Preparation method of hexaphenoxycyclotriphosphazene (HPCTP)

Abstract

The invention discloses a preparation method of hexaphenoxycyclotriphosphazene (HPCTP), which comprises the following steps: 1) uniformly dispersing phenol and an alkali metal hydroxide into methyl alcohol, and performing backflow reaction under the protection of inert gas; 2) removing and recycling the methyl alcohol solvent, cooling the obtained product, and drying; 3) placing the phenolate and the solvent obtained from the former previous step into a reaction kettle, and dropwise adding a ketone solution of phosphonitrilic chloride trimer into the reaction kettle; 4) performing the backflow reaction; 5) after reaction, removing and recycling the solvent; 6) adding deionized water into the reaction kettle, stirring to disperse the product uniformly, discharging the material for centrifugation, washing repeatedly until the pH value of the filtrate indicates neutral; 7) drying the product obtained from the previous step, so as to obtain a coarse product; 8) heating the coarse product and an alcohol solvent, stirring, cooling to less than 25 DEG C, and performing suction filtration to obtain a product; 9) drying the product. The preparation method is simple in process, low in energy consumption and high in yield, the solvent can be recycled, and the purity of the product is higher.

Description

technical field [0001] The invention relates to a preparation method of hexaphenoxycyclotriphosphazene. Background technique [0002] Hexaphenoxy cyclotriphosphazene Cyclotriphosphazene is a good halogen-free and environmentally friendly green flame retardant, used for large-scale integrated circuit packaging; epoxy resin molding compound, copper clad laminate, powder coating, LED light-emitting tube and The flame retardant of other polymer materials complies with EU REACH regulations and ROHS standards. It can achieve UL 94 V-0 flame retardant performance, and its flame retardant performance is much better than traditional flame retardant systems. [0003] Gabino A.Carriedo et al. published an article "On the synthesis of functionalized cyclic and polmeric aryloxyphosphazenes from phenols" in which acetone was used as solvent, potassium carbonate was used as acid binding agent, tetrabutylammonium bromide was used as catalyst, and the reactant was distilled and concentrated...

AI Technical Summary

Problems solved by technology

[0005] U.S. Patent No. 4124557 invented sodium phenate anhydrous dioxane solution and added it dropwise into hexachlorocyclotriphosphazene anhydrous dioxane solution under stirring at room temperature, refluxed for 5 hours, and poured the reactant into a large amount of deionized water after overnight reaction. The product was then washed with copious amounts of deionized water, yield 97%, purity not mentioned

Dioxane is easy to form explosive peroxide when there is no water, the experiment is dangerous and not conducive to production

[0008] To sum up, the existing synthetic methods of hexaphenoxycyclotriphosphazene have their own characteristics, but to a certain extent, they are dangerous, use a large amount of reaction solvent, complex operation, cumbersome post-treatment, difficult separation and purification, and high energy consumption. , high pollution, low yield, low quality and other problems, it is difficult to be accepted by industrial production

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