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Phosphate ester polymer intumescent flame retardant and preparation method thereof

An intumescent flame retardant and phosphoric acid ester technology, which is applied in the design and preparation of phosphoric acid ester polymers, can solve the problems of uncontrollable conditions, uneasy storage, harsh conditions, etc. High carbon content

Inactive Publication Date: 2012-04-18
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the number of flame retardant components, it can generally be divided into single-component and multi-component intumescent flame retardants, but these are all small molecule flame retardants, which will be precipitated, Migration and other issues
Moreover, the traditional preparation process conditions are relatively harsh, and generally need to be carried out under inert gas protection and anhydrous conditions, and the conditions are not easy to control; in addition, commonly used phosphorus oxychloride, phosphorus pentoxide, etc. are used as synthetic raw materials, which have certain corrosiveness. There are disadvantages such as not easy to store

Method used

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  • Phosphate ester polymer intumescent flame retardant and preparation method thereof
  • Phosphate ester polymer intumescent flame retardant and preparation method thereof
  • Phosphate ester polymer intumescent flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Add 20mmol of bisphenolic acid, 50ml of methanol, and 1mmol of catalyst p-toluenesulfonic acid into a 250ml flask, heat and reflux for 8h under stirring, cool to room temperature after the reaction is over, and rotary evaporate excess methanol, then add deionized water to precipitate, Rapidly stirred and filtered to obtain the crude product with the general structure formula (IV), recrystallized with methanol / water (volume ratio 50:1) to obtain a white solid with a melting point of 132-133°C and a yield of 80% (see figure 1 , 1 H NMR see figure 2 ). The compound with the general structural formula (Ⅳ), namely methyl bisphenolate (5mmol, 1.005g), 1mol / L NaOH (10mmol, 0.4g) solution, phase transfer catalyst tetrabutylammonium bromide 0.25mmol and deionized water Add 25ml into the three-necked flask, mechanically stir at 25°C to dissolve all the above mixture, then quickly add 25ml of dichloromethane solution of phenyl phosphate dichloride, stir rapidly, and after reac...

Embodiment 2

[0049] Add 20mmol of bisphenolic acid, 50ml of ethanol, 1mmol of catalyst concentrated sulfuric acid into a 250ml flask, heat and reflux for 8h under stirring, cool to room temperature after the reaction is over, and spin evaporate excess ethanol, then add hot deionized water to precipitate, and stir rapidly The crude product of ethyl bisphenolate was obtained by filtration, and recrystallized with methanol / water to obtain a white solid with a melting point of 128-129°C and a yield of 78%. Add 5mmol of ethyl bisphenolate, 10mmol of sodium hydroxide, 0.25mmol of phase transfer catalyst tetrabutylammonium chloride and 25ml of deionized water into the three-necked flask, mechanically stir at 25°C to dissolve all the EDP, and then quickly Add 25ml of dichloromethane solution containing 5mmol of phenyl phosphate dichloride, stir rapidly, and after reacting for 1h, filter the product with suction, wash with a large amount of deionized water and ethanol, and dry in vacuum at 70°C to o...

Embodiment 3

[0052] Add 20mmol of bisphenolic acid, 50ml of ethanol, and 1mmol of catalyst p-toluenesulfonic acid into a 250ml flask, heat and reflux for 8h under stirring, cool to room temperature after the reaction is over, and spin out excess ethanol, then add hot deionized water Precipitate, stir and filter rapidly to obtain the crude product of ethyl bisphenolate, recrystallize with methanol / water to obtain a white solid, melting point 128~129°C, yield 78%. Add 5mmol of ethyl bisphenolate, 10mmol of sodium hydroxide, 0.25mmol of phase transfer catalyst tetrabutylammonium bromide and 25ml of deionized water into a three-necked flask, mechanically stir at 25°C to dissolve all the EDP, and then quickly Add 25ml of dichloromethane solution containing 5mmol of phenyl phosphate dichloride, stir rapidly, and after reacting for 1h, filter the product with suction, wash with a large amount of deionized water and ethanol, and dry in vacuum at 70°C to obtain the general structural formula (II) T...

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Abstract

The invention discloses phosphate ester polymer intumescent flame retardant and a preparation method thereof. Polyhydroxyl acid compound serves as raw materials, and carboxyl is protected by esterification; and in the presence of phase transfer catalyst, with an interfacial polymerization method that esterified polyhydroxyl compounds, such as diphenolic acid methyl ester and phenyl dichlorophosphate, serve as main raw materials, an obtained intermediate polymer comprises a polyhydroxyl acid methyl ester and phenyl dichlorophosphate reaction unit. The synthesis method has the advantages of simple technology and cheap and abundant raw materials, is easy to operate and is suitable for industrial production; and the reaction is easy. The intermediate polymer and amido compound carry out esteramine solution reaction under the action of the catalyst to obtain the intumescent flame retardant. The flame retardant does not contain halogens and belongs to the environmentally-friendly flame retardant. The structural general formula (III) of the phosphate ester polymer intumescent flame retardant is showed as follows.

Description

technical field [0001] The invention relates to a design and preparation method of a phosphoric acid ester polymer. Specifically, it relates to a halogen-free, green and environment-friendly phosphoric acid ester polymer intumescent flame retardant used in the field of flame retardants and a preparation method thereof. Background technique [0002] With the advancement of science and technology, the application fields of organic polymer materials are becoming more and more extensive. However, most polymer materials are flammable, and the fire hazards caused by them have become a social issue of global concern. [0003] Flame retardants currently used in industrial production can be roughly divided into two types: halogen-based and halogen-free. Because halogen-containing flame-retardant materials produce more smoke and toxic and corrosive gases when burned, causing serious "secondary disasters", some brominated flame retardants have been banned in the RoHS directive issued...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C08K7/22C08K5/523C07F9/6521C07F9/14
Inventor 张艳刘妍方征平
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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