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Autocatalytic nitrile resin monomer, polymer and preparation method of polymer

A nitrile-based resin and polymer technology, applied in the field of organic polymer materials, can solve the problems of limited resin processability and comprehensive application, slow thermal curing reaction, narrow processing temperature window, etc., and achieves low curing temperature suitable for industrial production. , The method is simple and controllable

Active Publication Date: 2014-03-26
UNIV OF ELECTRONIC SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the melting temperature of bisphenol A bisphthalonitrile resin (monomer) is as high as 200 °C, which is only 20 °C lower than its curing reaction temperature, which makes its processing temperature window narrow (~20 °C), and its The thermal curing reaction is also relatively slow. If it is only thermal curing, it needs to be treated at 280 for nearly 100 hours to observe the obvious gel phenomenon.
Therefore, the high processing temperature, low curing rate and high post-curing temperature of phthalonitrile resins severely limit the processability and comprehensive application of such resins.

Method used

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  • Autocatalytic nitrile resin monomer, polymer and preparation method of polymer
  • Autocatalytic nitrile resin monomer, polymer and preparation method of polymer
  • Autocatalytic nitrile resin monomer, polymer and preparation method of polymer

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Experimental program
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Effect test

Embodiment 1

[0054] (1) A kind of synthetic method of described nitrile-based resin monomer

[0055] Step 1: Add diallyl bisphenol A, anhydrous potassium carbonate and dimethyl sulfoxide into a dry reaction vessel, heat in a water bath to 60° C., and reflux for 5 hours.

[0056] Step 2: Add 4-nitrophthalonitrile into the reaction vessel described in Step 1, and react under reflux at 60° C. for 3 hours.

[0057] Step 3: Filter the reaction mixture obtained in step 2 under anhydrous conditions.

[0058] Step 4: Pour the filtrate obtained in step 3 into clear water to precipitate and filter, and the solid obtained by filtering is washed with a large amount of clear water and then fully dried to obtain the final product nitrile resin monomer.

[0059] Wherein, the molar volume ratio of diallyl bisphenol A, anhydrous potassium carbonate, dimethyl sulfoxide and 4-nitrophthalonitrile is as follows:

[0060] Diallyl bisphenol A (grams)

137

Anhydrous Potassium Carbonate (g)

...

Embodiment 2

[0066] (1) A kind of synthetic method of described nitrile-based resin monomer

[0067] Step 1: Add diallyl bisphenol A, anhydrous calcium carbonate and N,N-dimethylformamide into a dry reaction vessel, heat in a water bath to 80°C, and reflux for 4 hours.

[0068] Step 2: Add 4-nitrophthalonitrile into the reaction vessel described in Step 1, and react under reflux at 80° C. for 2 hours.

[0069] Step 3: Filter the reaction mixture obtained in step 2 under anhydrous conditions.

[0070] Step 4: Pour the filtrate obtained in step 3 into clear water to precipitate and filter, and the solid obtained by filtering is washed with a large amount of clear water and then fully dried to obtain the final product nitrile resin monomer.

[0071] Wherein, the molar volume ratio of diallyl bisphenol A, anhydrous calcium carbonate, N,N-dimethylformamide and 4-nitrophthalonitrile is as follows:

[0072] Diallyl bisphenol A (grams)

123.3

Anhydrous calcium carbonate (g)

...

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Abstract

The invention provides an autocatalytic nitrile resin monomer, a polymer and a preparation method of the polymer, belonging to the technical field of organic polymer materials. The autocatalytic nitrile resin monomer is a bisphenol A bisphthalonitrile monomer containing allyl. The nitrile resin polymer is a product obtained by heating and polymerizing the nitrile resin monomer. The nitrile resin monomer has lower curing temperature and wider process window, so that the resin monomer has better processability. The nitrile resin polymer has good curing properties such as self-flame retardance, adhesion, thermal stability and the like. The nitrile resin monomer has low-temperature curing properties of the carbon-carbon double bond. The nitrile resin polymer maintains the high temperature resistance of the nitrile resin and can be widely applied to the fields of coatings, adhesives, electronic packaging materials, aeronautics and astronautics, ships, resin matrix composites and the like. The preparation method is simple and easy to control, is relatively low in reaction temperature and relatively short in reaction time, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic polymer materials, and relates to a self-catalyzed nitrile-based resin monomer, a polymer and a preparation method thereof. Background technique [0002] Phthalonitrile resin is a new type of high temperature resistant thermosetting resin developed by Keller and his team at the US Naval Laboratory in the 1980s. Due to the good thermal stability and mechanical properties of the fully cured phthalonitrile polymer, as well as excellent thermo-oxidative stability, flame retardancy and good moisture resistance, this type of resin is widely used in aerospace, ships, etc. It has a wide range of uses in the fields of microelectronics and machinery manufacturing, among which the most typical structures are mainly biphenyl-type bis-phthalonitrile and bisphenol A-type bis-phthalonitrile. However, the melting temperature of bisphenol A bisphthalonitrile resin (monomer) is as high as 200 °C, which is only 20 ...

Claims

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Application Information

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IPC IPC(8): C07C255/54C07C253/30C08G73/06
Inventor 刘孝波邹兴强徐明珍
Owner UNIV OF ELECTRONIC SCI & TECH OF CHINA
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