Nitrile resin monomer, nitrile resin polymer and preparation method of nitrile resin monomer and nitrile resin polymer

A nitrile-based resin and polymer technology, applied in the field of organic polymer materials, can solve the problems of post-curing temperature limitation of resin processability and comprehensive application, narrow processing temperature window, slow thermal curing reaction, etc., to achieve excellent low-temperature curing performance, The method is simple and controllable, the effect of low softening point and viscosity and fluidity

Inactive Publication Date: 2013-03-20
UNIV OF ELECTRONICS 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 bisphthalonitrile resin (monomer) is as high as 235°C, which is only 20°C lower than its curing reaction temperature, which makes its processing temperature window too narrow, and its thermal curing reaction is very slow. Curing requires nearly 100 hours of treatment at 280°C to observe obvious gel
Therefore, the high processing temperature, low curing rate, and high post-curing temperature of phthalonitrile resin severely limit the processability and comprehensive application of this kind of resin.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) preparation of bisphenol A type nitrile resin monomer:

[0062] Step 1: Add aminophenoxyphthalonitrile, bisphenol A, formaldehyde, dioxane / toluene to a reaction vessel with a water separation device, heat to 90°C and reflux for 5 hours; then Release the by-product water and toluene generated by the reaction in the water separator, continue to heat up to distill off the residual toluene in the reaction system and then cool to room temperature.

[0063] Step 2: Add 4-nitrophthalonitrile, anhydrous potassium carbonate / anhydrous sodium carbonate and N,N-dimethylformamide to the reaction vessel with water separator described in step 1, at 80 °C for 6 hours.

[0064] Step 3: Pour the reaction mixture in step 2 into clear water to precipitate, filter, and the solidified product obtained by filtering is washed with a large amount of distilled water and then fully dried to obtain the final product bisphenol A nitrile resin monomer.

[0065] Among them, bisphenol A, m-amino...

Embodiment 2

[0072] (2) preparation of biphenyl diphenol type nitrile resin monomer:

[0073] Step 1: Add aminophenoxyphthalonitrile, biphenol, formaldehyde, and dioxane / toluene to a reaction vessel with a water separation device, and heat to 90°C for reflux reaction for 5 hours; Then discharge the by-product water and toluene generated by the reaction in the water separator, continue to heat up and distill out the residual toluene in the reaction system and then cool to room temperature.

[0074] Step 2: Add 4-nitrophthalonitrile and N,N-methylformamide into the reaction vessel with the water separator described in step 1, and react at 80° C. for 6 hours.

[0075] Step 3: Pour the reaction mixture in step 2 into clear water to precipitate, filter, and filter the obtained cured product, wash it with a large amount of distilled water, and then dry it sufficiently to obtain the final product biphenol-type nitrile resin monomer.

[0076] Among them, biphenol, m-aminophenoxyphthalonitrile, fo...

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Abstract

The invention discloses a nitrile resin monomer, a nitrile resin polymer and a preparation method of the nitrile resin monomer and the nitrile resin polymer, belonging to the technical field of organic polymer materials. The nitrile resin monomer is a tetraphthalonitrile resin monomer containing benzoxazine cycle, and the nitrile resin polymer is a product obtained by heating polymerization of the nitrile resin monomer. The nitrile resin monomer has a low viscosity, a good mobility and the processing performances of low-temperature curing and the like at a low temperature. The nitrile resin polymer has the good curing performances of self-flame resistance, adhesion, heat stability and the like. The resin monomer has the good processing performances of benzoxazine resins, and the resin polymer has the high-temperature resistance of nitrile resins, thus reducing the curing processing temperature and being capable of being used in a high-temperature temperature, namely, having the advantages of low temperature processing, medium temperature formation and high temperature use; and the resin monomer and the resin polymer can be used in the fields of coatings, adhesives, electronic packaging materials, aeronautics, astronautics, ships, resin matrix composites and the like. The preparation method is simple and easy to control, low in reaction temperature, energy-saving, and suitable for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of organic polymer materials, and relates to tetraphthalonitrile resin monomers and polymers containing part of benzoxazine rings and a preparation method thereof. Background technique [0002] As a new type of phenolic resin, benzoxazine resin not only has good heat resistance and flame retardancy, but also overcomes the shortcomings of traditional phenolic resins that release small molecules during the forming and curing process. More importantly, benzoxazine mono The body has low viscosity and good processability, and can be cured and formed at a relatively low temperature. In 1944, Holly and Cope accidentally discovered benzoxazine compounds in the synthesis of Mannich reaction products. Since 1949, Burke et al. have conducted in-depth research on the synthesis of benzoxazines and synthesized a series of compounds containing benzoxazines. In 1973, Schreiner reported for the first time the research work...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/58C07C253/30C07C317/32C07C315/04C08G73/06
Inventor 刘孝波徐明珍杨旭林
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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