Cyanate ester resin modified by phosphoric hybridization and preparation method of cyanate ester resin

A cyanate ester resin and cyanate ester technology, which is applied in the field of phosphorus-containing hybrid graphene oxide modified cyanate resin and its preparation, can solve the problem of modified CE resin with low phosphorus content and low dielectric constant of deviated CE resin , Dielectric constant and loss increase, to achieve the effect of low phosphorus content, excellent carbon forming ability, and outstanding heat resistance

Active Publication Date: 2015-11-18
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The study found that with the increase of EPHSi-g-MWCNT content, the improvement of flame retardancy of modified CE resin increased, but the dielectric constant and loss increased significantly, which seriously deviated from the advantages of low dielectric constant of CE resin.
[0007] In summary, in the prior art, under the premise of basically maintaining the original thermal stability and dielectric properties of CE resin, the modified CE resin with greatly improved flame retardancy and low phosphorus content (≤0.1wt%) has not yet been developed. reported

Method used

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  • Cyanate ester resin modified by phosphoric hybridization and preparation method of cyanate ester resin
  • Cyanate ester resin modified by phosphoric hybridization and preparation method of cyanate ester resin
  • Cyanate ester resin modified by phosphoric hybridization and preparation method of cyanate ester resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. Preparation of phosphorus-containing hybrid graphene oxide flame retardant

[0039] Add 0.1g of graphene oxide to 100g of tetrahydrofuran, and ultrasonically disperse for 1 hour to obtain a fully mixed system A; under the condition of nitrogen protection and stirring, add 5g of triethylamine to system A, and react at 0°C for 1 hour to obtain system B ; Dissolve 1g of phosphazene in 20g of tetrahydrofuran to obtain system C; add system C dropwise to system B, and react at 3°C ​​for 2h; then raise the temperature to 60°C and react for 3h to obtain system D; 3.8g3 -Aminopropyltriethoxysilane was dissolved in 20g tetrahydrofuran to obtain system E; system E was added dropwise to system D, and reacted at 60°C for 3 hours to obtain system F; 0.4g water was added dropwise to In system F, react at 60°C for 3h; then react at 20°C for 10h. After the reaction, filter, wash with tetrahydrofuran and ethanol for 5 times, and dry in a vacuum oven at 60°C for 10 hours to obtain pho...

Embodiment 2

[0065] Add 0.25g of phosphorus-containing hybrid graphene oxide flame retardant prepared in Step 1 of Example 1 and 49.75g of 4,4'-dicyanato-diphenylpropane (bisphenol A cyanate) into the beaker , ultrasonically stirred at 85°C for 15min, and then mechanically stirred at 190°C for 6h to obtain a prepolymer; pour the prepolymer into a mold preheated at 190°C, and then defoam under vacuum at 190°C for 0.5h Put it in an oven, perform curing and post-treatment according to the processes of 200°C / 2h+220°C / 2h and 240°C / 4h, and naturally cool to room temperature to obtain a phosphorus-containing hybrid graphene oxide modified cyanate resin, which contains Phosphorus content is 0.055wt%, Tdi is 434.5℃, PHRR is 243.0kW / m 2 , the TTI is 85s, the LOI is 28.1, and the dielectric constant and loss at 1Hz are 3.6 and 0.007, respectively. Compared with CE resin, Tdi is slightly increased, PHRR is reduced by 20.5%, TTI is extended by 14s, and the dielectric properties are close to CE resin. ...

Embodiment 3

[0067] 1. Preparation of phosphorus-containing hybrid graphene oxide flame retardant

[0068] Add 0.1g of graphene oxide to 50g of tetrahydrofuran, and stir mechanically for 50 minutes to obtain a fully mixed system A; under argon protection and stirring conditions, add 1g of triethylamine to system A and react at 0°C for 0.5h to obtain System B; Dissolve 0.1g of phosphazene in 10g of tetrahydrofuran to obtain system C; add system C dropwise to system B and react at 4°C for 1h; then raise the temperature to 40°C and react for 2h to obtain system D; 2gγ -Aminopropyltrimethoxysilane was dissolved in 10g tetrahydrofuran to obtain system E; system E was added dropwise to system D, and reacted at 45°C for 2 hours to obtain system F; 0.4g water was added dropwise to In system F, react at 60°C for 2h; then react at 15°C for 10h. After the reaction, after filtering, washing with tetrahydrofuran and ethanol five times respectively, and drying in a vacuum oven at 60°C for 10 h, a phosp...

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Abstract

The invention discloses cyanate ester resin modified by phosphoric hybridization and a preparation method of the cyanate ester resin. The preparation method comprises the steps of: enabling oxidized graphene, a phosphonitrilic chloride trimer and hyperbranched polysiloxane to react so as to obtain phosphoric hybridization oxidized graphene formed under the action of chemical bonds of the oxidized grapheme, the phosphonitrilic chloride trimer and the hyperbranched polysiloxane; and then, uniformly mixing molten cyanate ester resin and the phosphoric hybridization oxidized graphene so as to obtain a mixture, and performing curing process on the mixture so as to obtain the cyanate ester modified by the phosphoric hybridization oxidized graphene. Compared with the cyanate ester resin, on the basis that a prominent dielectric property of conventional cyanate ester resin is basically maintained, under the condition that the phosphorus content is below 0.10wt%, the cyanate ester modified by the phosphoric hybridization oxidized graphene, prepared by the method disclosed by the invention, has excellent thermal properties and fire resistance properties, and solves the problems that according to the thermosetting resin modified by a general phosphoric fire retardant, the initial heat decomposition temperature is reduced, the start igniting time is shortened, and the dielectric property is notably reduced. The preparation method provided by the invention also has the characteristics of simple technology, low cost, wide source of raw materials, and the like.

Description

technical field [0001] The invention relates to a thermosetting resin and a preparation method thereof, in particular to a phosphorus-containing hybrid graphene oxide modified cyanate resin and a preparation method thereof. Background technique [0002] "High heat resistance", "high flame retardancy" and "environmental protection" have become key words in the development of high-performance materials, as well as the development of heat-resistant thermosetting resins, which are indispensable in some cutting-edge fields. Cyanate ester (CE) resin is currently a representative variety of heat-resistant thermosetting resins. Its very low dielectric constant (2.6-3.2) and dielectric loss (0.001-0.008) have become important indicators that distinguish it from other thermosetting resins. In recent years, more and more work has been done on the modification of CE resins. How to greatly improve the flame retardancy while maintaining the original outstanding heat resistance and excelle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C08L79/04C08K9/04C08K9/06C08K3/04
Inventor 顾嫒娟张志娟梁国正袁莉
Owner SUZHOU UNIV
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