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Novel phthalonitrile resin and preparation method thereof

A technology of phthalonitrile resin and phthalonitrile, which is applied in the field of thermosetting phthalonitrile resin and its preparation, can solve the problems of reducing the heat resistance and mechanical properties of the resin, so as to improve solubility and increase confusion degree, the effect of lowering the melting point

Active Publication Date: 2014-06-04
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And it has been verified by experiments that the introduction of m-phthalonitrile structure does not reduce the heat resistance and mechanical properties of the resin

Method used

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  • Novel phthalonitrile resin and preparation method thereof
  • Novel phthalonitrile resin and preparation method thereof
  • Novel phthalonitrile resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Under nitrogen protection at room temperature, 0.2 mol of 4,4'-biphenol was dissolved in 2.34 mol of N,N-dimethylformamide (DMF), and 0.3 mol of anhydrous potassium carbonate was added thereto, and the temperature was raised to 80 °C. 0.15mol of 4-nitrophthalonitrile and 0.25mol of 3-nitrophthalonitrile were dissolved in 4.68mol of DMF, and slowly added dropwise to the above solution. After the dropwise addition, the reaction was kept at 80° C. for 8 hours. After the reaction, the solution system was first lowered to room temperature, and then the solution was slowly precipitated in 5 times distilled water to obtain a brownish-yellow precipitate. The precipitate was repeatedly washed with distilled water until the filtrate was clear and the pH value was neutral, and dried in a vacuum oven at 60°C for 8 hours, a brown-yellow powder product was obtained, the product structure was shown in the following formula, and the yield was 85%.

[0082] The softening point of the re...

Embodiment 2

[0086] Under the protection of nitrogen at room temperature, 0.2mol bisphenol A and 0.1mol4,4'-difluorobenzophenone were dissolved in 7.2mol N-methylpyrrolidone (NMP), and 0.4mol anhydrous potassium carbonate was added to it, and the temperature was raised to 100 ℃, stirred and reacted for 1 hour, then filled the water separator with toluene, added 20 ml of toluene to the reaction system, heated to 170-175 ℃ and refluxed for 14 hours, and removed the water generated by the reaction. The reaction solution was cooled to 60°C, 0.05mol of 4-nitrophthalonitrile and 0.05mol of 3-nitrophthalonitrile were dissolved in 2.34mol of NMP, and slowly added dropwise to the above solution. The reaction was kept at 60°C for 6 hours. After the reaction is completed, the solution system is first lowered to room temperature, and then the solution is slowly precipitated in a 5-fold dilute hydrochloric acid distilled aqueous solution to obtain a brown precipitate, and the precipitate is repeatedly ...

Embodiment 3

[0089] Under the protection of argon at room temperature, 0.3mol of hydroquinone and 0.2mol of isophthalic dibromide were dissolved in 10.8mol of N,N-dimethylformamide (DMF), and 0.0064mol of 1,10-o-dinitrogen was added to it. Miscellaneous phenanthrene, 0.0035mol cuprous iodide and 0.7mol anhydrous potassium carbonate, then fill the water separator with toluene, add 20ml toluene to the reaction system, heat up to 140-145°C for reflux reaction for 16 hours, no more water generate. The reaction solution was cooled to 80°C, 0.025mol of 4-nitrophthalonitrile and 0.075mol of 3-nitrophthalonitrile were dissolved in 2.34mol of DMF, and slowly added dropwise to the above solution. The reaction was kept at 80°C for 8 hours. After the reaction is completed, the solution system is first lowered to room temperature, and then the solution is slowly precipitated in a 6-fold dilute hydrochloric acid ice-water solution to obtain a brown precipitate, which is repeatedly washed with ice-water...

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Abstract

The invention discloses a novel phthalonitrile resin and a preparation method thereof. Compared with a conventional phthalonitrile resin (only 4-nitro phthalonitrile as an end-capping reagent, the novel phthalonitrile resin is introduced with 3-nitro novel phthalonitrile resin to cooperate end capping, and thus the asymmetry of a resin structure is increased and the turbidity of a resin component is increased (see a formula 1). Compared with the conventional phthalonitrile resin, the novel phthalonitrile resin disclosed by the invention has the characteristics of low melting temperature, good solubility, wide processing window, low curing temperature and the like; a prepared resin molded part and a resin-based composite material are low in porosity, excellent heat-resistant quality, and high in mechanical property, and can be applied to the fields of aerospace, a space technology, machine manufacturing, and the like as a light-weight and high-temperature resistant part. The formula is described in the specification.

Description

technical field [0001] The invention relates to a thermosetting phthalonitrile resin and a preparation method thereof Background technique [0002] Resin Matrix Composite is a kind of composite material with mature technology and wide application. Raw materials for resin matrix composites, including matrix phase and reinforcement phase and additives. The matrix phase material refers to various polymers as the matrix, including thermosetting resins and thermoplastic resins, and the reinforcing phase refers to various fibers, such as glass fibers, carbon fibers, aramid fibers, and high-density polyethylene fibers. [0003] The thermosetting matrix resin of resin-based composite materials mainly includes three categories: epoxy resin, bis-horse resin and polyimide resin. Among them, only the temperature resistance level of polyimide can reach and exceed 300 ℃. Phthalonitrile resins are another class of resin systems that are considered to have a temperature rating in excess o...

Claims

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Application Information

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IPC IPC(8): C08G73/06B32B27/04B32B27/28
Inventor 周恒赵彤韩悦
Owner INST OF CHEM CHINESE ACAD OF SCI
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