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A kind of flame retardant based on naphthylaminocyclotriphosphazene and preparation method thereof

A technology of naphthylaminocyclotriphosphazene and cyclotriphosphazene, which is applied in the field of flame retardants based on naphthylaminocyclotriphosphazene and its preparation, and can solve the problems of low thermal stability and affecting the performance of flame retardants , to achieve the effects of good thermal stability, excellent flame retardant effect and high thermal decomposition temperature

Inactive Publication Date: 2018-06-05
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, among the reported phosphazene flame retardants, the thermal stability of the nucleophilic substitution with hexachlorocyclotriphosphazene is low, which will inevitably affect the performance of the obtained flame retardants.

Method used

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  • A kind of flame retardant based on naphthylaminocyclotriphosphazene and preparation method thereof
  • A kind of flame retardant based on naphthylaminocyclotriphosphazene and preparation method thereof
  • A kind of flame retardant based on naphthylaminocyclotriphosphazene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 250ml three-necked round-bottomed flask equipped with a spherical condenser, mechanical stirring, and constant pressure dropping funnel, add 6.95g (0.02mol) of hexachlorocyclotriphosphazene and 10.28g (0.065mol) of 1,8-naphthalene diamine , toluene 100ml, stirring to dissolve the solid particles completely.

[0029] Weighed 12.12g (0.12mol) of triethylamine, slowly added dropwise to the above-prepared solution at room temperature, raised the temperature to 110°C and refluxed for 12h.

[0030] After cooling to room temperature, the reaction solution was suction-filtered, the toluene in the filtrate was recovered, and the filter cake was washed 3 times with deionized water, and then washed with tetrahydrofuran to remove the remaining raw materials in the solid, and vacuum-dried at 50°C for 10 h to obtain a light gray solid. That is the product tris-1,8-naphthalenediaminocyclotriphosphazene with a yield of 90.2%.

Embodiment 2

[0032] In a 250ml three-necked round-bottomed flask equipped with a spherical condenser, mechanical stirring, and constant pressure dropping funnel, add 12.28g (0.02mol) of hexabromocyclotriphosphazene and 10.28g (0.065mol) of 1,8-naphthalene diamine , add toluene 100ml, stir to dissolve the solid particles completely.

[0033] Weighed 12.12g (0.12mol) of triethylamine, slowly added dropwise to the above-prepared solution at room temperature, raised the temperature to 110°C and refluxed for 12h.

[0034] After cooling to room temperature, the reaction solution was suction-filtered, the toluene in the filtrate was recovered, and the filter cake was washed 3 times with deionized water, and then washed with tetrahydrofuran to remove the remaining raw materials in the solid, and vacuum-dried at 50°C for 10 h to obtain a light gray solid. That is the product tris-1,8-naphthalenediaminocyclotriphosphazene with a yield of 93.2%.

Embodiment 3

[0036] In a 250ml three-neck round-bottomed flask equipped with a spherical condenser, mechanical stirring, and constant pressure dropping funnel, add 6.95g (0.02mol) of hexachlorocyclotriphosphazene and 18.62g (0.13mol) of 1-naphthylamine, and add toluene 100ml, stir to dissolve the solid particles completely.

[0037] Weighed 12.12g (0.12mol) of triethylamine, slowly added dropwise to the above-prepared solution at room temperature, raised the temperature to 110°C and refluxed for 12h.

[0038] After cooling to room temperature, suction filter the reaction solution, recover the toluene in the filtrate, wash the filter cake 3 times with deionized water, and then wash with tetrahydrofuran to remove the remaining raw materials in the solid, and vacuum-dry at 50°C for 10 hours to obtain a solid powder, which is The product hexanaphthylaminocyclotriphosphazene has a yield of 91.5%.

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Abstract

The invention relates to a flame retardant based on naphthylaminocyclotriphosphazene and a preparation method thereof. The preparation method of the present invention comprises: adding a certain ratio of hexa-substituted cyclotriphosphazene, naphthalene amino compound, and toluene into the reaction device, stirring, feeding nitrogen protection, and adding acid-binding agent three to the system dropwise at room temperature. Ethylamine, heated to 50-115°C, reacted for 12 hours, cooled to room temperature, filtered with suction, washed with water, then washed with tetrahydrofuran, and vacuum-dried to obtain the target product. The flame retardant of the present invention has the advantages of simple synthesis method, rich source of raw materials, good thermal stability, high combustion char formation rate and excellent flame retardant performance.

Description

technical field [0001] The invention relates to a flame retardant and its preparation, in particular to a naphthalene aminocyclotriphosphazene-based flame retardant and a preparation method thereof. Background technique [0002] At present, the domestic market for organic flame retardants is mainly halogen-based and phosphorus-based. Phosphorus-based flame retardants have the functions of flame retardancy, heat insulation, and oxygen insulation, and produce less smoke, are not easy to generate harmful gases, and have relatively little pollution to the environment. Phosphazene flame retardant is a phosphorus-containing flame retardant with excellent flame retardant effect. It has excellent flame retardant performance due to its high content of N and P elements. [0003] Phosphazene compounds are a typical class of organic-inorganic hybrid flame retardants. It not only has the processing superiority of organic flame retardants and the compatibility of polymer matrix, but also...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6593C08K5/5399
Inventor 张海良胡峰
Owner XIANGTAN UNIV
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