Preparation method of high purity hexaphenoxycyclotriphosphazene

A technology of hexaphenoxycyclotriphosphazene and hexachlorocyclotriphosphazene, which is applied in the field of synthesis of nitrogen-containing phosphorus organic compounds, can solve the problems of inconvenient industrial production, high volatility, and low boiling point, and reduce the pressure of purification , Increased reactivity, high yield effect

Active Publication Date: 2012-08-15
SHANDONG ZESHI NEW MATERIALS TECH CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

This method has adopted the TFH solvent that price is higher, boiling point is lower, volatility is bigger, brings some inconvenience to industrialized production

Method used

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  • Preparation method of high purity hexaphenoxycyclotriphosphazene

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Add 46 grams of ammonium chloride, 1.2 grams of magnesium chloride, and 250 grams of chlorobenzene into a three-necked flask equipped with a stirrer, condenser, and water separator tail gas absorption system, replace with nitrogen, and heat up to azeotropic dehydration at a temperature of 120-135°C. Finish, add dropwise at 125~135 ℃ the chlorobenzene solution that contains 150 grams of phosphorus pentachloride concentration and be 30%, the dropwise reaction time is 32 hours, after detecting that residual phosphorus pentachloride is qualified, reaction finishes, cools down, and filter out The reacted ammonium chloride is used in the next batch of reactions. The filtrate is washed twice with water at a washing temperature of 80°C. It is concentrated and steamed to remove most of the chlorobenzene, cooled and crystallized, filtered to obtain hexachlorocyclotriphosphazene, and recycled after filtering the mother liquor. The yield 80%, with a purity of over 99%; or the synthe...

Embodiment 2

[0040] Example 2: In Example 1, hexachlorocyclotriphosphazene was synthesized, adding 15 grams of catalyst pyridine, adding phosphorus pentachloride chlorobenzene solution dropwise, and reflux reaction for 16 hours, with a yield of 84% and a purity of 99%. In the synthesis of hexaphenoxycyclotriphosphazene, add 20 grams of PEG1000 catalyst, do not use alkali washing, acid washing, directly wash with methanol, the reaction is completed, the yield is 95%, the purity is 99%, and the chlorine content is less than 500ppm.

Embodiment 3

[0041] Embodiment 3: adopt the method of embodiment 1, hexachlorocyclotriphosphazene synthetic reaction finishes, reaction mixture is filtered, and mother liquor is washed with water, concentrates to obtain the chlorobenzene solution containing 25~30% of hexachlorocyclotriphosphazene. In the synthesis of hexaphenoxycyclotriphosphazene, a chlorobenzene solution containing 25% to 30% of hexachlorocyclotriphosphazene is used to react with sodium phenate, and the reaction ends with a yield of 80% and a purity of 95%.

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Abstract

The invention relates to a preparation method of hexaphenoxycyclotriphosphazene, in particular to a preparation method of high purity hexaphenoxycyclotriphosphazene, belonging to the technical field of the synthesis of organic compounds with nitrogen and phosphorus and the method contains the reaction process of hexachlorocyclotriphosphazene and sodium phenate substantially. The invention is characterized in that the reaction conditions are as follows: the catalyst is PEG-500-1000, the reaction temperature is 60-140 DEG C, the reaction time is 10-42h, the chlorinity of the target material is less than 500ppm at end point and the reaction solvent is chlorobenzene; concentrative crystallization method is used for purifying, the purity of hexaphenoxycyclotriphosphazene is not less than 99%. The preparation method of the invention has the advantage that the yield is as high as 95%, the type of the used solvent is less, the catalyst can be recycled to use, the consumption of the catalyst is low, the method is simple and is applicable to industrialized production and the purity of the product is high.

Description

technical field [0001] The invention belongs to the technical field of nitrogen and phosphorus-containing organic compound synthesis, and in particular relates to a method for producing high-purity hexaphenoxycyclotriphosphazene. Background technique [0002] Phenoxycyclotriphosphazene (PCPZ) is a cyclic phosphazene compound, which is light yellow or white powder or crystal. It can be directly added to polyethylene to prepare flame-retardant polyethylene materials. The LOI value of the material can reach 30.0~33.0. It can also be prepared into an emulsion, which can be used for flame retardant finishing of fibers, yarns and fabrics by dipping-drying method, spraying method or coating method, and can be added to viscose fiber spinning solution to obtain an LOI value of 25.3-26.7 flame retardant viscose fiber. [0003] Phenoxycyclotriphosphazene can be prepared by substitution reaction between chlorinated cyclic phosphazene and sodium phenate. At present, sodium metal or sod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6593B01J31/06
CPCY02P20/584
Inventor 路庆昌周晓王淑华
Owner SHANDONG ZESHI NEW MATERIALS TECH CO LTD
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