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Modified cyanate resin and preparation method thereof

A cyanate ester resin and modification technology, which is applied in the field of modified cyanate resin and its preparation, can solve the adverse effects of heat resistance and dielectric properties, can not take into account the catalytic and toughening properties, and destroy the triazine ring structure and other problems, to achieve the effect of high toughness, good curing process, and good dispersibility

Active Publication Date: 2016-10-26
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nevertheless, the above method still has shortcomings. On the one hand, the above-mentioned ionic liquid supports the catalyst in two steps, and the steps are cumbersome; hot issue
[0007] CE resin has good heat resistance and excellent dielectric properties due to the unique triazine ring structure of the cured product itself, while modifiers often destroy its triazine ring structure to varying degrees, thereby affecting its heat resistance and dielectric properties. Performance is adversely affected
And any modification of CE resin cannot be at the expense of its outstanding heat resistance and dielectric properties
[0008] To sum up, the current modification technology of CE resin cannot take into account the catalytic and toughening properties, or the synthesis steps are cumbersome, especially after adding modifiers, the triazine ring structure will be destroyed to varying degrees, thereby affecting its comprehensive performance.

Method used

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  • Modified cyanate resin and preparation method thereof
  • Modified cyanate resin and preparation method thereof
  • Modified cyanate resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] The present embodiment provides a kind of preparation of modified cyanate ester curing resin, and concrete steps are as follows:

[0046] (1) Preparation of 1-vinyl N-heterocyclic-3-chloroethylamine ionic liquid containing amino-terminated

[0047] In nitrogen (N 2 ) protection, 9.4 g of N-vinylimidazole was added dropwise to 11.3 g of 2-chloroethylamine hydrochloride, and the reaction was refluxed at a temperature of 70 ° C for 24 h. After the reaction was finished, it was repeatedly washed with ethanol three times, and dried in vacuum at 25° C. for 4 hours to obtain amino-terminated ionic liquid hydrochloride A.

[0048] Add 10.5g of amino-terminated ionic liquid hydrochloride A to 21mL of water to dissolve to obtain an aqueous solution of amino-terminated ionic liquid hydrochloride A; slowly add 2.1g of NaOH to the aqueous solution of amino-terminated ionic liquid hydrochloride A, at 20°C The reaction was stirred for 5h. Then freeze-dry to remove solvent water; di...

Embodiment 2

[0065] (1) Preparation of polyionic liquid modified carbon nanotube hybrid material / cyanate resin prepolymer

[0066] 0.5g of the polyionic liquid modified carbon nanotube hybrid material prepared in step (3) of Example 1 and 49.5g of 2,2'-bis(4-cyanophenyl)propane (also known as bisphenol A cyanate ) into a beaker, stirred at 110°C and ultrasonicated for 30 minutes; then prepolymerized and stirred at 140°C for 10 minutes to obtain a polyionic liquid modified carbon nanotube hybrid material / cyanate resin prepolymer, in which the polyionic liquid modified The content of the carbon nanotube hybrid material is 1wt%. The differential scanning calorimetry (DSC) curve of this modified cyanate resin prepolymer is shown in the appendix Figure 7 .

[0067] (2) Preparation of modified cyanate ester cured resin

[0068] Pour the polyionic liquid-modified carbon nanotube hybrid material / cyanate resin prepolymer prepared above into the mold, and degas the bubbles under vacuum at 140°C ...

Embodiment 3

[0080] (1) Preparation of polyionic liquid modified carbon nanotube hybrid materials

[0081] Add 5 g of the ionic liquid D containing amino-terminated and transition metals prepared in step (2) of Example 1 into 100 mL of deionized water and fully dissolve to obtain a clear and transparent solution E. Add 2g of single-walled carbon nanotubes to the E solution, and ultrasonically disperse for 30min to obtain a uniformly dispersed single-walled carbon nanotube dispersion F; then add 10mL of azobisisobutyronitrile Methanol solution (15mg / mL), reflux at 60°C for 24h. After the reaction, it was suction filtered, washed with deionized water, and freeze-dried for 48 hours to obtain a polyionic liquid-modified carbon nanotube hybrid material.

[0082] (2) Preparation of modified cyanate ester cured resin

[0083] Add 0.5g of the polyionic liquid-modified carbon nanotube hybrid material in the above step and 49.5g of 4,4'-dicyanate-diphenylethane (bisphenol E-type cyanate) into the ...

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Abstract

The invention discloses modified cyanate resin and a preparation method thereof. The preparation method comprises the following steps: uniformly mixing 100 parts by mass of molten cyanate resin and 0.10-1.55 parts by mass of poly ionic liquid modified carbon nanotube hybrid material, and carrying out curing and after-treatment to obtain the modified cyanate resin. The synthesis process of the poly ionic liquid modified carbon nanotube hybrid material comprises the following steps: 1. synthesizing amino-terminated ionic liquid containing a transition metal; and 2. carrying out in-situ polymerization by using the ionic liquid to coat the carbon nanotubes. Compared with the cyanate resin, the modified cyanate resin prepared by the method disclosed by the invention has the advantages of favorable curing manufacturability, higher toughness, higher heat stability, stable dielectric constant and lower dielectric loss. The preparation method of the modified cyanate resin has the characteristics of simple technique, high controllability and the like.

Description

technical field [0001] The invention relates to a thermosetting resin and a preparation method thereof, in particular to a modified cyanate resin and a preparation method thereof. Background technique [0002] Since the birth of the first artificial synthetic resin, thermosetting resin has been used as an indispensable basic material in cutting-edge fields such as aerospace, new energy, electronic information and electrical insulation. With the rapid development of modern industry, more and higher requirements are put forward for thermosetting resins. These requirements mainly include excellent curing process, high toughness and heat resistance, and stable dielectric properties. [0003] Cyanate ester (CE) resin is a typical representative of heat-resistant thermosetting resins. Although it has excellent heat resistance and dielectric properties, "high temperature curing" and high brittleness are common characteristics of heat-resistant thermosetting resins. People have bee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/04C08K9/10C08K7/24
CPCC08K7/24C08K9/10C08K2201/011C08L2201/08C08L79/04
Inventor 梁国正吕文锦顾嫒娟袁莉
Owner SUZHOU UNIV
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