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Polycondenseng phosphate and its preparation process and application thereof

A phosphate ester and polycondensation technology, applied in the direction of phosphorus organic compounds, etc., to reduce the amount of flame retardants and improve the flame retardant effect

Inactive Publication Date: 2008-01-16
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventions of the above patents are limited to aromatic phosphate compounds, and the required substances contain only one flame retardant element-phosphorus

Method used

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  • Polycondenseng phosphate and its preparation process and application thereof
  • Polycondenseng phosphate and its preparation process and application thereof
  • Polycondenseng phosphate and its preparation process and application thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0020] Preparation of resorcinol tetrakis(1-chloro-2-isopropyl) diphosphate

[0021] 22.0g (0.2mol) of resorcinol, 184.0g (1.2mol) of phosphorus oxychloride and 0.5g of AlCl were charged in a 250ml reactor equipped with a stirrer, a thermometer, a hydrogen chloride absorption device and a condenser 3 , these materials were heated to 115°C within 0.5h, stirred and reacted for 3h, no HCl was released as detected by a pH meter, and the hydrogen chloride gas produced was absorbed by a hydrogen chloride absorption device. Distill under reduced pressure in nitrogen atmosphere (130 ℃ 5h under 50mmHg column), remove unreacted phosphorus oxychloride, obtain 67.7g phosphorus oxychloride (y 1 = 98.43%).

[0022] The intermediate produced by the above reaction was heated to 65°C, and 54.8g (20wt% excess, measured by the amount of intermediate phosphorus oxychloride) propylene oxide was added dropwise within 1h, and after continuing the reaction for 3.5h, the unreacted ring was distilled ...

example 2

[0026] In the first step reaction, the phosphorus oxychloride consumption is changed into 153.3g (1.0mol), and the temperature of reaction is changed into 90 DEG C, and other reaction processes are with example 1. The yield of the target product obtained was 78.2%.

example 3

[0028] In the second step reaction, the propylene oxide consumption is changed to 69.7g (50wt% in excess, in resorcinol), and other reaction processes are the same as in Example 1. The yield of the obtained target product was 89.9%.

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Abstract

The invention relates to a polycondensation type phosphate ester. R1, R2, R3 and R4 each contains alkyl of 2-4 carbon atom, and R5 is bivalent aromatic radical. The invention supplies a stable method to make phosphate ester that could be used as fire retardant or used combining fire retardant.

Description

technical field [0001] The invention relates to a polycondensed phosphoric acid ester, in particular to a polycondensed phosphoric acid ester containing a halogen substituent and a preparation method and application thereof. Background technique [0002] Flame retardants are used to prevent the combustion of flammable substances. Commonly used flame retardants include halogenated compounds such as decabromodiphenyl ether, tetrabromobisphenol A and low molecular weight phosphorus compounds such as toluene phosphate, biphenyl ester and triphenyl phosphate etc. The former will produce highly toxic dioxin compounds when burned, and the latter will decompose, ooze or volatilize when heated, so they are gradually replaced by condensed phosphate flame retardants with large molecular chains, high phosphorus content, and symmetrical structures. . [0003] Patents US 2520090 (1950.8.22), GB 734767 (1955.8.10), US 3944633 (1976.3.16) and US5183905 (1993.2.2) all relate to polycondensa...

Claims

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Application Information

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IPC IPC(8): C07F9/09C09K21/12
Inventor 李效军王静李秀云陈炜冯成
Owner HEBEI UNIV OF TECH
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