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Quinoxaline diamine type polybenzoxazine foam material and preparation method

A technology of quinoxaline diamine type and polybenzoxazine, which is applied in the field of organic polymer materials, can solve the problems of rare reports on benzoxazine foam materials, achieve simple preparation methods, excellent flame retardant properties, The effect of good heat resistance and flame retardancy

Active Publication Date: 2016-03-02
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as a new type of phenolic resin, there are few reports on benzoxazine foam materials

Method used

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  • Quinoxaline diamine type polybenzoxazine foam material and preparation method
  • Quinoxaline diamine type polybenzoxazine foam material and preparation method
  • Quinoxaline diamine type polybenzoxazine foam material and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Add 3-dinitrobenzil (30.0g) and o-phenylenediamine (11.9g) and 50mL of glacial acetic acid to a three-necked flask respectively, and the mixture is refluxed for 7h, then cooled to room temperature, and the formed Precipitate, dry, and recrystallize the obtained crude product twice with glacial acetic acid to obtain 2,3-bis(3-nitrophenyl)quinoxaline with a yield of 85.2%;

[0024] (2) 2,3-bis(3-nitrophenyl)quinoxaline (18.6g) and palladium carbon catalyst (0.7g) were added in 300mL ethanol, then 80% hydrazine hydrate (8.8g) was added dropwise , reacted at reflux temperature for 8 hours, filtered while it was hot, removed the palladium carbon catalyst, cooled the filtrate to room temperature, precipitated crystals, filtered, washed with distilled water for 3 to 4 times, and finally dried in vacuum to obtain 2,3-bis(3- Aminophenyl) quinoxaline, yield 91.2%;

[0025] (3) Add 50mL xylene, 2,3-bis(3-aminophenyl)quinoxaline (15.6g), phenol (9.4g) and polymer Formaldehyde...

Embodiment 2

[0029] Except that the phenol in the synthesis step (3) is replaced by 4-phenoxyphenol (18.6g), other conditions are the same as in Example 1 to obtain the p-phenoxyphenol-quinoxalinyl benzoxazine monomer with a yield of 78.3 %; Proton NMR spectrum test result (500M, CDCl 3 , ppm): 6.55~8.16 (m, 28H, Ar-H), 5.10 (s, 4H, O-CH 2 -N), 4.28(s,4H,Ar-CH 2 -N); infrared spectrum test results (KBr, cm -1 ): 1321, 1234, 1070, 1160 and 947.

[0030] The curing and testing conditions were the same as in Example 1, and the polybenzoxazine foam Poly(B-DAMQ-p-pop) was obtained, and the properties are shown in Table 1.

Embodiment 3

[0032] Except that the phenol in the synthesis step (3) is replaced by 4-methoxyphenol (12.4g), other conditions are the same as in Example 1 to obtain the p-methoxyphenol-quinoxalinyl benzoxazine monomer with a yield of 78.3 %; Proton NMR spectrum test result (500M, CDCl 3 , ppm): 6.56~8.17 (m, 18H, Ar-H), 5.08 (s, 4H, O-CH 2 -N), 4.29(s, 4H, Ar-CH 2 -N), 3.75(s, 6H, -OCH 3 ); infrared spectrum test results (KBr, cm -1 ): 1322, 1233, 1073, 1158 and 950.

[0033] The curing and testing conditions were the same as those in Example 1, and finally the benzoxazine foam Poly(B-DAMQ-p-omp) was obtained, and the properties are shown in Table 1.

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Abstract

The invention discloses a quinoxaline diamine type polybenzoxazine foam material and a preparation method. The method includes the steps that 3-dinitrobenzil and o-phenylenediamine are used as raw materials, so that 2,3-bis(3-nitrophenyl)quinoxaline is synthesized; 2,3-bis(3-phenyl)quinoxaline is obtained through catalytic reduction, and then undergoes an Mannich condensation reaction with a phenolic compound and paraformaldehyde, so that a diamine type quinoxaline-based benzoxazine monomer is obtained; quinoxaline-based polybenzoxazine foam is obtained through temperature programming thermocuring. The diamine type benzoxazine foam which is prepared through the method and is of a quinoxaline structure has good flame resistance, heat and humidity resistance and low dielectric losses; no extra foaming agents need to be added in the polybenzoxazine foam, and the preparation method is simple; the foam material has good heat resistance and flame resistance and can be applied to various fields such as heat insulating materials, flame resistance materials and buoyancy materials.

Description

technical field [0001] The invention relates to an organic polymer material, and also relates to a preparation method of the organic polymer material. Specifically, it relates to a diamine-type polybenzoxazine foam material containing quinoxaline structure and a preparation method thereof. Background technique [0002] Foam polymers are aggregates formed by gas dispersion in solid polymers. This polymer has excellent properties such as low density, low thermal conductivity, heat insulation, sound absorption and cushioning, and is widely used in various fields, such as thermal insulation materials, shock-absorbing packaging materials, floating materials, gasket materials, electrical insulation materials etc. Common foam polymers include polyurethane (PU), polystyrene (PS), polyethylene (PE), phenolic foam, etc. Among them, phenolic foam has good heat resistance, low temperature shrinkage, and resistance to heat. The characteristics of good flammability and dimensional stab...

Claims

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Application Information

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IPC IPC(8): C08G73/06C08G101/00
Inventor 刘文彬冯甜甜王军桑梓车智慧
Owner HARBIN ENG UNIV
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