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Cyclotriphosphazene derivative containing sulfydryl group and preparation method thereof

A technology for cyclotriphosphazene and derivatives, which is applied in the field of cyclotriphosphazene derivatives and their preparation, and phosphazene derivatives, can solve the problems of few applications, achieve good repeatability, mild reaction conditions, and high yield Effect

Active Publication Date: 2014-02-12
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Sulfur element is an excellent flame retardant element, which is currently less used in halogen-free flame retardants

Method used

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  • Cyclotriphosphazene derivative containing sulfydryl group and preparation method thereof
  • Cyclotriphosphazene derivative containing sulfydryl group and preparation method thereof
  • Cyclotriphosphazene derivative containing sulfydryl group and preparation method thereof

Examples

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Effect test

Embodiment 1

[0027] Dissolve 5.4g of thiophenol in 25ml of tetrahydrofuran, stir magnetically to fully dissolve, then add 1.05g of sodium hydride, slowly heat to 45°C, and drop 1.74g of hexachlorocyclotriphosphazene into the above tetrahydrofuran solution, at 45 Under the condition of ℃, react for 20h. After the reaction, the obtained liquid was suction-filtered to remove by-products, and vacuum rotary evaporation was used to remove tetrahydrofuran and excess raw materials in the system. Finally, the target product was a light yellow-green liquid with a pungent odor. The productive rate is 82.6%; The spectrogram data of five and six substituted cyclotriphosphazene derivatives containing mercapto groups are:

[0028] FT-IR (cm -1 ): 2500—2600 (Sulfhydryl), 3000—3100 (C=C), 1440—1510 (C-H) 1163 (P=N). 31 P NMR (CDCl 3 , δ, ppm, TMS): 40—50 (6P, -P-S-), 18—22 (1P, -P-Cl).

Embodiment 2

[0030] Dissolve 5.4g of thiophenol in 25ml of tetrahydrofuran, stir magnetically to fully dissolve, then add 1.05g of sodium hydride, slowly heat to 55°C, and drop 1.74g of hexachlorocyclotriphosphazene into the above tetrahydrofuran solution, at 55 Under the condition of ℃, react for 20h. The liquid obtained after the reaction was filtered to remove by-products, vacuum rotary evaporation to remove tetrahydrofuran and excess raw materials in the system, and finally the target product obtained was a light yellow-green liquid with a pungent smell. The yield is 83.2%;

Embodiment 3

[0032] Dissolve 5.4g of thiophenol in 25ml of tetrahydrofuran, stir magnetically to fully dissolve, then add 1.05g of sodium hydride, slowly heat to 65°C, and drop 1.74g of hexachlorocyclotriphosphazene into the above tetrahydrofuran solution, at 65 Under the condition of ℃, react for 20h. The liquid obtained after the reaction was filtered to remove by-products, vacuum rotary evaporation to remove tetrahydrofuran and excess raw materials in the system, and finally the target product obtained was a light yellow-green liquid with a pungent smell. The yield is 84.6%;

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Abstract

The invention relates to a cyclotriphosphazene derivative containing a sulfydryl group and a preparation method thereof, and belongs to the technical field of processing aids. The method comprises the following steps: adding thiophenol and a solvent to a reactor in an inert gas atmosphere; simultaneously, slowly adding a sodium compound to stir, and adding phosphonitrilic chloride trimer, so as to obtain reaction liquid, wherein the reaction temperature is 20-120 DEG C; leaching a reaction by-product, and removing the solvent by evaporating; and finally obtaining the cyclotriphosphazene derivative containing the sulfydryl group. By adopting the preparation method, the nucleophilic substitution is carried out by using sulfydryl and the phosphonitrilic chloride trimer; a hexasubstituted cyclotriphosphazene derivative (named) containing the sulfydryl group, which is accompanied with a little of incompletely-substituted penta-substitution product, is successfully synthetized; the molar ratio of the hexasubstituted cyclotriphosphazene derivative to the incompletely-substituted penta-substitution product is 2.61:1. The preparation method disclosed by the invention is mild in reaction condition, and has the characteristics of being easy to control, good in repeatability, high in yield and the like.

Description

technical field [0001] The invention relates to a cyclotriphosphazene derivative containing a mercapto group and a preparation method thereof. The phosphazene derivative is added to a polymer material as an improved auxiliary agent and belongs to the technical field of processing aids. Background technique [0002] The phosphazene compound contains two flame retardant elements, phosphorus and nitrogen, and is a new type of phosphorus / nitrogen halogen-free flame retardant with great potential. According to the shape of phosphorus and nitrogen skeleton, it can be divided into two categories: cyclic phosphazene and linear phosphazene. Cyclic phosphazene is a six-membered cyclic compound formed by alternately connecting P and N single and double bonds. Each phosphorus atom is connected with two chlorine atoms. Since the chlorine atoms on the side chain are highly active and unstable, they can be combined with some The SN2 nucleophilic substitution reaction of organic small mole...

Claims

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Application Information

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IPC IPC(8): C07F9/6593
Inventor 李定华张毅杨荣杰
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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