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High-efficiency N/P flame retardant, as well as preparation method and application thereof

A technology of nitrogen-phosphorus flame retardants and flame retardants, applied in the field of high-efficiency nitrogen-phosphorus flame retardants and their preparation, to achieve the effect of simplifying process steps and improving flame retardant performance

Inactive Publication Date: 2013-04-17
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In this application, 4,4'-diaminodiphenylmethane (DDM for short) is used for condensation reaction with aromatic aldehyde, and then DOPO is added to the reacted mixture for reaction to prepare nitrogen-phosphorus flame retardant and the obtained nitrogen-phosphorus flame retardant agent, no relevant literature disclosure

Method used

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  • High-efficiency N/P flame retardant, as well as preparation method and application thereof
  • High-efficiency N/P flame retardant, as well as preparation method and application thereof
  • High-efficiency N/P flame retardant, as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] flame retardant ( 1 ) The synthetic steps are as follows:

[0023] Add 9.91g of DDM, 10.61g of benzaldehyde and about 82.08g of absolute ethanol into a three-necked flask with a stirring device. Under stirring, the reaction temperature is 0 o C is reacted for 2-4h, and the mixture A is obtained after the reaction is completed;

[0024] Then, 21.62 g DOPO was added to the mixture A in the three-necked flask, and under stirring, the temperature of reaction was 0 o C was reacted for 18 h. After the reaction was finished, the final mixture was suction-filtered, washed, and dried in a vacuum oven for 60 o C drying for 8 h to obtain the required flame retardant ( 1 ), the yield is 89.2%.

[0025] flame retardant ( 1 ) test analysis results are as follows:

[0026] 1 H HMR (ppm, DMSO-d 6 ), δ=3.45(H 1’ ), 4.08(H 1 ), 5.01-5.10 (H 6 ), 5.48-5.58 (H 6’ ), 6.10 (NH’), 6.50-6.60 (H 4 , H 4’ , NH), 6.60-6.68 (H 3 , H 3’ ), 7.05 (H 21 ), 7.20 (H 21’ ), 7,25-7.35 (H...

Embodiment 2

[0030] flame retardant ( 2 ) The synthetic steps are as follows:

[0031] Add 9.91g of DDM, 12.21g of 2-hydroxybenzaldehyde and about 884.8 g of ethyl acetate into a three-necked flask with a stirring device. Under stirring, the reaction temperature is 20 o C was reacted for 2-4 h to obtain mixture A;

[0032] Then, 21.62 g DOPO was added to the mixture A in the three-necked flask, and under stirring, the temperature of reaction was 50 o C was reacted for 18h. After the reaction was finished, the final mixture was suction-filtered, washed, and dried in a vacuum oven for 60 oC Dry for 8 h to get the required flame retardant ( 2 ), the yield was 90.7%.

[0033] flame retardant ( 2 ) test analysis results are as follows:

[0034] 1 H HMR (ppm, DMSO-d 6), δ=3.45(H 1’ ), 4.08(H 1 ), 5.23 (H 6 ), 5.38(H 6’ ), 6.12 (NH’), 6.40-6.60 (H 4 , H 4’ , H 11 , H 11’ , H 9 , H 9’ , NH), 6.70-6.80 (H 3 , H 3’ , H 8 , H 8’ ), 6.95 (H 23 , H 10 ), 7.09 (H 10’ ), 7.13(H ...

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Abstract

The invention provides a high-efficiency N / P flame retardant, as well as a preparation method and application thereof. The method comprises the following steps: firstly performing condensation reaction of 4,4'-diaminodiphenylmethane (DDM) with aromatic aldehydes, and then adding DOPO into the resulting mixture for reaction, to obtain the N / P flame retardant. The flame retardant has higher activity, can promote curing of epoxy resins, and is added to epoxy resin for curing to form a cured epoxy product which has higher flame retardancy. When the phosphorus content of the cured epoxy system reaches 1.0 wt% to 1.5 wt%, the vertical combustion level reaches the grade UL94V-0, the limited oxygen index reaches 37.8-41.2, and the char yield reaches 22.1%-24.9% at 800 DEG C.

Description

technical field [0001] The invention relates to the preparation technology of nitrogen-phosphorus flame retardant for epoxy resin, especially a high-efficiency nitrogen-phosphorus flame retardant and its preparation method and application. The nitrogen-phosphorus flame retardant is added to epoxy resin materials in various ways , effectively improve the flame retardant properties of epoxy resin materials. Background technique [0002] At present, epoxy resin materials are widely used in electronic packaging materials, surface coatings, adhesives and other fields due to their excellent insulation, thermal stability, and chemical resistance. The more widespread and the rapid increase in the amount of use, the higher the performance requirements of the material. Therefore, improving the flame retardant properties of epoxy resins has become a hot spot in the current research on the properties of polymer materials. Traditionally, the method of flame retardant modification of ep...

Claims

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Application Information

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IPC IPC(8): C08K5/5313C07F9/6574C08L63/00
Inventor 姚有为牛天力孙德朝
Owner SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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