Preparation method of hexaphenoxy cyclotriphosphazene fire retardant

A technology of hexaphenoxycyclotriphosphazene and hexachlorocyclotriphosphazene, which is applied in the field of synthesis of phosphorus nitrogen compounds, can solve the problems of troublesome separation and purification, slow reaction speed, complicated operation, etc., and achieve simplified separation and purification methods and steps , avoid cost waste, simple preparation process

Active Publication Date: 2014-02-19
JINAN TAIXING FINE CHEM
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  • Abstract
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AI Technical Summary

Problems solved by technology

This phase-transfer catalytic method has slow reaction speed, long reaction time, poor product quality, high impurity content of low substitutes, and only 70% to 80% yield, high cost, and is not conducive to industrial transformation.
[0007] The fourth method is to use a quaternary ammonium salt as a catalyst without using an acid-binding agent, then wash the organic layer in sequence, and concentrate the solvent to obtain the product. This method has a long reaction time, and the post-treatment is relatively cumbersome, and it is difficult to obtain a solid product.
[0008] In summary, the existing synthetic methods of hexaphenoxycyclotriphosphazene have their own characteristics, but there are more or less long reaction times, complex operations, troublesome separation and purification, low product yield or quality, high cost and Problems such as heavy pollution are difficult to accept for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 500ml flask, add 17.2g sodium hydroxide, 35.5g phenol, 1g potassium iodide, add to 200g acetone, react for 2 hours, then add 18g hexachlorocyclotriphosphazene into the system, reflux when the system heats up, and react at 90°C for 10 Hours, cooling and filtering, the filtrate crystallized at -18 ° C, the resulting solid was washed with 100 ° C 5% sodium hydroxide aqueous solution for 3 hours, then filtered at room temperature to obtain 34.4 g of the product white powdery solid, the yield was 95.3%, and the purity was 97.2% .

Embodiment 2

[0027] In a 500ml flask, add 17.2g sodium hydroxide, 35.5g phenol, 0.5g potassium chloride, add in 200g acetonitrile, react for 1 hour, then add 18g hexachlorocyclotriphosphazene in the system, reflux when the system heats up, 80 ℃ for 6 hours, cooling and filtering, the filtrate crystallized at -18 ℃, the obtained solid was washed with 100 ℃ 4% sodium hydroxide aqueous solution for 3 hours, and then filtered at room temperature to obtain 34.9 g of the product white powdery solid, with a yield of 96.7%. Purity 97.0%.

Embodiment 3

[0029] In a 500ml flask, add 17.2g sodium hydroxide, 35.5g phenol, 0.8g potassium iodide, add 200g DMF, react for 2 hours, then add 18g hexachlorocyclotriphosphazene into the system, reflux when the system heats up, and react at 83°C After 3 hours, the temperature was lowered and filtered, and the filtrate was crystallized at -18 ° C. The obtained solid was washed with 100 ° C 3% sodium hydroxide aqueous solution for 5 hours, and then filtered at room temperature to obtain 34.6 g of the product white powdery solid, with a yield of 96.1% and a purity of 98.1 %.

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Abstract

The invention discloses a preparation method of a hexaphenoxy cyclotriphosphazene fire retardant. The method comprises the following steps: taking a polar aprotic solvent as a solvent; taking halogenated potassium as a catalyst; reacting alkali metal hydroxide with phenol for 1-2 h; adding hexachlorocyclotriphosphazene in the reactant; raising the temperature to 70-96 DEG C and keeping the temperature for reaction for 2-10 h; after the reaction, filtering the reactant at room temperature, and crystallizing at low temperature; using alkaline water to wash the crystals; filtering to obtain the hexaphenoxy cyclotriphosphazene fire retardant. By virtue of the method, the yield is more than or equal to 95%; the purity is more than or equal to 97%.

Description

technical field [0001] The invention relates to a preparation method of a high-purity, high-yield hexaphenoxycyclotriphosphazene flame retardant, and belongs to the technical field of phosphorus nitrogen compound synthesis. Background technique [0002] As an environmentally friendly flame retardant product, phosphazene flame retardants have developed rapidly in recent years, among which hexaphenoxycyclotriphosphazene is currently available in commercial applications. At present, domestic and foreign companies have applied for a large number of patents on the preparation and application of phosphazene series flame retardants. As a typical representative of cyclic phosphazene compounds, hexaphenoxycyclotriphosphazene has outstanding characteristics such as high heat resistance, excellent hydrolysis resistance, good compatibility with polymer materials, and remarkable flame retardant efficiency. One of the hotspots of combustion research. [0003] There are many research rep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593
Inventor 毕燕张晓华张雅民李加智
Owner JINAN TAIXING FINE CHEM
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