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Bisphenol A type bis-phthalonitrile resin with aryl ether nitrile segments, cured product and preparation method thereof

A technology of phthalonitrile resin and bisphthalonitrile, which is applied to the preparation of carboxylic acid nitrile, chemical instruments and methods, and the preparation of organic compounds, can solve the problem of low melting point, post-curing temperature preparation method, The post-curing temperature is high and the problems have not been well solved, so as to achieve the effect of excellent curing molding performance, lower curing processing temperature, and wide processing temperature window

Inactive Publication Date: 2010-12-15
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the lowering of the melting point widens the processing temperature window, the problem of too high post-curing temperature has not been well resolved.
[0005] At present, there is no report on the preparation method of bisphenol A type bis-phthalonitrile resin containing aryl ether nitrile segment with low melting point and relatively low post-curing temperature and its cured product

Method used

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  • Bisphenol A type bis-phthalonitrile resin with aryl ether nitrile segments, cured product and preparation method thereof
  • Bisphenol A type bis-phthalonitrile resin with aryl ether nitrile segments, cured product and preparation method thereof
  • Bisphenol A type bis-phthalonitrile resin with aryl ether nitrile segments, cured product and preparation method thereof

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Embodiment 1

[0060] Preparation of bisphenol A type bis-phthalonitrile resin containing aryl ether nitrile chain segment (n=2) and cured product of the present invention

[0061] (1) Synthesis of bisphenol A type bis-phthalonitrile resin containing aryl ether nitrile segment (n=2):

[0062] Step 1: Add bisphenol A, 2,6-dichlorobenzonitrile, anhydrous potassium carbonate, N,N-dimethylformamide / toluene mixed solvent into a reaction vessel with water separation device, heat to 130 ℃ reflux reaction for 6 hours; then release the by-product water and toluene generated by the reaction in the water separator, continue to raise the temperature to distill out the residual toluene in the reaction system, and then cool to room temperature.

[0063] Step 2: Add 4-nitrobisphthalonitrile to the reaction vessel with the water separation device described in step 1, and react at 90° C. for 6 hours.

[0064] Step 3: Pour the reaction mixture of step 2 into 0.1mol / L HCl solution to precipitate, filter, wash...

Embodiment 2

[0074] The invention relates to the preparation of the bisphenol A type bisphthalonitrile resin containing aryl ether nitrile chain segment (n=4) and its cured product.

[0075] (1) Synthesis of bisphenol A type bis-phthalonitrile resin containing aryl ether nitrile segment (n=4):

[0076] Step 1: Add bisphenol A, 2,6-dichlorobenzonitrile, anhydrous potassium carbonate, N,N-dimethylformamide / toluene mixed solvent into a reaction vessel with a water separator, heat to 150 Reflux reaction at ℃ for 3.5 hours; then release the by-product water and toluene generated by the reaction in the water separator, continue to raise the temperature to distill out the residual toluene in the reaction system, and then cool to room temperature.

[0077] Step 2: Add 4-nitrobisphthalonitrile to the reaction vessel with the water separation device described in step 1, and react at 85° C. for 9.5 hours.

[0078] Step 3: Pour the reaction mixture of step 2 into 0.1mol / L HCl solution to precipitate,...

Embodiment 3

[0088] The invention relates to the preparation of the bisphenol A type bisphthalonitrile resin containing aryl ether nitrile chain segment (n=6) and its cured product.

[0089](1) Synthesis of bisphenol A type bis-phthalonitrile resin containing aryl ether nitrile segment (n=6):

[0090] Step 1: Add bisphenol A, 2,6-dichlorobenzonitrile, anhydrous potassium carbonate, and N-methylpyrrolidone / toluene mixed solvent into a reaction vessel with a water separation device, and heat to 160°C for reflux reaction 3 hour; Then emit the by-product water and toluene generated by the reaction in the water trap, continue to heat up and distill out the residual toluene in the reaction system and then cool to room temperature.

[0091] Step 2: Put 4-nitrobisphthalonitrile into the reaction vessel with the water separation device described in step 1, and react at 90° C. for 9 hours.

[0092] Step 3: Pour the reaction mixture of step 2 into 0.1mol / L HCl solution to precipitate, filter, wash w...

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Abstract

The invention discloses a bisphenol A type bis-phthalonitrile resin with aryl ether nitrile segments, a cured product and a preparation method thereof and belongs to the field of polymer materials. Raw materials of bisphenol A and 2,6-dichlorobenzonitrile are subjected to nucleophilic substitution reaction, anhydrous potassium carbonate and anhydrous sodium carbonate are used as a catalyst, a hydroxyl-terminated bisphenol A type oligomer intermediate is formed in mixed liquor of a strong polar solvent and toluene, and then hydroxyl groups are substituted by 4-nitrophthalonitrile, thus obtaining the resin. A cure-crosslinking agent, the mass of which is equal to 5 percent of the resin, is added into the resin, and then after pre-curing at 220-240DEG C and heat treatment at 375DEG C at least, the cured product of the resin can be obtained. The bis-phthalonitrile resin provided by the invention has different chain lengths and the aryl ether nitrile segments as well as a low melting point and wider curing process temperature, and the cured product is of a net structure which comprises a phthalocyanine ring and a triazine ring and has excellent heat stability. The manufacturing methods of the resin and the cured product are simple and controllable and are suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of polymer materials, and relates to a bisphenol A type bisphthalonitrile resin containing an aromatic ether nitrile chain segment, a cured product and a preparation method thereof. Background technique [0002] Phthalonitrile resin was first developed by Keller and his team in the US Naval Laboratory in the 1980s as a new material with high temperature resistance. Due to the good thermal stability and mechanical properties of fully cured phthalonitrile polymers, as well as good thermo-oxidative stability, flame retardancy and high moisture resistance, such resins are used in aerospace, ships, It has a wide range of uses in the fields of microelectronics and mechanical manufacturing. [0003] Bis-phthalonitrile (BPh) is currently the most mature high-performance thermosetting resin matrix (monomer) studied, which can form a polymer (cured product) with high cross-linking density under the action of a cross-linking ag...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/54C07C253/30C08G73/06
Inventor 杨小莉杜荣华雷雅杰张建东钟家春刘孝波
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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