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

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Problems solved by technology

The inventions of the above patents are limited to aromatic phosphate compounds,

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 Embodiment

[0019] Example 1

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

[0021] A 250ml reactor equipped with a stirrer, thermometer, hydrogen chloride absorption device and condenser is charged with 22.0g (0.2mol) resorcinol, 184.0g (1.2mol) phosphorus oxychloride and 0.5g AlCl 3 , Heat these materials to 115°C within 0.5h, stir the reaction for 3h, use a PH meter to detect that no HCl is released, and the generated hydrogen chloride gas is absorbed by the hydrogen chloride absorption device. Distill under reduced pressure in a nitrogen atmosphere (130°C for 5h under a 50mmHg column) to remove unreacted phosphorus oxychloride to obtain 67.7g of phosphorus oxychloride (y 1 = 98.43%).

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

Example Embodiment

[0025] Example 2

[0026] In the first reaction, the amount of phosphorus oxychloride was changed to 153.3 g (1.0 mol), the reaction temperature was changed to 90°C, and the other reaction processes were the same as in Example 1. The yield of the obtained target product was 78.2%.

Example Embodiment

[0027] Example 3

[0028] In the second step of the reaction, the amount of propylene oxide was changed to 69.7 g (50 wt% excess, calculated as resorcinol), and the other reaction processes were 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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