Efficient nitrogen and phosphorus fire retardant for epoxy resin and preparation method of efficient nitrogen and phosphorus fire retardant

A technology for nitrogen-phosphorus flame retardants and epoxy resins, applied in the field of high-efficiency nitrogen-phosphorus flame retardants, to achieve the effects of simplified process steps, high char formation rate and glass transition temperature, and improved flame retardant and mechanical properties

Inactive Publication Date: 2013-04-03
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First, 4,4'-diaminodiphenyl ether (DDE) and aromatic aldehydes are used for condensation reaction, and then DOPO is added to the reacted mixture for reaction to prepare nitrogen-phosphorus flame retardants. There is no relevant literature disclosure.

Method used

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  • Efficient nitrogen and phosphorus fire retardant for epoxy resin and preparation method of efficient nitrogen and phosphorus fire retardant
  • Efficient nitrogen and phosphorus fire retardant for epoxy resin and preparation method of efficient nitrogen and phosphorus fire retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] flame retardant ( 1 ) The synthetic steps are as follows:

[0025] Add 10.01 g of DDE, 10.61 g of benzaldehyde and 412 g of absolute ethanol into a three-necked flask with a stirring device, and under stirring, the reaction temperature is 0°C for 2-4 h until the end of the reaction;

[0026] Then, 21.62g DOPO was added to the reaction mixture in the three-necked flask, and under stirring, the reaction temperature was 0°C for 18 hours. After the reaction, the final mixture was suction-filtered, washed, and dried in a vacuum oven at 60°C. Dry 8h, obtain required flame retardant ( 1 ).

[0027] flame retardant ( 1 ) test analysis results are as follows:

[0028] 1 H HMR (ppm, DMSO-d 6 ), δ=4.96-5.10 (H), 5.45-5.57 (H), 6.10 (NH), 6.40-6.51 (2H), 6.55 (NH), 6.57-6.68 (2H), 7.05 (H), 7.20 (H ), 7.25-7.35 (6H), 7.35-7.43 (2H), 7.43-7.50 (3H), 7.55 (H), 7.70-7.80 (2H), 7.95-8.05 (2H), 8.15-8.25 (4H).

[0029] 13 C NMR (ppm, DMSO-d 6 ), Δ = 55.3, 56.5, 56.9, 57.7, 115...

Embodiment 2

[0034] flame retardant ( 2 ) The synthetic steps are as follows:

[0035] Add 10.01 g of DDE, 12.21 g of 4-hydroxybenzaldehyde and 200 g of absolute ethanol into a three-necked flask with a stirring device. Under stirring, the reaction temperature is 30 ° C for 2-4 h until the end of the reaction;

[0036] Then, 21.62g DOPO was added to the reaction mixture in the three-necked flask, and under stirring, the reaction temperature was 30°C for 18 hours. After the reaction, the final mixture was suction filtered, washed, and dried in a vacuum oven for 60 ℃ drying for 8 h to obtain the required flame retardant ( 2 ).

[0037] flame retardant ( 2 ) test analysis results are as follows:

[0038] 1 H HMR (ppm, DMSO-d 6 ), δ=4.80-4.91 (H), 5.20-5.33 (H), 5.98 (NH), 6.40 (NH), 6.45-6.70 (8H), 7.05 (H20), 7.15-7.23 (3H), 7.40-7.50 (H), 7.55 (H), 7.70-7.80 (2H), 7.95-8.05 (2H), 8.15-8.25 (4H), 9.36 (H), 9.40 (H).

[0039] 13 C NMR (ppm, DMSO-d6), δ=55.1, 55.8, 56.5, 57.0, 115.0, 11...

Embodiment 3

[0044] flame retardant ( 3 ) The synthetic steps are as follows:

[0045] Add 10.01g of DDE, 12.21g of 2-hydroxybenzaldehyde and 89g of ethyl acetate into a three-necked flask with a stirring device, and under stirring, the reaction temperature is 60°C for 2-4 hours;

[0046] Then, 21.62g DOPO was added to the reaction mixture in the three-necked flask, and under stirring, the reaction temperature was 60°C for 18 hours. After the reaction, the final mixture was suction-filtered, washed, and dried in a vacuum oven for 60 ℃ drying for 8 h to obtain the required flame retardant ( 3 ),

[0047] flame retardant ( 3 ) test analysis results are as follows:

[0048] 1 H HMR (ppm, DMSO-d 6 ), δ=5.20 (H), 5.35(H), 6.12 (NH), 6.40-6.60 (7H), 6.70-6.80 (4H), 7.02 (2H), 7.09 (H), 7.13(H), 7, 25-7.45 (4H), 7.50 (H), 7.58 (H), 7.65-7.80 (2H), 8.00-8.10 (2H), 8.15-8.25 (4H), 9.40 (H), 9.54 (H).

[0049] 13 C NMR (ppm, DMSO-d 6 ), Δ = 48.4, 49.5, 49.7, 50.7, 115.0, 119.5, 120.5, 121....

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Abstract

The invention relates to an efficient nitrogen and phosphorus fire retardant for epoxy resin, and a preparation method of the efficient nitrogen and phosphorus fire retardant. The method comprises the steps of allowing 4,4'-diaminodiphenyl ether (DDE) and aromatic aldehyde to conduct condensation reaction, and adding DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) to a reacted mixture for reaction to prepare the nitrogen and phosphorus fire retardant. According to the method, an intermediate product is not required to be separated; the method has simplified processing steps, is efficient, safe and environment-friendly and facilitates industrial batch production. Molecules of the obtained fire retardant are higher in activity; the fire retardant can facilitate epoxy resin curing; after the fire retardant is added into the epoxy resin, a cured epoxy condensate has better flame resistance; when the phosphorus content of an epoxy curing system reaches 0.75-1.0wt%, the vertical burning grade reaches UL94V-0; the limit oxygen index is greater than 38; and the char yield reaches 21.2-22.7% at 800 DEG C.

Description

technical field [0001] The invention relates to a high-efficiency nitrogen-phosphorus flame retardant, its preparation process and application. The nitrogen-phosphorus flame retardant is added to epoxy resin materials in various ways to promote the curing of epoxy resin and effectively improve the flame retardancy of epoxy resin materials. properties, mechanical properties. 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 epoxy resin materials is to introd...

Claims

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Application Information

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