Halogen-free flame-retardant heat-resistant water-soluble epoxy resin, composition, preparation method and application thereof

An epoxy resin, water-soluble technology, applied in the synthesis and application of epoxy resin, can solve the problems that the comprehensive performance cannot meet the copper clad laminate, low cross-linking density, low mechanical strength, etc., and achieves good environmental performance and heat resistance. High and good water solubility

Active Publication Date: 2019-10-15
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The application of water-based phosphorus-containing epoxy resin on copper clad laminates has not been seen in the prior art. The phosphorus-containing epoxy resin in the prior art is generally made of 2-functionality bisphenol A epoxy or 3-functionality novolac epoxy , because 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO for short) consumes an epoxy group when it reacts with epoxy, if the water-based ring is made according to the prior art Oxygen needs to consume one more epoxy group, then the remaining epoxy group content will be very low, the crosslinking density after curing is low, the mechanical strength is low, and the heat resistance is low, so that the comprehensive performance cannot meet the requirements of copper clad laminate manufacturing. Require

Method used

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  • Halogen-free flame-retardant heat-resistant water-soluble epoxy resin, composition, preparation method and application thereof
  • Halogen-free flame-retardant heat-resistant water-soluble epoxy resin, composition, preparation method and application thereof
  • Halogen-free flame-retardant heat-resistant water-soluble epoxy resin, composition, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 3

[0041] A halogen-free flame-retardant and hot-water-resistant epoxy resin, the chemical structural formula of the halogen-free flame-retardant and hot-water-resistant epoxy resin is:

[0042]

[0043] The halogen-free flame retardant and heat-resistant water-soluble epoxy resin is composed of 4,4'-diaminodiphenylmethane tetraglycidyl epoxy resin and 9,10-dihydro-9-oxa-10-phosphaphenanthrene- 10-oxide (referred to as DOPO) is heated under the action of 2-ethyl-4-methylimidazole to generate phosphorus-containing epoxy resin, then reacted with diethanolamine, added lactic acid, and finally added (appropriate amount) water and stirred evenly. get. The halogen-free flame-retardant and heat-resistant water-soluble epoxy resin is light yellow liquid, and when the solid content is 75% by mass, the viscosity at normal temperature is 800-1200mpas.

Embodiment 4

[0045] The preparation method of the halogen-free flame-retardant and heat-resistant water-soluble epoxy resin is: add 60 parts by mass of 4,4'-diaminodiphenylmethane tetraglycidyl epoxy resin liquid into the reactor, and raise the temperature to 140°C , add 20 mass parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO for short), stir to make 9,10-dihydro-9-oxa-10-phosphorus Heterophenanthrene-10-oxide (DOPO for short) is dissolved in the liquid of 4,4'-diaminodiphenylmethane tetraglycidyl epoxy resin, and then 0.02 parts by mass of 2-ethyl-4-methylimidazole is added, Raise the temperature to 150°C and react for 4 hours, then cool down to 80°C, add 5 parts by mass of diethanolamine, stir and react for 4 hours, then cool down to 60°C, add 4 parts by mass of lactic acid, and finally add an appropriate amount of water, stir evenly, and make a solid A halogen-free flame-retardant and heat-resistant water-soluble epoxy resin with a mass percentage of 75% (pale yellow l...

Embodiment 5

[0047] The preparation method of the halogen-free flame-retardant and heat-resistant water-soluble epoxy resin is as follows: 70 parts by mass of 4,4'-diaminodiphenylmethane tetraglycidyl epoxy resin liquid is added to the reactor, and the temperature is raised to 140°C , add 25 mass parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO for short), stir to make 9,10-dihydro-9-oxa-10-phosphorus Heterophenanthrene-10-oxide (DOPO for short) is dissolved in the liquid of 4,4'-diaminodiphenylmethane tetraglycidyl epoxy resin, and then 0.1 parts by mass of 2-ethyl-4-methylimidazole is added, Raise the temperature to 180°C for 1 hour, then lower the temperature to 120°C, add 10 parts by mass of diethanolamine, stir and react for 2 hours, then cool down to 60°C, add 8 parts by mass of lactic acid, and finally add an appropriate amount of water, stir evenly, and make a solid The mass percent content is 75% (pale yellow liquid) halogen-free flame-retardant heat-resistant wat...

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Abstract

The invention discloses halogen-free flame-retardant heat-resistant water-soluble epoxy resin, a composition and a preparation method and application thereof. The halogen-free flame-retardant heat-resistant water-soluble epoxy resin is obtained by heating 4,4'-diaminodiphenylmethane tetraglycidyl epoxy resin and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide under the action of 2-ethyl-4-methylimidazole to generate phosphorus-containing epoxy resin, reacting the phosphorus-containing epoxy resin with diethanolamine, adding lactic acid, and adding water and stirring uniformly. The halogen-free flame-retardant heat-resistant water-soluble epoxy resin composition comprises 80-100 parts by mass of halogen-free flame-retardant heat-resistant water-soluble epoxy resin with a solid content of75%, 5-10 parts by mass of an amino resin curing agent, 3-5 parts by mass of an aqueous isocyanate curing agent, 1-2 parts by mass of boron trifluoride monoethylamine, and 10-20 parts by mass of water. The composition is particularly suitable for use as base resin for manufacturing copper clad laminates and has strong practicability.

Description

technical field [0001] The invention belongs to the synthesis and application of epoxy resin, and relates to a halogen-free flame-retardant and hot-water-resistant epoxy resin, its composition and its preparation method and application. The halogen flame retardant and hot water soluble epoxy resin composition is especially suitable as a matrix resin for manufacturing copper clad laminates. Background technique [0002] Copper clad laminate is the basic material of the electronics industry. It is mainly used for processing and manufacturing printed circuit boards (referred to as PCBs), and is widely used in electronic products such as televisions, computers, and mobile communications. The existing resins for copper clad laminates are basically produced by resins such as various common epoxy resins, phenolic resins, benzoxazine resins, etc., together with curing agents and a large amount of solvents. Volatilizes into the air, so the volatile organic substances (VOC for short)...

Claims

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Application Information

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IPC IPC(8): C08G59/30C07F9/6574
CPCC08G59/304C07F9/657172
Inventor 叶伦学唐文东黄杰李建学
Owner SICHUAN DONGFANG INSULATING MATERIAL
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