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Hyperbranched silicon-phosphorus synergistic flame retardant modified epoxy resin and preparation method thereof

A technology of hyperbranched silicon phosphorus and epoxy resin, which is applied in the field of advanced polymer material science, can solve the problems of small functionality, unfavorable epoxy resin cross-linked network structure, and difficulty in meeting toughness requirements, and achieves improved toughness and excellent resistance. The effect of combustion effect and excellent mechanical properties

Active Publication Date: 2019-12-20
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the flame retardant with linear structure obtained by this method has low functionality, which is not conducive to the cross-linked network structure of epoxy resin, and it is difficult to meet higher toughness requirements.

Method used

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  • Hyperbranched silicon-phosphorus synergistic flame retardant modified epoxy resin and preparation method thereof
  • Hyperbranched silicon-phosphorus synergistic flame retardant modified epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add γ-(2,3-epoxypropoxy)propyltrimethoxysilane, triethyl phosphate and 1,3-propanediol into a three-necked flask at a molar ratio of 1:1:4.375, under nitrogen protection Stirring in an oil bath, controlling the reaction temperature at 80-150° C., and reacting for 10-12 hours until no distillate is produced, to prepare phosphorus-containing hyperbranched polysiloxane.

[0032] Mix 60 parts of bisphenol A epoxy resin and 3 parts of phosphorus-containing hyperbranched polysiloxane, and stir at room temperature for 10-15 minutes to prepare a resin prepolymer. Then, add 50 parts of acid anhydride curing agent and 1 part of tertiary amine curing accelerator to the above prepolymer, stir for 5 to 10 minutes, pour it into a preheated mold, and put it in a vacuum oven at 80 to 100 ° C. , remove the air bubbles by vacuuming, put it into the blast drying oven for stage heating and curing, the curing process is 100~120°C / 2~4h+140~170°C / 2~3h, cooling, demoulding, and then at 170~200...

Embodiment 2

[0034] Add γ-(2,3-epoxypropoxy)propyltrimethoxysilane, triethyl phosphate and 1,3-propanediol into a three-necked flask at a molar ratio of 1:1:4.375, under nitrogen protection Stirring in an oil bath, controlling the reaction temperature at 80-150° C., and reacting for 10-12 hours until no distillate is produced, to prepare phosphorus-containing hyperbranched polysiloxane.

[0035] Mix 60 parts of bisphenol A epoxy resin and 5 parts of phosphorus-containing hyperbranched polysiloxane, and stir at room temperature for 10-15 minutes to prepare a resin prepolymer. Then, add 50 parts of acid anhydride curing agent and 1 part of tertiary amine curing accelerator to the above prepolymer, stir for 5 to 10 minutes, pour it into a preheated mold, and put it in a vacuum oven at 80 to 100 ° C. , remove the air bubbles by vacuuming, put it into the blast drying oven for stage heating and curing, the curing process is 100~120°C / 2~4h+140~170°C / 2~3h, cooling, demoulding, and then at 170~200...

Embodiment 3

[0037] Add γ-(2,3-epoxypropoxy)propyltrimethoxysilane, triethyl phosphate and 1,3-propanediol into a three-necked flask at a molar ratio of 1:1:4.375, under nitrogen protection Stirring in an oil bath, controlling the reaction temperature at 80-150° C., and reacting for 10-12 hours until no distillate is produced, to prepare phosphorus-containing hyperbranched polysiloxane.

[0038] Mix 70 parts of bisphenol A epoxy resin, add 3 parts of phosphorus-containing hyperbranched polysiloxane, and stir at room temperature for 10-15 minutes to prepare a resin prepolymer. Then, add 50 parts of acid anhydride curing agent and 1 part of tertiary amine curing accelerator to the above prepolymer, stir for 5 to 10 minutes, pour it into a preheated mold, and put it in a vacuum oven at 80 to 100 ° C. , remove the air bubbles by vacuuming, put it into the blast drying oven for stage heating and curing, the curing process is 100~120°C / 2~4h+140~170°C / 2~3h, cooling, demoulding, and then at 170~20...

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Abstract

The invention relates to hyperbranched silicon-phosphorus synergistic flame retardant modified epoxy resin and a preparation method thereof. The resin is composed of an epoxy phosphorus-containing hyperbranched polysiloxane flame retardant, bisphenol-A epoxy resin, an anhydride-type curing agent and a tertiary amine-type curing accelerator. On the one hand, a synergistic flame retardant of a hyperbranched structure contains both silicon and phosphorus flame retardant elements, and the synergistic effect between different flame retardant elements achieves an excellent flame retardant effect. Onthe other hand, the hyperbranched phosphorus-silicon synergistic flame retardant contains a large number of epoxy groups which can participate in a curing reaction together with epoxy resin and has good compatibility with a resin matrix, wherein a large number of nano-scale cavities reduce the crosslinking density of a resin system; and at the same time, Si-O-Si soft segments are introduced intothe epoxy resin, thereby effectively improving the toughness of the resin system. Various functional groups can be introduced to an active end through formulation, so that the epoxy resin can be endowed with different properties, and the hyperbranched silicon-phosphorus synergistic flame retardant modified epoxy resin has broad application prospects in aerospace, electronic packaging and other fields.

Description

technical field [0001] The invention belongs to the technical field of advanced polymer materials, and relates to a hyperbranched silicon-phosphorus synergistic flame retardant modified epoxy resin and a preparation method thereof. Background technique [0002] Epoxy resin is a common thermosetting resin. Due to the active epoxy groups in the molecular structure, they can cross-link with curing agents such as amines, phenols, and acid anhydrides to form insoluble and infusible resins. High polymer with three-dimensional network structure. The cured epoxy resin has excellent mechanical properties, good dielectric properties, small shrinkage rate, and is stable to alkali and most solvents, so it is widely used in national defense, people's livelihood and other fields for casting, impregnation, adhesives, coatings, etc. . However, due to the poor flame retardancy of epoxy resin itself, and the high crosslinking density of pure epoxy resin cured products, it shows the disadvan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08L63/02C08L83/08C08G77/30C08G77/06
CPCC08L63/00C08G77/30C08G77/06C08L2201/02C08L2312/00C08L83/08
Inventor 颜红侠张渊博郭留龙李林杨开明
Owner NORTHWESTERN POLYTECHNICAL UNIV
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