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High-performance fluorine-containing cyanate ester resin system and preparation method thereof

A technology of fluorine-containing cyanate ester and cyanate ester resin, which is applied in the field of high-performance fluorine-containing cyanate ester resin system and preparation, and can solve the problems of decreased heat resistance of resin system and the like

Active Publication Date: 2021-09-17
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the hyperbranched polysiloxane modifiers used in current research can significantly improve the toughness of the resin matrix, there is still a common problem that the heat resistance of the resin system will decrease.

Method used

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  • High-performance fluorine-containing cyanate ester resin system and preparation method thereof
  • High-performance fluorine-containing cyanate ester resin system and preparation method thereof
  • High-performance fluorine-containing cyanate ester resin system and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Preparation of fluorine-containing hyperbranched polysiloxane

[0038] Add γ-glycidyl etheroxypropyltriethoxysilane and hexafluorobisphenol A into a three-necked flask at a molar ratio of 3:1, stir under the protection of nitrogen, and control the reaction temperature between 80-150°C During the reaction period, react for 2 to 12 hours until no distillate is produced, and the fluorine-containing hyperbranched polysiloxane is obtained;

[0039] (2) Preparation of high-performance fluorine-containing cyanate resin system

[0040] After melting 100 parts of bisphenol A cyanate resin at 80°C, add 6 parts of fluorine-containing hyperbranched polysiloxane into it, stir mechanically for 30 minutes, pour it into a preheated mold, and heat it at 120°C In a vacuum oven, after evacuating for 30 minutes, put it into a blast drying oven for staged heating and curing. The curing process is 160°C / 2h+190°C / 3h+220°C / 2h, cooling, demoulding, and then curing at 240°C After 4 hours o...

Embodiment 2

[0042] (1) Preparation of fluorine-containing hyperbranched polysiloxane

[0043] Add γ-glycidyl etheroxypropyltriethoxysilane and hexafluorobisphenol A into the three-necked flask at a molar ratio of 2:1, stir under the protection of nitrogen, and control the reaction temperature between 80-150°C During the reaction period, react for 2 to 12 hours until no distillate is produced, and the fluorine-containing hyperbranched polysiloxane is obtained;

[0044] (2) Preparation of high-performance fluorine-containing cyanate resin system

[0045] Melt 100 parts of bisphenol A cyanate resin at 80°C, add 9 parts of fluorine-containing hyperbranched polysiloxane into it, heat up to 120°C, stir mechanically for 1 hour, and pour it into a preheated mold , in a vacuum oven at 120°C, after evacuating for 1 hour, put it into a blast drying oven for step-by-step heating and curing. Post-treatment at 240°C for 4 hours to obtain a high-performance fluorine-containing cyanate resin system.

Embodiment 3

[0047] (1) Preparation of fluorine-containing hyperbranched polysiloxane

[0048] Add γ-glycidyl etheroxypropyl triethoxysilane and hexafluorobisphenol A into a three-necked flask at a molar ratio of 1.8:1, stir under the protection of nitrogen, and control the reaction temperature between 80-150°C In between, react for 2 to 12 hours until no distillate is produced, and the fluorine-containing hyperbranched polysiloxane is obtained;

[0049] (2) Preparation of high-performance fluorine-containing cyanate resin system

[0050] Melt 100 parts of bisphenol A cyanate resin at 80°C, add 12 parts of fluorine-containing hyperbranched polysiloxane into it, heat up to 120°C, stir mechanically for 40 minutes, and pour it into a preheated mold , in a vacuum oven at 120°C, after evacuating for 2 hours, put it into a blast drying oven for staged heating and curing. The curing process is 160°C / 2h+190°C / 3h+220°C / 2h. Post-treatment at 240°C for 4 hours to obtain a high-performance fluorine-...

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Abstract

The invention relates to a high-performance fluorine-containing cyanate ester resin system and a preparation method thereof and aims to solve the problems that a cyanate ester resin cured product is high in brittleness, and the original excellent dielectric property and heat resistance of the cyanate ester resin cured product are often damaged by an existing toughening modification method. Fluorine-containing hyperbranched polysiloxane is synthesized through an ingenious molecular structure design, and the bisphenol A type cyanate ester resin is modified by using the fluorine-containing hyperbranched polysiloxane. A large number of active functional groups exist at the end position of the fluorine-containing hyperbranched polysiloxane, so that the fluorine-containing hyperbranched polysiloxane and the bisphenol A type cyanate resin can be subjected to copolymerization reaction; a flexible Si-O chain segment and a rigid benzene ring structure are introduced into the cyanate resin at the same time, and the toughness and heat resistance of a resin system are synergistically improved through the effect of combining hardness and softness. In addition, the contained low-polarizability C-F bonds can effectively improve the dielectric properties of the cyanate ester resin. The high-performance fluorine-containing cyanate resin system has a wide application prospect in the fields of high-performance wave-transmitting materials, 5G communication and the like.

Description

technical field [0001] The invention belongs to the scientific and technical field of advanced polymer materials, and relates to a high-performance fluorine-containing cyanate resin system and a preparation method. Background technique [0002] As a high-performance resin matrix, cyanate resin has the advantages of excellent dielectric properties, good heat resistance, small curing shrinkage and excellent processing performance, so it is widely used in electronics and aerospace and other fields. However, the triazine ring structure formed after curing of cyanate resin is highly symmetrical and has a high degree of crystallinity, resulting in high brittleness of the cured product, which severely limits its application. At present, although various cyanate ester modification methods can improve its toughness to a certain extent, it will reduce its original excellent dielectric properties and heat resistance. Therefore, simultaneously improving the toughness, heat resistance ...

Claims

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Application Information

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IPC IPC(8): C08L79/04C08L83/08C08G77/24
CPCC08L79/04C08G77/24C08L2205/05C08L2201/08C08L83/08
Inventor 颜红侠刘锐杨开明张运生张渊博杜尚
Owner NORTHWESTERN POLYTECHNICAL UNIV
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