, 15g, 10g in 3 times, each addition of alkali interval 0.5h, add After that, continue the initial ring-closing epoxidation dechlorination for 1h. Filter and distill under reduced pressure to recover isopropanol and excess epichlorohydrin. The temperature was raised to 90° C., and 200 ml of methyl isobutyl ketone and 25 g of 10% NaOH were added to carry out the second ring-closing epoxidative dechlorination reaction for 2 hours. Filter, wash, and distill under reduced pressure at 150°C to obtain crude epoxy resin. Then the crude product was dissolved with methyl is...

Embodiment 2

[0030]Introduce nitrogen into a 1L four-neck flask equipped with a stirring, thermometer and condensing reflux device to replace the air, add 245g of epichlorohydrin, 50g of tetraphenol ethane and 45g of isopropanol, stir, heat up to 90°C, add Tetraethylammonium bromide 3.8g, ring-opening addition etherification reaction for 3h; then control the reaction temperature at 80°C, add 30% NaOH solution 25g, 20g, 13g in 3 times, add alkali at intervals of 1h, and finish adding Then continue the initial ring-closing epoxidation dechlorination for 0.5h. Filter and distill under reduced pressure to recover isopropanol and excess epichlorohydrin. The temperature was raised to 90° C., and 200 ml of methyl isobutyl ketone and 22 g of 15% NaOH were added to carry out the second ring-closing epoxidative dechlorination reaction for 3 hours. Filter, wash, and distill under reduced pressure at 150°C to obtain crude epoxy resin. Then the crude product was dissolved with methyl isobutyl ketone ...

Embodiment 3

[0032] Introduce nitrogen into a 1L four-neck flask equipped with a stirring, thermometer and condensing reflux device to replace the air, add 245g of epichlorohydrin, 50g of tetraphenol ethane and 50g of propanol, stir, raise the temperature to 80°C, add four 7.7g of phenylphosphonium bromide, ring-opening addition etherification reaction for 5h; then control the reaction temperature at 80°C, add 35% NaOH solution 23g, 17g, 11g in 3 times, each addition of alkali interval 1h, after adding Continue the initial ring-closing epoxidative dechlorination for 2h. Filter and distill under reduced pressure to recover isopropanol and excess epichlorohydrin. The temperature was raised to 100° C., and 200 ml of methyl isobutyl ketone and 22 g of 15% NaOH were added to carry out the second ring-closing epoxidative dechlorination reaction for 4 hours. Filter, wash, and distill under reduced pressure at 150°C to obtain crude epoxy resin. Then the crude product was dissolved with methyl is...

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Abstract

This invention relates to preparation method of a high-pure electronic grade four phenolic group methylmethane, four ethyl oxide ester araldite, includes ring cleavage addition and etherealization, ring closure epoxy dechlorinate and ethoxyline resin refine. It takes four phenolic group methylmethane and epichlorohydrin as raw material, add solvent, under protection of inert gas, at the presence of phase transfer catalyst phase transfer catalyst quaternary ammonium salt or quaternary alkylphosphonium salt or their mixture, occur ring cleavage addition and etherealization, generate chlorine hydroxyl ether intermediate; then by stage add aqueous alkali, carry out first time ring closure epoxy dechlorinate reaction, control the reaction temperature at 60 to 80 deg.C; abstract solvent and over dose epichlorohydrin, then add aqueous alkali and methyl isobutyl ketone methyl isobutyl ketone solvent to carry out second time ring closure epoxy dechlorination, control reaction temperature at 70 to 110 deg.C, gain 1, 1, 2, 2 - four ( hydroxybenzene group) ethane four ethyl oxide ester araldite crude product; Refine crude product to obtain final product.

Description

technical field [0001] The invention relates to a preparation method of high-purity electronic grade 1,1,2,2-tetrakis(p-hydroxyphenyl)ethane tetraglycidyl ether epoxy resin. technical background [0002] With the rapid development of the field of microelectronics, microelectronic devices tend to be more highly integrated, high-performance, and thinner. The electrical insulation reliability, heat dissipation, heat resistance, corrosion resistance, high strength, toughness, and stability of the main epoxy resin of electronic packaging materials , Anti-UV penetration, etc. put forward higher performance requirements. Traditional electronic packaging materials, such as bisphenol-A epoxy resin and o-cresol novolac epoxy resin, have the disadvantage of being brittle and prone to packaging cracks. As an improvement measure, the practice of dispersing the rubber component in the resin is generally adopted. However, if additive components are used to improve the performance of epox...

Claims

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Application Information

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IPC IPC(8): C08G59/06
Inventor 刘跃进彭红星危自燕李胜国
Owner XIANGTAN UNIV