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Method for synthesizing phenoxycycloposphazene

A technology of hexaphenoxycyclotriphosphazene and hexachlorocyclotriphosphazene, which is applied in the field of phosphazene compound synthesis, can solve the problems of unfavorable industrial transformation, difficult recovery of reaction solvent, and low reaction temperature, and achieve easy control and equipment The effect of small footprint and high synthesis efficiency

Inactive Publication Date: 2020-02-07
山东省海洋化工科学研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction temperature of this homogeneous system is low, the reaction time is long, the reaction solvent is difficult to recover, the product yield is only 85%, the cost is high, and it is not conducive to industrial transformation

Method used

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  • Method for synthesizing phenoxycycloposphazene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The synthetic method of hexaphenoxy cyclotriphosphazene comprises the following steps:

[0027] (1) Add chlorobenzene, hexachlorocyclotriphosphazene and tetrabutylammonium chloride into the organic phase raw material preparation kettle 1, stir and dissolve to obtain the organic phase raw material, and the content of hexachlorocyclotriphosphazene in the organic phase raw material is 225 g / L, the consumption of tetrabutylammonium chloride is 4% of hexachlorocyclotriphosphazene quality; Sodium hydroxide aqueous solution and phenol are added in the preparation kettle 2 of water phase raw material, react and generate sodium phenate, make water phase raw material, The sodium phenate content of the aqueous phase raw material is 450 g / L.

[0028] (2) Let the organic phase raw material in the organic phase raw material preparation kettle 1 flow into the centrifugal extractor 3 through the upper liquid inlet of the centrifugal extractor, and at the same time let the aqueous phase...

Embodiment 2

[0031] The synthetic method of hexaphenoxy cyclotriphosphazene comprises the following steps:

[0032] (1) Add o-dichlorobenzene, hexachlorocyclotriphosphazene and tetrabutylammonium bromide into the organic phase raw material preparation kettle 1, stir and dissolve to obtain the organic phase raw material, and the content of hexachlorocyclotriphosphazene in the organic phase raw material The amount of tetrabutylammonium bromide is 225 g / L, and the consumption of tetrabutylammonium bromide is 3% of the quality of hexachlorocyclotriphosphazene; sodium hydroxide aqueous solution and phenol are added in the water phase raw material preparation kettle 2, and the reaction generates sodium phenate, and the water phase Raw material, the sodium phenate content of aqueous phase raw material is 225 g / L.

[0033] (2) Let the organic phase raw material in the organic phase raw material preparation kettle 1 flow into the centrifugal extractor 3 through the upper liquid inlet of the centrifu...

Embodiment 3

[0036] The synthetic method of hexaphenoxy cyclotriphosphazene comprises the following steps:

[0037] (1) Add toluene, hexachlorocyclotriphosphazene and dodecyltrimethylammonium chloride into the organic phase raw material preparation kettle 1, stir and dissolve to obtain the organic phase raw material, the hexachlorocyclotriphosphazene of the organic phase raw material The content is 562.5 g / L, and the amount of dodecyltrimethylammonium chloride is 2% of the mass of hexachlorocyclotriphosphazene; sodium hydroxide aqueous solution and phenol are added to the water phase raw material preparation kettle 2, and the reaction generates sodium phenoxide , the aqueous phase raw material was obtained, and the sodium phenate content of the aqueous phase raw material was 225 g / L.

[0038] (2) Let the organic phase raw material in the organic phase raw material preparation kettle 1 flow into the centrifugal extractor 3 through the upper liquid inlet of the centrifugal extractor, and at ...

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Abstract

The invention discloses a method for synthesizing phenoxycycloposphazene. The method comprises the following steps: dissolving hexachlorocyclotriphosphazene and a phase transfer catalyst into an organic solvent so as to obtain an organic-phase raw material; by taking a sodium phenate aqueous solution as a water-phase raw material, simultaneously feeding the organic-phase raw material and the water-phase raw material into a multi-stage centrifugal extractor with a heating function, performing a multi-stage countercurrent reaction, dissolving generated phenoxycycloposphazene into an organic solvent to form an organic-phase reaction liquid, and dissolving generated sodium chloride into water to form a water-phase reaction liquid; and distilling the organic-phase reaction liquid supporting thephenoxycycloposphazene to remove the solvent, washing hot residues obtained after the solvent is removed by using a low-molecule alcohol, and performing solid-liquid separation after washing, so as to obtain the phenoxycycloposphazene. The method is possible in continuous production, simple in process and easy to control, and the product is high in yield and purity.

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 phosphazene compound synthesis. Background technique [0002] Hexaphenoxycyclotriphosphazene is a cyclic phosphazene compound, which is light yellow or off-white powder or crystal. It is a halogen-free flame retardant with high thermal decomposition temperature, excellent flame retardant effect, and smoke It is widely used in industries such as engineering plastics, high-end high-voltage cables, and copper-clad laminates. [0003] There are a lot of research reports on hexaphenoxycyclotriphosphazene at home and abroad. The current general process is to use hexachlorocyclotriphosphazene and sodium phenate to react to generate the target product. During the phenoxy substitution process, the steric hindrance effect will lead to insufficient phenoxy substitution degree and affect the yield of hexa...

Claims

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Application Information

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IPC IPC(8): C07F9/6593
CPCC07F9/65815
Inventor 耿建齐杨瑞光李远超李善清
Owner 山东省海洋化工科学研究院
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