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P-N intumescent flame retardant and preparation method thereof

An intumescent flame retardant, P-N technology, applied in the field of chemistry, can solve the problems of large amount of addition, smoke, environmental pollution, etc.

Inactive Publication Date: 2014-10-22
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 intumescent flame retardant and preparation method thereof
  • P-N intumescent flame retardant and preparation method thereof
  • P-N intumescent flame retardant and preparation method thereof

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Effect test

Embodiment 1

[0022] Embodiment 1: Preparation of P-N series intumescent flame retardant

[0023] (a) Add solvent glacial acetic acid, 0.10mol bisphenol A, 0.2mol phenylphosphonic dichloride, catalyst aluminum trichloride, and 200rpm magnetic stirring and heating up to 80°C, and continued stirring reaction at 200rpm for 4h. After the reaction was completed, the solution was light yellow and viscous, which was the intermediate product poly 2,2-bis(4-phenylphosphonochlorophenyl)propane ;

[0024] (b) Add 0.2 mol of p-aminobenzoic acid dissolved in glacial acetic acid to the above intermediate product, then raise the temperature to 90°C, stir and react at 200rpm for 4h, continue to raise the temperature to 130°C, keep stirring at 200rpm for 2h, and then end the reaction;

[0025] (c) cooling, hydrolyzing, suction filtering, alkali washing, suction filtering, water washing, and drying the reaction product obtained in step b to obtain a white powder, which is the P-N series intumescent flam...

Embodiment 2

[0036] Add solvent glacial acetic acid, 0.10mol bisphenol A, 0.19mol phenylphosphonic dichloride, catalyst aluminum trichloride, 200rpm magnetic stirring and Raise the temperature to 80°C, and continue stirring at 200 rpm for 4 hours. After the reaction is completed, the solution is light yellow and viscous, which is the intermediate product poly-2,2-bis(4-phenylphosphonochlorophenyl)propane;

[0037] Add 0.21mol p-aminobenzoic acid dissolved in glacial acetic acid to the intermediate product obtained in the above steps, then raise the temperature to 90°C, stir at 200rpm for 4h, continue to raise the temperature to 130°C, stir at 200rpm for 2h; After the product is cooled, hydrolyzed, filtered with suction, washed with alkali, filtered with suction, washed with water, and dried, a white powder is obtained, which is the P-N series intumescent flame retardant poly(2,2-bis(4-p-aminobenzoic acid) - phenylphosphine oxide phenyl)) propane.

Embodiment 3

[0039] Add solvent glacial acetic acid, 0.10mol bisphenol A, 0.21mol phenylphosphonic dichloride, catalyst aluminum trichloride, 200rpm magnetic stirring and Raise the temperature to 80°C, and continue to stir and react at 200rpm for 4 hours. After the reaction is completed, the solution is light yellow and viscous, which is poly-2,2-bis(4-phenylphosphonochlorophenyl)propane;

[0040] Add 0.19mol p-aminobenzoic acid dissolved in glacial acetic acid to the above intermediate product, then raise the temperature to 90°C, stir and react at 200rpm for 4h, continue to raise the temperature to 130°C, stir and react at 200rpm for 2h; after the reaction is completed, cool the reaction product , hydrolysis, suction filtration, alkali washing, suction filtration, water washing, and drying, a white powder is obtained, which is the P-N series intumescent flame retardant poly(2,2-bis(4-p-aminobenzoic acid-benzene Phosphine oxide phenyl)) propane.

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Abstract

The invention discloses a P-N intumescent flame retardant and a preparation method thereof. The P-N intumescent flame retardant is poly2, 2-bis(4-para-aminobenzoic acid-phenylphosphine oxide phenyl)propane. The preparation method includes: (a) adding a solvent glacial acetic acid, a catalyst aluminium trichloride, phenylphosphonic dichloride and bisphenol A into a flask in order to react for 4h; (b) dissolving para-aminobenzoic acid in glacial acetic acid to form a mixed solution, then adding the solution obtained in step a, firstly raising the temperature to 90DEG C and conducting high speed stirring reaction for 4h, then further raising the temperature to 130DEG C, and performing high speed stirring reaction for 2h; and (c) subjecting the reaction product obtained in step b to cooling, hydrolysis, alkali washing, water washing, suction filtration and drying so as to obtain white powder, i.e. the P-N intumescent flame retardant. The P-N intumescent flame retardant provided by the invention overcomes the disadvantages of generation of harmful gas, environment pollution, fuming, influence to mechanical properties and the like of common flame retardants, has double carboxyl terminal group, can key effective flame retardant components to a PA66 main chain to play an essential flame retardant role, and has the advantages of no harm, fume suppression, high efficiency and environmental protection, etc.

Description

technical field [0001] The invention belongs to the field of chemistry, in particular to a P-N series intumescent 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 flame retardants...

Claims

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Application Information

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IPC IPC(8): C08G79/02C08L85/02C08L77/06
Inventor 吕文晏崔益华
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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