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P-N expanded reaction type flame retardant and preparation method thereof

An expansion reaction, P-N technology, applied in the field of chemistry, can solve the problems of smoke, large amount of addition, affecting mechanical properties, etc.

Inactive Publication Date: 2014-10-01
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the application method of flame retardants, they can be divided into additive flame retardants and reactive flame retardants. According to the composition, additive flame retardants mainly include inorganic flame retardants, halogenated flame retardants (organic chlorides and organic Bromide), phosphorus-based flame retardants (red phosphorus, phosphoric acid ester and halogenated phosphate ester, etc.) Such as: halogenated flame retardants produce harmful gases in high temperature environment, pollute the environment, generate smoke, add a large amount, affect mechanical properties, etc.

Method used

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  • P-N expanded reaction type flame retardant and preparation method thereof
  • P-N expanded reaction type flame retardant and preparation method thereof
  • P-N expanded reaction type flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1 Preparation of P-N series intumescent reactive flame retardant

[0026] (a) Add 0.13mol of acrylic acid to a 250ml three-neck flask equipped with a constant pressure low liquid funnel, stirrer and reflux device, stir magnetically at a rate of 200rpm and raise the temperature to 90°C. At this time, add 0.1mol of benzene Phosphorous dichloride, the dropping rate is controlled at 1.0ml / min, and the dropping time is 2h; after the dropping is completed, the temperature is raised to 110°C and refluxed, and the reaction is continuously stirred at 200rpm for 4h. After the reaction is completed, the solution becomes a colorless transparent liquid. It is 2-carboxyethylphenylphosphorous acid;

[0027] (b) Cool the 2-carboxyethylphenylphosphorous acid obtained in step a to 1°C in a low-temperature reaction constant temperature bath, add 0.26mol triethylamine acid-binding agent, raise the temperature to 5°C, and take 0.2mol p-aminobenzene Dissolve formic acid in glacial a...

Embodiment 2

[0041] Add 0.13 mol of acrylic acid to a 250 ml three-necked flask equipped with a constant-pressure low-liquid funnel, a stirrer and a reflux device, stir magnetically at a rate of 200 rpm and heat up to 90 ° C. The dropping rate was controlled at 1.0ml / min, and the dropping time was 2h; after the dropping was completed, the temperature was raised to 110°C for reflux, and the stirring reaction was continued at a rate of 200rpm for 4h. - Carboxyethylphenylphosphorous acid;

[0042] Place the above product in a low-temperature reaction constant temperature bath and cool it to about 1°C, add 0.26mol triethylamine acid-binding agent, heat up to 5°C, dissolve 0.19mol p-aminobenzoic acid in glacial acetic acid, add it to 2-carboxyethyl In the mixed solution of phenylphosphinic acid and triethylamine, stir the reaction at a rate of 200rpm for 2h, then raise the temperature to 80°C, and continue to stir the reaction at a rate of 200rpm for 4h; After suction filtration and drying, a ...

Embodiment 3

[0044] Add 0.13 mol of acrylic acid to a 250 ml three-necked flask equipped with a constant-pressure low-liquid funnel, a stirrer and a reflux device, stir magnetically at a rate of 200 rpm and heat up to 90 ° C. The dropping rate was controlled at 1.0ml / min, and the dropping time was 2h; after the dropping was completed, the temperature was raised to 110°C for reflux, and the stirring reaction was continued at a rate of 200rpm for 4h. - Carboxyethylphenylphosphorous acid.

[0045] Put the above product in a low-temperature reaction constant temperature bath and cool it to about 1°C, add 0.26mol triethylamine acid-binding agent, heat up to 5°C, dissolve 0.21mol p-aminobenzoic acid in glacial acetic acid, add it to 2-carboxyethyl In the mixed solution of phenylphosphinic acid and triethylamine, stir the reaction at a rate of 200rpm for 2h, then raise the temperature to 80°C, and continue to stir the reaction at a rate of 200rpm for 4h; After suction filtration and drying, a wh...

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Abstract

The invention discloses a P-N expanded reaction type flame retardant p-(carboxyphenyl-amino)-(carboxyphenyl-amidoethyl) phenylphosphine oxide and a preparation method thereof. The preparation method comprises the following steps: (a) adding a p-aminobenzoic acid solution into glacial acetic acid; (b) adding triethylamine and mixed solution obtained in the step (a) into a 2-carboxethylphenyl hypophosphorous acid solution, stirring at a high speed and reacting for 2 hours, raising the temperature to 80 DEG C, reacting for 4 hours, cooling, hydrolyzing, performing suction filtration, washing and drying to obtain white powder, namely the P-N expanded reaction type flame retardant. The defects that harmful gases are generated by general flame retardants, the environment is polluted, fuming is caused and the mechanical property is influenced are overcome, the P-N expanded reaction type flame retardant has double-carboxyl end groups, effective flame retardant components are bonded to a PA66 main chain, an inherently flame retardant effect is achieved, and the flame retardant has the advantages of harmlessness, smoke inhibition, high efficiency, environmental friendliness and the like.

Description

technical field [0001] The invention belongs to the field of chemistry, in particular to a P-N series expansion reaction flame retardant and a preparation method thereof. Background technique [0002] With the advancement of science and technology, polymer materials such as synthetic fibers, rubber, and plastics are increasingly used in various fields, especially engineering plastics play a more important role in the national economy and people's lives. However, engineering plastics belong to Flammable or combustible polymer materials are prone to fire and other accidents. In order to solve the problems of engineering plastics such as heat resistance and smoke suppression, the most effective method is to introduce flame retardants to convert flammable or combustible polymer materials into flame-retardant or Non-combustible materials, reduce the burning rate, delay the spread of flames, and control the occurrence of fires. According to the application method of flam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42C07F9/36
Inventor 崔益华吕文晏
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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