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Bisphenol A cyanate ester resin prepolymer and preparation method thereof

A type of cyanate ester and prepolymer technology, applied in the field of cyanate ester resin, can solve the problems of increasing the stability and storage time of the prepolymer, improve the polymerization curing efficiency, increase the toughness and heat resistance and flame retardant performance, The effect of increasing the curing reaction rate

Active Publication Date: 2020-10-30
YANGZHOU TECHIA MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, on the basis of improving the polymerization and curing efficiency of bisphenol A cyanate ester monomers, the toughness, heat resistance and flame retardancy, and hygroscopicity still need to be improved to further increase the stability and storage time of the prepolymer.

Method used

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  • Bisphenol A cyanate ester resin prepolymer and preparation method thereof
  • Bisphenol A cyanate ester resin prepolymer and preparation method thereof
  • Bisphenol A cyanate ester resin prepolymer and preparation method thereof

Examples

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Effect test

Embodiment 1

[0029] A bisphenol A cyanate ester resin prepolymer of this embodiment is composed of bisphenol A cyanate ester monomers, polymerization compatible catalysts, and composite hygroscopic agents through heat preservation and stirring reaction. When the refractive index reaches 1.586, the temperature is lowered , Post-processing;

[0030] The synthesis reaction formula of the polymerization compatible catalyst is as follows:

[0031]

[0032] The composite moisture absorbent is obtained by polymerization reaction of diatomaceous earth, anhydrous magnesium sulfate and super absorbent acrylic resin under the action of a crosslinking agent and an initiator.

[0033] The preparation method of the polymerization compatible catalyst is as follows:

[0034] S1. Add 930g (6.2mol) of 4-hydroxy-1,3-phthalaldehyde, 16740g of solvent tetrahydrofuran, and then add 647.62g (6.4mol) of triethylamine to the reaction kettle, increase the temperature to 70°C, and stir at 460rpm. 346.74g (1mol) of hexachlo...

Embodiment 2

[0041] The bisphenol A cyanate ester resin prepolymer of this embodiment is composed of bisphenol A cyanate ester monomer, polymerization compatible catalyst, and composite moisture absorbent after heat preservation and stirring reaction. When the refractive index reaches 1.587, the temperature is lowered , Post-processing;

[0042] The synthesis reaction formula of the polymerization compatible catalyst is as follows:

[0043]

[0044] The composite moisture absorbent is obtained by polymerization reaction of diatomaceous earth, anhydrous magnesium sulfate and super absorbent acrylic resin under the action of a crosslinking agent and an initiator.

[0045] The preparation method of the polymerization compatible catalyst is as follows:

[0046] S1. Add 918g (6.12mol) of 4-hydroxy-1,3-phthalaldehyde, 17442g of solvent tetrahydrofuran to the reaction kettle, then add 637.50g (6.3mol) of triethylamine, raise the temperature to 69°C, stir at 500rpm, 346.74g (1mol) of hexachlorocyclotriph...

Embodiment 3

[0053] A bisphenol A cyanate ester resin prepolymer of this embodiment consists of a bisphenol A cyanate ester monomer, a polymerization compatible catalyst, and a composite hygroscopic agent through heat preservation and stirring reaction. When the refractive index reaches 1.584, the temperature is lowered , Post-processing;

[0054] The synthesis reaction formula of the polymerization compatible catalyst is as follows:

[0055]

[0056] The composite moisture absorbent is obtained by polymerization reaction of diatomaceous earth, anhydrous magnesium sulfate and super absorbent acrylic resin under the action of a crosslinking agent and an initiator.

[0057] The preparation method of the polymerization compatible catalyst is as follows:

[0058] S1. Add 927g (6.18mol) of 4-hydroxy-1,3-phthalaldehyde, 12051g of solvent tetrahydrofuran to the reaction kettle, then add 632.44g (6.25mol) of triethylamine, raise the temperature to 69°C, stir at 490rpm, 346.74g (1mol) of hexachlorocyclotr...

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Abstract

The invention discloses a bisphenol A cyanate ester resin prepolymer and a preparation method thereof. The preparation method comprises the following steps of: heating and melting a bisphenol A type cyanate ester monomer, adding a prepared polymerization compatible catalyst and a composite moisture absorbent, carrying out a heat preservation reaction, terminating the reaction by monitoring a refraction coefficient, cooling, adding butanone, and cooling to obtain the bisphenol A type cyanate ester resin prepolymer. Compared with the traditional bisphenol A type cyanate ester resin prepolymer, the prepolymer has the advantages that the cyclic structure of cyclotriphosphazene has good compatibility with a bisphenol A type cyanate ester monomer and can participate in the polymerization reaction of the bisphenol A type cyanate ester monomer, the curing reaction rate is greatly increased, rigid units of a phosphazene ring and a benzene ring greatly improve the toughness of the prepolymer anddo not influence the tensile strength and the thermal performance, the cyclotriphosphazene core can exert a phosphorus-nitrogen synergistic flame-retardant effect, and the polymerization compatible catalyst improves the polymerization curing efficiency of the bisphenol A type cyanate ester monomer, and improves the toughness, heat resistance and flame retardancy of the bisphenol A type cyanate ester resin prepolymer.

Description

Technical field [0001] The invention relates to the technical field of cyanate ester resins, in particular to a bisphenol A type cyanate ester resin prepolymer and a preparation method thereof. Background technique [0002] Cyanate ester resin is a new type of high-performance thermosetting resin. Its monomer contains two or more cyanate ester functional groups (-OCN). After curing reaction, it forms a highly crosslinked triazine cyclized polymer. The outstanding performance feature is excellent dielectric performance, with very low dielectric constant (ε=2.64-3.11) and dielectric loss value (tgδ=0.001-0.008) in a wide frequency range from X-band to W-band. In addition, it also has outstanding heat resistance, excellent mechanical properties, and low moisture absorption. Therefore, it is used in cutting-edge fields including microelectronics, aerospace, aerospace and other industries, especially for dielectric properties, damp and heat properties, and mechanical properties. Cyan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C07F9/6593
CPCC07F9/65815C08G73/0644C08G73/065
Inventor 王跃彪朱芝峰吕嘉木邵家伟
Owner YANGZHOU TECHIA MATERIAL CO LTD
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