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Cyclic polyphosphoester oligmer, and preparation method and application thereof

A polyphosphate and oligomer technology, applied in the field of flame retardants, can solve the problems of unfavorable mechanical properties of polymer materials, low decomposition temperature of flame retardants, influence on flame retardant effect, etc., and achieve high yield and thermal stability. Good, improve the effect of mechanical properties

Inactive Publication Date: 2015-05-20
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, after the above-mentioned polymeric polymeric phosphonate flame retardant is added to the polymer material, it will have an adverse effect on the mechanical properties of the polymer material.
Moreover, the decomposition temperature of the above-mentioned linear polymer flame retardants is low, and they decompose to varying degrees during processing, thus affecting the flame retardant effect

Method used

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  • Cyclic polyphosphoester oligmer, and preparation method and application thereof
  • Cyclic polyphosphoester oligmer, and preparation method and application thereof
  • Cyclic polyphosphoester oligmer, and preparation method and application thereof

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preparation example Construction

[0030] The invention also provides a method for preparing the cyclic polyphosphate oligomer, which comprises the following steps:

[0031] The compound having the structure of formula (II) is mixed with the compound having the structure of formula (III), and the polymerization reaction is carried out in the presence of a catalyst or acid scavenger to obtain a cyclic polyphosphate oligomer having a structure of formula (I) ,

[0032]

[0033] The R 1 Is phenyl, substituted phenyl or C1-C10 alkyl, said R 2 It is a C1-C10 alkylene group or a bisphenol compound after losing two hydroxyl groups, n is the degree of polymerization, and n=2-7.

[0034] In the present invention, the compound having the structure of formula (II) is The R 1 It is a phenyl group, a substituted phenyl group, or a C1-C10 alkyl group, preferably a methyl group, a phenyl group, or a phenoxy group, and more preferably a phenyl group. That is, the compound having the structure of formula (II) is preferably phenylpho...

Embodiment 1

[0056] Weigh 7mmol of phenylphosphonic dichloride and dissolve in 50ml of dichloromethane to obtain a dichloromethane solution of phenylphosphonic dichloride. Weigh 7mmol of bisphenol A monomer and dissolve in 50ml of 0.28mol / L sodium hydroxide aqueous solution In the process, an aqueous sodium hydroxide solution of bisphenol A monomer is obtained.

[0057] Add the above two solutions slowly and uniformly within 10 hours to a 500ml four-neck flask filled with 200ml dichloromethane, 40ml deionized water and 0.2g cetyltrimethylammonium bromide under vigorous stirring In, and access to N 2 Protected, the reaction temperature is controlled at -20°C-20°C, and the reaction is continued for 3 hours after the addition is completed. After the reaction, the organic phase was separated with a separatory funnel, washed 2-3 times with deionized water to remove inorganic salts, and the solvent was evaporated to obtain a white solid product, namely 2.1 g of cyclic polyphosphate oligomer, with a...

Embodiment 2

[0065] Weigh 7mmol of phenylphosphonic dichloride and dissolve it in 50ml of dichloromethane to obtain a dichloromethane solution of phenylphosphonic dichloride. Weigh 7mmol of phenolphthalein monomer and dissolve it in 50ml of 0.28mol / L sodium hydroxide aqueous solution. A sodium hydroxide aqueous solution of phenolphthalein monomer was obtained.

[0066] Add the above two solutions slowly and uniformly within 10 hours to a 500ml four-neck flask filled with 200ml dichloromethane, 40ml deionized water and 0.2g cetyltrimethylammonium bromide under vigorous stirring In, and access to N 2 Protected, the reaction temperature is controlled at -20°C-20°C, and the reaction is continued for 3 hours after the addition is completed. After the reaction, the organic phase was separated with a separatory funnel, washed 2-3 times with deionized water to remove inorganic salts, and the solvent was evaporated to dryness to obtain a white solid product, namely 2.22 g of cyclic polyphosphate oligo...

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Abstract

The invention provides a cyclic polyphosphoester oligmer; the thermal stability of the cyclic polyphosphoester oligmer is good; the cyclic polyphosphoester oligmer can meet polymer material processing requirements; furthermore, after being added into a polymer material substrate, the cyclic polyphosphoester oligmer provided by the invention is capable of increasing the mechanical property of the polymer material substrate; and in addition, a series of cyclic polyphosphoester oligmers synthesized through condensation polymerization by adopting a pseudo-high dilution technology can be simple in preparation method and high in yield.

Description

Technical field [0001] The invention belongs to the technical field of flame retardants, and specifically relates to a cyclic polyphosphate oligomer, a preparation method and application thereof. Background technique [0002] In today's society, fires are frequent, and people have higher and higher requirements for flame retardant materials. As we all know, the commonly used flame retardants are halogen flame retardants and inorganic metals. Although halogen-based flame retardants have good flame retardant effects, they will produce a large amount of toxic and harmful gases during the combustion process, so they cannot meet people's requirements for environmental protection. When inorganic metal flame retardants are applied, the addition amount is relatively large, generally 40% to 60%, which can easily lead to a significant reduction in the physical and mechanical properties of the material. [0003] Due to the presence of PC bonds in polymeric polymer phosphonates, it has enhan...

Claims

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Application Information

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IPC IPC(8): C08K5/5357C07F9/6574C08G79/04C08L85/02C08L67/02
Inventor 周光远李娜娜姜国伟
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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