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Aromatic diamine type cyano group-containing benzoxazine resin and its preparation method

A technology of aromatic diamine type and oxazine resin, which is applied in the field of thermosetting resin and its preparation, can solve the problems of high brittleness, unsatisfactory process performance, high curing temperature, etc., and achieve the effect of low cost, high yield and high purity

Inactive Publication Date: 2012-06-27
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, benzoxazine also has some defects: (1) high brittleness; (2) high curing temperature; (3) heat resistance needs to be further improved
At present, research at home and abroad is mainly focused on the improvement of the carbon residue rate and heat resistance of benzoxazine resin, but its process performance is often not ideal

Method used

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  • Aromatic diamine type cyano group-containing benzoxazine resin and its preparation method
  • Aromatic diamine type cyano group-containing benzoxazine resin and its preparation method
  • Aromatic diamine type cyano group-containing benzoxazine resin and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a four-necked flask equipped with magnetic stirrer, thermometer, nitrogen pipe, water separator and spherical condenser, add 0.2mol 2,7-dihydroxynaphthalene, 0.44mol p-nitrochlorobenzene, 0.24mol potassium carbonate in turn , 60ml of toluene and 240ml of N,N-dimethylformamide; under the protection of nitrogen, the temperature was slowly raised to 145℃ and reacted at a constant temperature for 8 hours; after the reaction, the inorganic salt was filtered while hot, concentrated by rotary evaporation, and deionized water was added gradually. After cooling down to room temperature, the product slowly precipitated out; the crude product was collected by filtration and dried in vacuum for 24 hours (85°C) to obtain a dihydroxynaphthalene type aromatic dinitro compound with a yield of 99%.

[0032] In a four-necked flask equipped with a magnetic stirrer, thermometer, nitrogen pipe and spherical condenser, put 0.0375mol dihydroxynaphthalene type aromatic dinitro compound, 0.125g ...

Embodiment 2

[0036] In a four-necked flask equipped with a magnetic stirrer, thermometer, nitrogen pipe, water separator and spherical condenser, add 0.2mol 2,7-dihydroxynaphthalene, 0.4mol p-nitrochlorobenzene, 0.2mol potassium carbonate in sequence , 50ml of toluene and 240ml of N,N-dimethylformamide; under the protection of nitrogen, the temperature was slowly increased to 145℃, and the reaction was kept at a constant temperature for 8 hours; after the reaction, the inorganic salt was filtered while hot, concentrated by rotary evaporation, and deionized water was added gradually. The product was cooled to room temperature to slowly precipitate out; the crude product was collected by filtration, and dried in vacuum for 24 hours (85°C) to obtain a dihydroxynaphthalene type aromatic dinitro compound with a yield of 90%.

[0037] In a four-necked flask equipped with a magnetic stirrer, thermometer, nitrogen pipe and spherical condenser, put 0.015mol dihydroxynaphthalene type aromatic dinitro co...

Embodiment 3

[0041] In a four-necked flask equipped with a magnetic stirrer, thermometer, nitrogen pipe, water separator and spherical condenser, add 0.2mol 2,7-dihydroxynaphthalene, 0.42mol p-nitrochlorobenzene, 0.21mol potassium carbonate in sequence , 50ml of toluene and 240ml of N,N-dimethylformamide; under the protection of nitrogen, the temperature was slowly increased to 145℃, and the reaction was kept at a constant temperature for 8 hours; after the reaction, the inorganic salt was filtered while hot, concentrated by rotary evaporation, and deionized water was added gradually After cooling down to room temperature, the product was slowly precipitated out; the crude product was collected by filtration and dried in vacuum for 24 hours (85°C) to obtain a dihydroxynaphthalene type aromatic dinitro compound with a yield of 92%.

[0042] In a four-necked flask equipped with a magnetic stirrer, thermometer, nitrogen pipe and spherical condenser, put 0.015mol dihydroxynaphthalene type aromatic...

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Abstract

The invention discloses an aromatic diamine type cyano group-containing benzoxazine resin and its preparation method. The benzoxazine resin belongs to the aromatic diamine type, its monomer main chain contains benzene rings and ether bonds, and the ends of the main chain contain cyano groups. A cured monomer has high heat resistance, high rate of combustion carbon residue, and certain toughness, thus being suitable for manufacturing high temperature resistant and flame retarding materials. The preparation method of the aromatic diamine type cyano group-containing benzoxazine resin takes an aromatic diamino compound, cyano group-containing monohydric phenol and formaldehyde as reaction raw materials to synthesize a benzoxazine monomer, which is then subjected to curing and crosslinking so as to obtain the benzoxazine resin. The monomer of the resin has reasonable synthesis process, high purity, high yield and low cost. And the monomer for synthesizing the aromatic diamine type cyano group-containing benzoxazine resin has a structural formula as the following.

Description

Technical field [0001] The invention relates to a thermosetting resin and the technical field of its preparation, in particular to an aromatic diamine type cyano group-containing benzoxazine resin and a preparation method thereof. Background technique [0002] Benzoxazine resin is prepared by reacting phenolic compounds, primary amine compounds and formaldehyde to form monomers, and then crosslinking and curing under the action of heating and / or catalyst. Compared with traditional thermosetting resins, benzoxazine resins have unique advantages: (1) The volume change during curing is small; (2) Water absorption is very low; (3) Carbon residue rate is higher; (4) Curing process There is no need for strong acid as a catalyst; (5) no by-products are generated during the curing process; (6) the flexibility of molecular design is higher. However, benzoxazine also has some disadvantages: (1) brittleness; (2) high curing temperature; (3) heat resistance needs to be further improved. At...

Claims

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Application Information

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IPC IPC(8): C08G73/06
Inventor 闫红强方征平张涛
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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