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Polyfunctional epoxy resin and its preparation method

A kind of epoxy resin-based, multi-functional technology, applied in the field of multi-functional epoxy resin and its preparation, can solve the problems of large dosage, poor product stability, and increased resin viscosity, and achieve low water absorption, excellent Heat resistance and dimensional stability, high heat resistance effect

Inactive Publication Date: 2004-12-15
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] There are also reports to use naphthalene-containing polyhydroxy aromatic compounds as the curing agent for common epoxy resins. For example, U.S. Pat. No. 5,459,223 proposes to prepare naphthalene-modified novolac resins ( novolak), due to the large amount of addition, the epoxy resin cured by this phenolic resin is relatively brittle, and the methylene in the phenolic resin molecule is easily oxidized during storage, the viscosity of the resin will increase, and the stability of the product will change. Difference

Method used

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  • Polyfunctional epoxy resin and its preparation method
  • Polyfunctional epoxy resin and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Add 288g of 1-naphthol, 30g of paraformaldehyde and 800mL of toluene into a reaction flask equipped with a thermometer, constant flow pump, condenser and stirrer, heat to 70°C, and slowly add 4.2g of citric acid. After the addition, the temperature was raised to 100° C., and the reaction was refluxed for 8 hours. After the reaction was completed, neutralize the reaction mixture with 10% aqueous sodium carbonate solution, wash to neutrality with distilled water, and remove solvent, water and unreacted monomers in the organic phase under reduced pressure to obtain 240g polyhydroxynaphthalene compound, M n =410, M w = 670, D = M w / M n = 1.63.

[0041] In another reaction flask equipped with a thermometer, a constant flow pump, a stirrer, a water separator and a vacuum system, add 152g of the polyhydroxynaphthalene compound and 850mL of epichlorohydrin obtained above, stir and dissolve, and then continuously within 6 hours Add 75g of 48% sodium hydroxide aqueous soluti...

Embodiment 2

[0043] Add 216g of 1-naphthol, 72g of 2-naphthol, 48g of paraformaldehyde, and 800mL of toluene into a reaction flask equipped with a thermometer, a constant flow pump, a condenser and a stirrer, heat to 70°C, and slowly add 4.2g of A mixture of citric acid and 1.9 g of p-toluenesulfonic acid. After the addition, the temperature was raised to 100°C, and the reaction was refluxed for 10 hours. After the reaction was completed, neutralize the reaction mixture with 10% aqueous sodium carbonate solution, wash to neutrality with distilled water, and remove solvent, water and unreacted monomers in the organic phase under reduced pressure to obtain 295g polyhydroxynaphthalene compound, M n =819, M w =1273, D=M w / M n = 1.55.

[0044] In another reaction flask equipped with thermometer, constant flow pump, stirrer, water separator and vacuum system, add the polyhydroxynaphthalene compound obtained above 150g, all the other operating steps are with embodiment 1, obtain 187g epoxy r...

Embodiment 3

[0046] In a reaction flask equipped with a thermometer, a constant flow pump, a condenser and a stirrer, add 288g of 1-naphthol, 800mL of toluene, 2.91g of phosphotungstic acid, and 3.8g of p-toluenesulfonic acid, heat to 50°C, and slowly add 69.6 g of acetone. After the addition, the temperature was raised to 70°C, and the reaction was refluxed for 3 hours. After the reaction was completed, the reaction mixture was neutralized with 10% aqueous sodium hydroxide solution, washed with distilled water to neutrality, and the solvent, water and unreacted monomers in the organic phase were removed under reduced pressure to obtain 230 g of polyhydroxynaphthalene compounds.

[0047] In another reaction flask equipped with thermometer, constant flow pump, stirrer, water separator and vacuum system, add the polyhydroxynaphthalene compound and 900mL epichlorohydrin obtained above 165g, and all the other operating steps are the same as in Example 1, to obtain 205g epoxy resin of the pres...

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Abstract

A kind of multifunctinoal epoxy resin and its preparation method is involved in this invention. In the formula, A3 is selected from hydrogen atom, cymene, methoxy, bromine atom, R1, R2, R3 are shrink glycerin aethers, the value of n lies between 0 and 8. The preparation process of the method includes: firstly, hydroxy naphthalene compound and bifunctional aldehyde or ketone shrink in the presence of proton acid activator, and multihydroxy naphthalene compound is gained, and then it makes aether reaction with PAE in the action of alkali activator. The epoxy resin has good capability such as high heat-resistance, low moisture absorption and low expandability etc., and fits madding glass cloth or epoxy resin pressing board covering copper and foil, and encapsulation of semiconductor component and IC, so it has capacious application foreground in the electronic industry.

Description

technical field [0001] The present invention relates to polyfunctional epoxy resin and preparation method thereof, especially react with naphthol and aldehydes and ketones compounds such as formaldehyde and acetone to obtain the condensation product containing multiple phenolic hydroxyl groups, and the molecular skeleton derived from the condensation product contains naphthalene Unit multifunctional epoxy resins, and methods for their preparation. [0002] Further, it relates to high heat resistance, low moisture absorption, low expansion and other excellent properties, as an electrical insulation material, especially for the manufacture of glass cloth / epoxy resin copper clad laminates (copper clad laminates, CCL) and then the manufacture of rigid Printed circuit board (printed circuit board, PCB) or base epoxy resin for packaging of semiconductor components and integrated circuits and its preparation method. technical background [0003] Epo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/08
Inventor 许凯陈鸣才胡红旗
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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