Polybenzoxazine connected bisphthalonitrile monomer as well as preparation method and application thereof

A bis-phthalonitrile and polybenzoxazine technology, applied in the field of bis-phthalonitrile monomer and its preparation, can solve the problems of high curing reaction temperature, high brittleness of cured products, insufficient thermal stability, etc. , to achieve the effect of low water absorption and high carbon residue rate

Inactive Publication Date: 2016-01-20
NANXIONG MATERIAL PRODION BASE OF CHINESE ACADEMY OF SCI GUANGZHOU CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But it also has obvious disadvantages, such as high curing reaction temperature, high brittleness of cured products and insufficient thermal stability for use under many harsh conditions.

Method used

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  • Polybenzoxazine connected bisphthalonitrile monomer as well as preparation method and application thereof
  • Polybenzoxazine connected bisphthalonitrile monomer as well as preparation method and application thereof
  • Polybenzoxazine connected bisphthalonitrile monomer as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1 (n=10)

[0042] (1) Add 7.93g (0.04mol) 4,4'-diaminodiphenylmethane, 4.80g (0.16mol) paraformaldehyde and 150mL dioxane to a 250mL flask equipped with a magnetic stirrer; the mixture After stirring at room temperature for 30 minutes, 10.04 g (0.044 mol) of bisphenol A was added, and then the temperature was gradually raised to 100°C for reflux and maintained for 8 hours; after the reaction was lowered to room temperature, anhydrous sodium sulfate was added, dried for 12 hours and filtered, and the filtrate was passed through The solvent was removed by rotary evaporation to obtain compound 1;

[0043] (2) Dissolve the compound 1 prepared in step (1) with 150 mL of dry DMF, and add 1.39 g (0.008 mol) 4-nitrophthalonitrile and 2.21 g (0.016 mol) After adding anhydrous potassium carbonate, stir and react at 60°C for 2 hours. After the reaction was completed, the reaction mixture was poured into a large amount of water to precipitate, and the precipitate was coll...

Embodiment 2

[0044] Example 2 (n=5)

[0045] (1) Add 7.93g (0.04mol) 4,4'-diaminodiphenylmethane, 4.80g (0.16mol) paraformaldehyde and 150mL chloroform in a 250mL flask equipped with a magnetic stirrer; After stirring at room temperature for 30 minutes, 10.96 g (0.048 mol) of bisphenol A was added, and then the temperature was gradually raised to 60° C. for reflux and kept for 12 hours. After the reaction was lowered to room temperature, anhydrous sodium sulfate was added, dried for 12 hours and then filtered, and the filtrate was removed by rotary evaporation to obtain compound 1;

[0046] (2) Dissolve the compound 1 obtained in step (1) with 150 mL of dry DMF, and add 2.77 g (0.016 mol) 4-nitrophthalonitrile and 4.42 g (0.032 mol) After the addition of anhydrous potassium carbonate, stir the reaction at room temperature (25°C) for 24 hours. After the reaction was completed, the reaction mixture was poured into a large amount of water to precipitate, and the precipitate was collected by...

Embodiment 3

[0047] Embodiment 3 (n=1)

[0048](1) In a 250mL flask equipped with a magnetic stirrer, add 7.93g (0.04mol) 4,4'-diaminodiphenylmethane, 4.80g (0.16mol) paraformaldehyde and 150mL chloroform; After stirring at room temperature for 30 minutes, 18.26 g (0.08 mol) of bisphenol A was added, and then the temperature was gradually raised to 60° C. for reflux and kept for 12 hours. After the reaction was lowered to room temperature, anhydrous sodium sulfate was added, dried for 12 hours and then filtered, and the filtrate was removed by rotary evaporation to obtain compound 1;

[0049] (2) Dissolve the compound 1 prepared in step (1) with 150 mL of dry DMF, and add 13.85 g (0.08 mol) 4-nitrophthalonitrile and 22.11 g (0.16 mol) After the addition of anhydrous potassium carbonate, stir the reaction at room temperature (25°C) for 24 hours. After the reaction was completed, the reaction mixture was poured into a large amount of water to precipitate, and the precipitate was collected ...

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Abstract

The invention belongs to the technical field of polymer synthetic materials and particularly relates to a polybenzoxazine connected bisphthalonitrile monomer as well as a preparation method and an application thereof. The polybenzoxazine connected bisphthalonitrile monomer has a structure represented as a formula I, wherein n is an integer larger than or equal to 1. The preparation method comprises steps as follows: bisphenol A, formaldehyde and 4,4- diaminodiphenyl-methane react at the temperature of 60-120 DEG C in the presence of a solvent, and a compound 1 is obtained; the compound 1 reacts with 4-nitrophthalonitrile at the temperature of 25-60 DEG C in the presence of an alkaline reagent and a solvent, and the polybenzoxazine connected bisphthalonitrile monomer is obtained. According to the method, the synthesis period is greatly shortened, the raw materials for the monomer synthesis are cheap and easily available, the preparation method is simple and convenient, and the yield is high; a product obtained through preparation has excellent performance such as thermal oxidation stability, high temperature resistance, flame retardancy, corrosion resistance, low water absorption property, high carbon yield and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer synthetic materials, and in particular relates to a polybenzoxazine-linked bis-phthalonitrile monomer and a preparation method and application thereof. Background technique [0002] Phthalonitrile resin is a new type of high-performance thermosetting polymer material. It has attracted widespread attention due to its excellent comprehensive properties. It has been widely used as a high-performance resin material in high-tech fields such as the electronics industry and aerospace engineering. . Functional polymer materials, resin-based composite materials, magnetic functional materials and high-temperature-resistant materials can be prepared by thermal curing of phthalonitrile monomers, which have thermo-oxygen stability, radiation resistance, high temperature resistance, flame retardancy, corrosion resistance and Low water absorption and other properties. These properties make phthalonitrile resin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C07D319/08
Inventor 吕满庚郑剑王莹梁利岩吴昆
Owner NANXIONG MATERIAL PRODION BASE OF CHINESE ACADEMY OF SCI GUANGZHOU CHEM
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