Preparation method for low-dielectric halogen-free flame retardant glass fiber pre-impregnation material

A technology of flame-retardant glass fiber and prepreg, which is applied in the field of composite materials, can solve problems such as high dielectric constant and unsatisfactory production process, and achieve the effect of improving flame-retardant performance and low water absorption

Active Publication Date: 2015-04-08
山东光轩新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese patent (CN1488672A) discloses a reactive epoxy resin composition with high flame retardant performance, excellent flame retardant performance, but relatively high dielectric constant
Chinese patent (CN1721475A) discloses a halogen-free epoxy resin and its preparation method, which has excellent flame retardancy, but the resin does not meet the production process of the two-step hot-melt method

Method used

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  • Preparation method for low-dielectric halogen-free flame retardant glass fiber pre-impregnation material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 2000g liquid novolak epoxy resin, 500g DOPO and 2g triphenylphosphorus catalyst respectively, place in the reactor, under nitrogen protection, react at 160 ℃ for 3 hours, then add 100g double-terminated hydroxyl polyphenylene ether (number average molecular weight 2000, GPC test), continue to react for 1h, then add 3903g of bisphenol A glycidyl ether and mix, cool down to 120°C, add 500g of dicyandiamide curing agent, stir evenly and vacuum degassing, and prepare a pre-prepared compound with a phosphorus content of 1.0wt%. The resin system used for impregnation is prepared according to the curing process of 130°C / 2h+150°C / 2h to prepare cast body specimens. The adhesive film of the above resin system is combined with glass fiber to make a prepreg, and then laminated to make a composite material. The dielectric constant, limiting oxygen index, flame retardant grade and glass transition temperature of the resin system and the composite sheet were tested respectively....

Embodiment 2

[0018] Weigh 2000g of bisphenol A glycidyl ether, 900g of DOPO and 10g of benzyl triphenylphosphine bromide catalyst respectively, place them in a reaction kettle, and react at 140°C for 4.5 hours under the protection of nitrogen, then add 300g of double-terminated hydroxyl polyphenylene Ether (number-average molecular weight 1800, GPC test), continue to react for 2 hours, then add 1370g of liquid novolak epoxy to mix, cool down to 120°C, add 458g of dicyandiamide curing agent, stir evenly and vacuum defoam to obtain a phosphorus content of 2.5wt % resin system for prepreg, according to the curing process of 130 ℃ / 2h + 150 ℃ / 2h, to prepare cast body samples. The adhesive film of the above resin system is combined with glass fiber to make a prepreg, and then laminated to make a composite material. The dielectric constant, limiting oxygen index, flame retardant grade and glass transition temperature of the resin system and the composite sheet were tested respectively. The re...

Embodiment 3

[0020] Weigh 2000g of bisphenol A glycidyl ether, 820g of DOPO and 40g of tetramethylammonium hydroxide catalyst respectively, place in a reaction kettle, under the protection of nitrogen, react at 120°C for 6 hours, then add 200g of double-ended hydroxyl polyphenylene ether ( Number average molecular weight 1700, GPC test), continue to react for 3 hours, then add 2020g trifunctional glycidylamine epoxy resin and mix, cool down to 120°C, add 730gDDS curing agent, stir evenly and vacuum degassing, the obtained phosphorus content is 2.0wt % resin system for prepreg, according to the curing process of 130 ℃ / 2h + 180 ℃ / 2h + 200 ℃ / 1h, to prepare cast body samples. The adhesive film of the above resin system is combined with glass fiber to make a prepreg, and then laminated to make a composite material. The dielectric constant, limiting oxygen index, flame retardant grade and glass transition temperature of the resin system and the composite sheet were tested respectively. The...

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Abstract

The invention provides a preparation method for a low-dielectric halogen-free flame retardant glass fiber pre-impregnation material. The preparation method comprises the following steps of: preparing low-dielectric flame retardant epoxy resin by adopting a two-step process of enabling a phosphorus flame retardant and low-molecular-weight double-end hydroxyl polyphenyl ether to respectively react with epoxy resin according to phosphor-nitrogen cooperative flame retardant effect and the low-dielectric characteristic of polyphenyl ether; compounding the low-dielectric epoxy flame retardant resin with liquid epoxy resin, and uniformly mixing the compound with a latent curing agent to prepare a resin system for pre-impregnation material; and preparing the resin system for the pre-impregnation material into a film by a film laminating machine, compounding the film with the glass fiber or fabric by a compounding machine to obtain the low-dielectric halogen-free flame retardant pre-impregnation material. The glass fiber pre-impregnation material disclosed by the invention is excellent in flame retardant performances, small in dielectric constant, capable of satisfying the production process adopting the two-step process of thermally melting the pre-impregnation material, and suitable for large-scale production of the pre-impregnation material for electric appliances.

Description

technical field [0001] The invention belongs to the field of composite materials, and in particular relates to a preparation method of a low-dielectric halogen-free flame-retardant glass fiber prepreg. Background technique [0002] Epoxy resin prepregs have been widely used in electronic and electrical fields such as printed circuit boards and transformer inner insulation materials. In order to meet the flame retardant requirements of materials, brominated epoxy resins are often used as the resin matrix of flame retardant prepregs. However, , bromine-containing epoxy resin will produce a large amount of toxic gas harmful to the human body when it is burned; at the same time, the existing solvent method to prepare glass fiber / epoxy resin prepreg will bring environmental pollution problems such as difficulty in solvent volatilization and recovery. With people's emphasis on environmental protection, halogenated flame retardants will gradually be replaced, and the melting proces...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L63/00C08L63/02C08L63/04C08G59/14C08G81/00C08K7/14
Inventor 李刚李波杨小平王丽丽刘大伟
Owner 山东光轩新材料有限公司
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