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Preparation method of hexaphenoxycyclotriphosphazene

A technology of hexaphenoxycyclotriphosphazene and hexachlorocyclotriphosphazene, which is applied in the field of preparation of hexaphenoxycyclotriphosphazene, can solve the problems of low repeatability, improve product purity, and be easy to realize Effects of industrialization, reduction of raw material consumption and energy consumption

Inactive Publication Date: 2014-01-29
威海金威化学工业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the color of the prepared product is slightly different, and the repeatability is not very high

Method used

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  • Preparation method of hexaphenoxycyclotriphosphazene

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Experimental program
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Effect test

Embodiment 1

[0033] (1) Preparation of hexachlorocyclotriphosphazene

[0034] A. raw material preparation, prepare raw material according to ammonium chloride 51.2g, composite catalyst 2.56g, pyridine 12.8g, phosphorus pentachloride 256g and chlorobenzene 1024g, wherein catalyzer is the composite catalyst of zinc chloride, ferric chloride, magnesium chloride, its The molar ratio is 1:1:1. Heat in an oil bath, slowly raise the temperature to 120±5°C and reflux, keep the temperature under reflux for 6 to 10 hours, the solution turns from light yellow to light green after a period of reaction, then the reflux temperature rises to 130±5°C until the reaction is completed.

[0035] b. After the reaction, the tap water was cooled to room temperature, and the residue was filtered to obtain a chlorobenzene solution of hexachlorocyclotriphosphazene.

[0036] (2) Preparation of hexaphenoxycyclotriphosphazene

[0037] a. Raw material preparation, the mass ratio of hexachlorocyclotriphosphazene: phen...

Embodiment 2

[0044] (1) Preparation of hexachlorocyclotriphosphazene

[0045] A. raw material preparation, prepare raw material according to ammonium chloride 51.2g, composite catalyst 2.56g, pyridine 12.8g, phosphorus pentachloride 256g and chlorobenzene 1024g, wherein catalyzer is the composite catalyst of zinc chloride, ferric chloride, magnesium chloride, its The molar ratio is 1:1:1. Heat in an oil bath, slowly raise the temperature to 120±5°C and reflux, keep the temperature under reflux for 6 to 10 hours, the solution turns from light yellow to light green after a period of reaction, then the reflux temperature rises to 130±5°C until the reaction is completed.

[0046] b. After the reaction, the tap water was cooled to room temperature, and the residue was filtered to obtain a chlorobenzene solution of hexachlorocyclotriphosphazene.

[0047] (2) Preparation of hexaphenoxycyclotriphosphazene

[0048] a. Raw material preparation, the mass ratio of hexachlorocyclotriphosphazene: phen...

Embodiment 3

[0055] (1) Preparation of hexachlorocyclotriphosphazene

[0056] A. raw material preparation, prepare raw material according to ammonium chloride 51.2g, composite catalyst 2.56g, pyridine 12.8g, phosphorus pentachloride 256g and chlorobenzene 1024g, wherein catalyzer is the composite catalyst of zinc chloride, ferric chloride, magnesium chloride, its The molar ratio is 1:1:1. Heat in an oil bath, slowly raise the temperature to 120±5°C and reflux, keep the temperature under reflux for 6 to 10 hours, the solution turns from light yellow to light green after a period of reaction, then the reflux temperature rises to 130±5°C until the reaction is completed.

[0057] b. After the reaction, the tap water was cooled to room temperature, and the residue was filtered to obtain a chlorobenzene solution of hexachlorocyclotriphosphazene.

[0058] (2) Preparation of hexaphenoxycyclotriphosphazene

[0059] a. Raw material preparation, the mass ratio of hexachlorocyclotriphosphazene: phen...

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Abstract

The invention discloses a preparation method of hexaphenoxycyclotriphosphazene. The method comprises the following steps of: with phosphorus pentachloride and ammonium chloride as starting raw materials and chlorobenzene as a solvent, carrying out a high-selectivity synthetic reaction, and filtering to obtain high-purity chlorobenzene solution of hexachlorocyclotriphosphazene, and then reacting the high-purity chlorobenzene solution of hexachlorocyclotriphosphazene with potassium phenate to obtain high-purity hexaphenoxycyclotriphosphazene. The preparation method is simple in process and good in reproducibility; and as a result, the problems of low conversion rate and difficult industrialization in the synthesis of hexaphenoxycyclotriphosphazene can be effectively solved.

Description

technical field [0001] The invention belongs to the technical field of synthesis of nitrogen- and phosphorus-containing organic compounds, and in particular relates to a preparation method of hexaphenoxycyclotriphosphazene. Background technique [0002] Hexaphenoxycyclotriphosphazene is a phosphazene derivative obtained by replacing the active chlorine atom of the phosphazene side group with a phenoxy group using hexachlorocyclotriphosphazene as an intermediate, and can be directly added to the polymer matrix Prepared flame retardant materials. If it is added to polycarbonate to prepare a flame-retardant polycarbonate material, the LOI value of the material can reach 30, and it can also be added to PC / ABS resin to prepare a flame-retardant PC / ABS alloy material, and the LOI value of the material can reach 26~30. Compared with other flame retardants, hexaphenoxycyclotriphosphazene has the advantages of high oxygen index, low smoke emission, non-corrosion and low toxicity of...

Claims

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Application Information

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IPC IPC(8): C07F9/6593
Inventor 成国亮
Owner 威海金威化学工业有限责任公司
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