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Low-hydroxyl phosphorus-containing epoxy resin and composition for copper clad laminate and preparation method thereof

A technology of epoxy resin and resin for copper-clad laminates, which is applied in the field of low-hydroxyl phosphorus-containing epoxy resin and copper-clad laminates and its preparation, raw materials for copper-clad laminates, and can solve the problems of high dielectric constant, dielectric loss, and water absorption. High efficiency, affecting the stability of copper clad laminates and other issues, to achieve the effect of low dielectric constant, low water absorption, glass transition temperature Tg increase

Active Publication Date: 2021-09-17
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the existence of a large number of hydroxyl groups, the polarity of the final molecular system is strong, so the dielectric constant and dielectric loss are high, while the hydroxyl equivalent (about 1000) is low. Because the hydroxyl group is highly hydrophilic, the water absorption rate of the resin after curing High, which affects the stability of copper clad laminates in humid environments

Method used

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  • Low-hydroxyl phosphorus-containing epoxy resin and composition for copper clad laminate and preparation method thereof
  • Low-hydroxyl phosphorus-containing epoxy resin and composition for copper clad laminate and preparation method thereof
  • Low-hydroxyl phosphorus-containing epoxy resin and composition for copper clad laminate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2-1~2-8

[0057] Example 2-1~2-8 Formulation Raw Material Consumption Table of Resin Composition for Copper Clad Laminate (Unit: kg)

[0058]

[0059]

[0060] Example 2-1 to 2-8 Sheet performance results of the resin composition for copper-clad laminates

[0061]

Embodiment 3

[0063] A low-hydroxyl phosphorus-containing epoxy resin is produced by mixing novolac epoxy resin, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO for short) and catalyst A Phosphorus-containing epoxy, then add isocyanate for further reaction to obtain low-hydroxyl phosphorus-containing epoxy resin;

[0064] The chemical structural formula of described novolak epoxy resin is:

[0065] In the formula: R is H, -CH 3 , n=1~7;

[0066] The catalyst A is tetraethylammonium bromide, tetramethylammonium chloride, triphenylphosphine, ethyltriphenylphosphine bromide, ethyltriphenylphosphine iodide, and ethyltriphenylphosphine acetate One or more mixtures;

[0067] The isocyanate is one or a mixture of two or more of diphenylmethane diisocyanate (abbreviated as MDI), toluene diisocyanate (abbreviated as TDI), and hexamethylene isocyanate (abbreviated as HDI).

Embodiment 4

[0069] The preparation method of low-hydroxyl phosphorus-containing epoxy resin, the steps are: 40 parts by mass of novolac epoxy resin, 10 parts by mass of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (abbreviated as DOPO) into the reactor (for example: three-necked flask, reaction kettle, etc.), heated to 110 ° C, stirred until 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (referred to as DOPO ) (completely) melted, add 0.1 parts by mass of catalyst A, stir and heat up to 140°C, and stir and react at this temperature for 1 hour, add 5 parts by mass of isocyanate, and then heat up to 170°C and stir for 1 to 6 hours, when When the hydroxyl equivalent is greater than or equal to 5000, lower the temperature, add 25 parts by mass of propylene glycol methyl ether and butanone mixed solvent, and stir evenly to obtain a low-hydroxyl phosphorus-containing epoxy resin.

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Abstract

The invention discloses a low-hydroxyl phosphorus-containing epoxy resin and a composition for copper clad laminates and a preparation method thereof, which is characterized in that: novolac epoxy resin, 9,10-dihydro-9-oxa-10-phosphor Phenanthrene-10-oxide and catalyst A are mixed and reacted to generate phosphorus-containing epoxy, and isocyanate is added to react to obtain low-hydroxyl phosphorus-containing epoxy resin; the resin composition for copper-clad laminates consists of 5-10 parts by mass of silicone resin, 3-6 Parts by mass of tris(2-hydroxyethyl)isocyanurate, 5-10 parts by mass of novolac resin, 5-10 parts by mass of unsaturated polyesterimide resin, 5-10 parts by mass of unsaturated benzoxazine resin , 40-50 parts by mass of low-hydroxyl phosphorus-containing epoxy resin, 0.1-0.5 parts by mass of imidazole catalyst and 10-15 parts by mass of butanone. The low-hydroxyl epoxy resin of the present invention is particularly suitable as a raw material for copper-clad laminates with low water absorption, low dielectric constant and low dielectric loss.

Description

technical field [0001] The invention belongs to flame-retardant epoxy resin for copper-clad laminates and its preparation, and relates to a low-hydroxyl phosphorus-containing epoxy resin, a composition for copper-clad laminates and a preparation method thereof. The low-hydroxyl phosphorus-containing epoxy resin and the composition for copper clad laminates of the present invention have the characteristics of low hydroxyl content, low water absorption, low dielectric constant, low dielectric loss, etc., and are especially suitable as raw materials for copper clad laminates. Background technique [0002] Now all kinds of organic resins are used in all walks of life, among which epoxy resins are widely used, especially phosphorus-containing epoxy resins, which are valued by more and more fields because of their flame retardancy. In the copper clad laminate industry, although phosphorus-containing epoxy resin has the advantages of low toxicity, low smoke, high flame retardant ef...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/14C08G18/58C08L63/04C08L83/04C08L61/06C08L61/34C08L67/06
CPCC08G18/58C08G59/1477C08G59/1488C08G59/1494C08L63/04C08L2201/02C08L2205/035C08L83/04C08L61/06C08L61/34C08L67/06
Inventor 叶伦学唐文东黄杰李建学
Owner SICHUAN DONGFANG INSULATING MATERIAL