Phthalonitrile modified benzoxazine and epoxy resin composite material, preparation and application

A technology of phthalonitrile and epoxy resin, which is applied in the direction of organic chemistry, can solve the problems of insufficient thermal stability, high brittleness of cured products, high curing reaction temperature, etc., and achieve high yield, shortened synthesis cycle, and preparation method easy effect

Inactive Publication Date: 2016-01-20
国科广化(南雄)新材料研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But it also has obvious disadvantages, such as high curing reaction temperature, high brittle

Method used

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  • Phthalonitrile modified benzoxazine and epoxy resin composite material, preparation and application
  • Phthalonitrile modified benzoxazine and epoxy resin composite material, preparation and application
  • Phthalonitrile modified benzoxazine and epoxy resin composite material, preparation and application

Examples

Experimental program
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Effect test

Example Embodiment

[0040] Example 1

[0041] A 500 mL flask equipped with a magnetic stirrer was added with 9.91 g (0.05 mol) 4,4'-diaminodiphenylmethane, 6.00 g (0.20 mol) paraformaldehyde and 250 mL chloroform. The mixture was stirred in an ice bath for 30 minutes, and 22.83 g (0.10 mol) of bisphenol A was added, and then gradually heated to 60° C. to reflux and kept at reflux for 12 hours. After the reaction was cooled to room temperature, anhydrous sodium sulfate was added, dried for 12 hours, and then filtered. The filtrate was rotary evaporated to remove the solvent. The residue was dissolved in 250mL of dried DMF. After the dissolution was completed, 17.31g (0.10mol) of 4-nitrate was added sequentially. After adding phthalonitrile and 27.64 g (0.20 mol) of anhydrous potassium carbonate, the mixture was stirred and reacted at room temperature for 24 hours. After the completion of the reaction, the reaction mixture was poured into a large amount of water to precipitate, the precipitate was co...

Example Embodiment

[0043] Example 2

[0044] A 500 mL flask equipped with a magnetic stirrer was charged with 9.91 g (0.05 mol) 4,4'-diaminodiphenylmethane, 6.00 g (0.20 mol) paraformaldehyde and 250 mL dioxane. The mixture was stirred in an ice bath for 30 minutes, 22.83 g (0.10 mol) of bisphenol A was added, and then the temperature was gradually raised to 100° C. to reflux and kept at reflux for 8 hours. After the reaction was cooled to room temperature, anhydrous sodium sulfate was added, dried for 12 hours, and then filtered. The filtrate was rotary evaporated to remove the solvent. The residue was dissolved in 250mL of dried DMF. After the dissolution was completed, 17.31g (0.10mol) of 4-nitrate was added sequentially. After adding phthalonitrile and 27.64g (0.20mol) anhydrous potassium carbonate, the reaction was stirred at 60°C for 6 hours. After the completion of the reaction, the reaction mixture was poured into a large amount of water to precipitate, the precipitate was collected by fil...

Example Embodiment

[0045] Example 3

[0046] A 500 mL flask equipped with a magnetic stirrer was charged with 9.91 g (0.05 mol) 4,4'-diaminodiphenylmethane, 6.00 g (0.20 mol) paraformaldehyde and 250 mL dimethyl sulfoxide. The mixture was stirred in an ice bath for 30 minutes, 22.83g (0.10mol) of bisphenol A was added, and then the temperature was gradually raised to 120°C for 6 hours. After the reaction was cooled to room temperature, anhydrous sodium sulfate was added, dried for 12 hours and filtered to obtain a DMSO solution of the product, and then 17.31g (0.10mol) 4-nitrophthalonitrile and 43.25g (0.20mol) were sequentially added to it. After adding anhydrous tripotassium phosphate, stir and react at room temperature for 24 hours. After the completion of the reaction, the reaction mixture was poured into a large amount of water to precipitate, the precipitate was collected by filtration and washed with water and ethanol several times to remove impurities. The compound of general formula 1 wa...

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Abstract

The invention discloses a phthalonitrile modified benzoxazine and epoxy resin composite material, preparation and an application. According to the invention, phthalonitrile modified benzoxazine and epoxy resin are composited, and the hthalonitrile modified benzoxazine and epoxy resin composite material is a novel high-performance thermoset polymer composite material; phenolic hydroxyl groups produced through benzoxazine curing not only can be taken as a phthalonitrile curing catalyst, but also can be taken as an epoxy resin curing agent, through synthetic curing of phthalonitrile, benzoxazine and epoxy resin, the crosslinking density of the material is further increased, and properties such as thermal oxidation stability, radiation resistance, high temperature resistance, flame retardancy, corrosion resistance, low water absorption property and the like are further improved, so that the material has excellent comprehensive performance to attract broad attention and is taken as high-performance resin material for wide application in the high-technology fields such as electronic industry, aerospace and the like. According to the monomer preparation method, the synthesis period is greatly shortened, raw materials for monomer synthesis are cheap and easily available, the preparation method is simple and convenient, and the yield is high. The related processing technology of the composite material is simple, and the performance is good.

Description

technical field [0001] The invention belongs to the field of benzoxazine and epoxy resin in polymer synthetic materials, and specifically relates to a composite material of benzoxazine and epoxy resin modified by phthalonitrile, its preparation method and application. Background technique [0002] Epoxy resins generally refer to organic compounds containing two or more epoxy groups in the molecule. Due to the active epoxy groups in the molecular structure, they can undergo cross-linking reactions with various types of curing agents. It forms an insoluble polymer with a three-way network structure. The cured epoxy resin has good physical and chemical properties, such as high bonding strength, good dielectric properties, small curing shrinkage, good dimensional stability, high hardness, good flexibility, and is resistant to alkalis and most solvents. Stable, so it is widely used in various sectors of national defense and national economy for pouring, impregnation, lamination,...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08L79/04C08G73/06C08G59/62C07D265/16
Inventor 吕满庚郑剑王莹梁利岩吴昆
Owner 国科广化(南雄)新材料研究院有限公司
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