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Preparation method of nitrogen and phosphorus fire retardant, nitrogen and phosphorus fire retardant and application thereof

A technology of nitrogen-phosphorus flame retardants and flame retardants, which is applied in the field of nitrogen-phosphorus flame retardants and their preparation, can solve the problems of low flame retardant efficiency and decline in comprehensive mechanical properties, and achieve low cost, high char formation rate, Achieve the effect of industrialization

Inactive Publication Date: 2012-12-26
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the additive flame retardant is dispersed in the polymer in a physical way, its flame retardant efficiency is not high, and its comprehensive mechanical properties are reduced.

Method used

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  • Preparation method of nitrogen and phosphorus fire retardant, nitrogen and phosphorus fire retardant and application thereof
  • Preparation method of nitrogen and phosphorus fire retardant, nitrogen and phosphorus fire retardant and application thereof
  • Preparation method of nitrogen and phosphorus fire retardant, nitrogen and phosphorus fire retardant and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Nitrogen phosphorus flame retardant ( 1 ) The synthetic steps are as follows:

[0029] 1) Add 10.913g of 4-aminophenol, 6.707g of 1,4-benzenedicarbaldehyde and 70.480g of absolute ethanol into a three-necked flask with a stirring device, stir at a speed of 50-400 rpm, and control the reaction temperature to React at 0°C for 2-4 h. After the reaction, the reaction mixture was suction-filtered, washed, and dried in a vacuum oven at 80°C for 8 h to obtain the imine intermediate ( 1 ), the test analysis results are as follows:

[0030] FTIR (KBr, cm -1 ): 1620 (C=N), 3421 (OH), 1596, 1498, 1445, 1355, 1244, 1193, 1101, 1010, 889, 825, 767 and other characteristic peaks.

[0031] MS: m / z=315.1146 [M-H] - .

[0032] 1 H NMR (DMSO-d 6 , ppm): δ=9.56 (2OH), 8.68 (2H), 8.00 (4H), 7.26 (4H), 6.82 (4H).

[0033] 13 C NMR (DMSO-d 6 , ppm): δ=156.5, 156.2, 142.3, 138.3, 128.4, 122.6, 115.7.

[0034] 2), the above-mentioned imine intermediate product ( 1 ) 15.820 g, DOPO...

Embodiment 2

[0044] Nitrogen phosphorus flame retardant ( 2 ) The synthetic steps are as follows:

[0045] 1) Add 10.913 g of 4-aminophenol, 10.512 g of 4,4'-biphenyldicarbaldehyde and 200.0 g of absolute ethanol into a three-necked flask with a stirring device, under the action of stirring (50-400 rpm) , the reaction temperature is 60 ° C for 2-4 h, after the reaction, the reaction mixture is suction filtered, washed, and dried in a vacuum oven at 80 ° C for 8 h to obtain the imine intermediate product ( 2 ), the test analysis results are as follows:

[0046] FTIR absorption (KBr, cm -1 ): 1620 (C=N), 3430 (OH), 1593, 1505, 1446, 1367, 1251, 1103,889, 837, 781, etc.

[0047] MS: m / z=391.1447 [M-H] - .

[0048] 1 H NMR (DMSO-d 6 , ppm): δ=9.53 (2OH), 8.69 (2H), 8.01 (4H), 7.90 (4H), 7.25 (4H), 6.82 (4H).

[0049] 13 C NMR (DMSO-d 6 , ppm): δ=157.0, 156.9, 143.0, 141.8, 136.5, 129.4, 127.5, 123.1, 116.2.

[0050] 2), the above-mentioned imine intermediate product ( 2 ) 19.625g, ...

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Abstract

The invention discloses a preparation method of a nitrogen and phosphorus fire retardant, a nitrogen and phosphorus fire retardant and an application thereof. The preparation method comprises the following steps of: carrying out condensation reaction on aromatic dicarboxaldehyde and 4-aminophenol, then carrying out addition reaction with DOPO and obtaining a nitrogen and phosphorus fire retardant molecule. The obtained nitrogen and phosphorus fire retardant molecule has amino and phenolic active groups, and further can react with substances containing epoxy functional groups, so that the defects of low thermal decomposition temperature, poor compatibility with polymer matrix and easy mobility of the traditional small-molecular flame retardant are overcome. After the nitrogen and phosphorus fire retardant is added into an epoxy resin system, the formed cured matter has good flame retardant performance, and the limit oxygen index is greatly improved. The method is simple and easy, does not need to use a catalyst and gas protection, is easy to control, good in repeatability, simple in after-treatment process and high in yield and is suitable for enlarged production.

Description

technical field [0001] The invention belongs to the technical field of synthesis of nitrogen-phosphorus flame retardants, in particular to a nitrogen-phosphorus flame retardant and its preparation method and application. The nitrogen-phosphorus flame retardant is added to epoxy resin materials in various ways, and can Effectively improve the flame retardant, mechanical, electrical insulation and other properties of the material. Background technique [0002] In aerospace, electrical and electronics, machinery, optical instruments, light industry and other fields, polymer materials have been widely used due to their good processability and bonding performance. With the rapid development of industry, higher requirements are put forward for polymer materials. In addition to excellent comprehensive performance, good flame retardancy is also required. Most polymer materials are flammable, so they are Flame retardant modification is very necessary. [0003] At present, the most ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5313C07F9/6574C08L63/00
Inventor 姚有为肖玲孙德朝牛天力
Owner SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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