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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 problems such as post-processing troubles and increase production costs, and achieve simplified separation and purification way, reduce the formation of by-products, and improve the effect of product yield and purity

Active Publication Date: 2017-12-19
山东旭锐新材股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patented method has simple process, high yield, and no catalyst, but the solvent is a mixture of chlorobenzene and water, which is troublesome for post-processing and increases production costs.

Method used

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  • Preparation method of hexaphenoxycyclotriphosphazene
  • Preparation method of hexaphenoxycyclotriphosphazene
  • Preparation method of hexaphenoxycyclotriphosphazene

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Add ammonium chloride, inert solvent chlorobenzene, and a mixed catalyst of magnesium chloride and pyridine with a mass ratio of 1:3 to the synthesis kettle, mix evenly and heat up to 135°C, and use a frequency conversion solid feeder to dissolve phosphorus pentachloride within 10 hours. The solid is evenly dropped into the synthesis kettle, the consumption of chlorobenzene is 1.5 times that of phosphorus pentachloride, and the mass ratio of phosphorus pentachloride, ammonium chloride, and mixed catalyst is 1:0.28:0.06; keep the temperature at 135 ° C until the end of the reaction. After the complete reaction of phosphorus chloride is completed, the temperature is lowered to 40°C, excess ammonium chloride and catalyst are filtered out, the solvent is removed from the feed solution under reduced pressure, the temperature is lowered to 10°C, and hexachlorocyclotriphosphazene is obtained by centrifugation.

[0035] Add the inert solvent chlorobenzene, phenol, sodium hydroxi...

Embodiment 2

[0038] Add ammonium chloride, inert solvent toluene, and a mixed catalyst of zinc chloride and pyridine with a mass ratio of 1:2.5 to the synthesis kettle, mix well and then heat up to 115°C, and use a frequency conversion solid feeder to dissolve pentachloride within 15 hours. Phosphorus solids are evenly put into the synthesis kettle, the amount of inert solvent toluene is twice that of phosphorus pentachloride, and the mass ratio of phosphorus pentachloride, ammonium chloride, and mixed catalyst is 1:0.25:0.04; keep the temperature at 115°C until the end of the reaction After the complete reaction of phosphorus pentachloride is completed, cool down to 40°C, filter out excess ammonium chloride and catalyst, remove the solvent toluene from the feed solution under reduced pressure, cool down to 10°C, and centrifuge to obtain hexachlorocyclotriphosphazene.

[0039] Add inert solvent toluene, phenol, potassium hydroxide and water into the synthesis kettle, stir and dissolve, then...

Embodiment 3

[0042]Add ammonium chloride, inert solvent tetrachloroethane, and a mixed catalyst of magnesium chloride and pyridine with a mass ratio of 1:3 in the synthesis kettle, mix well and then heat up to 145°C, and use a frequency conversion solid feeder to dissolve the pentachloride within 12 hours. Phosphate solids are evenly put into the synthesis kettle, the amount of inert solvent tetrachloroethane is 3 times that of phosphorus pentachloride, and the mass ratio of phosphorus pentachloride, ammonium chloride, and mixed catalyst is 1:0.3:0.08; keep the temperature at 145 °C to the end of the reaction, after the complete reaction of phosphorus pentachloride is completed, cool down to 40 °C, filter out excess ammonium chloride and catalyst, remove the solvent tetrachloroethane from the feed solution under reduced pressure, cool down to 10 °C, and centrifuge to obtain six Chlorocyclotriphosphazene.

[0043] Add the inert solvent tetrachloroethane, phenol, sodium hydroxide and water i...

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Abstract

The invention discloses a preparation method of hexaphenoxycyclotriphosphazene. The preparation method comprises the following steps: (1) adding ammonium chloride, an inert solvent and a catalyst into a synthesis kettle, heating to 100-145 DEG C, uniformly putting phosphorus pentachloride into the synthesis kettle within 5-40 hours, and after the reaction is ended, carrying out filtrate concentration and cooling crystallization to obtain phosphonitrilic chloride trimer; (2) adding the inert solvent, phenol, alkali metal hydroxide and water into the synthesis kettle, heating to 100-145 DEG C, dropwise adding an inert solvent solution of phosphonitrilic chloride trimer after azeotropic separation of water, insulating and carrying out reflux reaction; and (3) adding a chloride-ion removing agent, continuously reacting for 3-6 hours at the temperature of 100-135 DEG C, then carrying out alkali washing, acid washing, water washing and steam distillation, and drying to obtain granular hexaphenoxycyclotriphosphazene with low chloride content. The preparation method disclosed by the invention has the advantages that the process is simple, the obtained product is low in chloride content and the stability is good in the use process.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation technology of hexaphenoxycyclotriphosphazene. Background technique [0002] Phosphazene compound is a kind of inorganic compound with alternating double bonds of P and N as the main chain structure. It exists in a ring or linear structure. A phenoxy group is connected to the phosphorus atom to obtain hexaphenoxycyclotriphosphazene, benzene The introduction of oxygen makes the phosphazene compound a combination of inorganic compounds and organic compounds. Due to the good synergistic effect between phosphorus and nitrogen, it has a high thermal decomposition temperature and flame retardant effect, and has less smoke and toxic gases. , good compatibility with polymer materials, remarkable flame retardant efficiency and other outstanding features, has become one of the hot spots in the current research of halogen-free flame retardant. [0003] There are many...

Claims

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Application Information

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IPC IPC(8): C07F9/6593
CPCC07F9/65815
Inventor 张荣华王强李金忠秦新华杨清波郭文君陶书伟
Owner 山东旭锐新材股份有限公司
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