Double base compound based on phosphonitrile and triazine group and preparation method of double base compound

A technology of triazine group and dihydroxy compound, which is applied in the fields of flame retardants and their preparation, double-radical compounds based on phosphazene and triazine groups and their preparation, achieving high char formation rate, good processability, thermal good stability effect

Active Publication Date: 2016-04-20
杭州志合新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Double base compound based on phosphonitrile and triazine group and preparation method of double base compound
  • Double base compound based on phosphonitrile and triazine group and preparation method of double base compound
  • Double base compound based on phosphonitrile and triazine group and preparation method of double base compound

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Embodiment 1

[0033] Step (1). Dissolve 2.00g cyanuric chloride in 15ml tetrahydrofuran solution, join in the tetrahydrofuran solution 40ml that is dissolved with 0.68g ethanolamine, add sodium carbonate 1.15g, in N 2 In the atmosphere, stir at -15°C for 2 hours to obtain 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound;

[0034] Step (2). Add 0.68g of hexachlorocyclotriphosphazene in 30ml of tetrahydrofuran to the 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound, add 1.15g of sodium carbonate, and heat at 50°C Condensation and reflux under stirring conditions for 5 hours;

[0035] Step (3). Add 1.30 g of ethylenediamine in 10 ml of tetrahydrofuran to the reaction solution; raise the temperature to 40° C., react under stirring and condensation conditions for 3 hours, continue to raise the temperature to 80° C., and react under stirring and condensation conditions 3 hours;

[0036] Step (4). After the reaction, suction filtration, water washing, and drying are performed to ...

Embodiment 2

[0039] Step (1). 4.00g cyanuric chloride is dissolved in 30ml acetone solution, joins in the acetone solution 50ml of 1.36g ethanolamine, adds potassium hydroxide 1.22g, in N 2 In the atmosphere, stir at -10°C for 2 hours to obtain 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound;

[0040] Step (2). Add 1.36g of hexachlorocyclotriphosphazene in 40ml of acetone solution to 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound, add 1.22.00g of potassium hydroxide, Condensation and reflux for 5 hours under stirring at 50°C;

[0041] Step (3). Add 2.80 g of hexamethylenediamine in 15 ml of acetone solution to the reaction solution; raise the temperature to 45° C., react under stirring and condensation conditions for 3 hours, continue to raise the temperature to 85° C., and react under stirring and condensation conditions 3 hours;

[0042] Step (4). After the reaction, suction filtration, water washing, and drying are performed to obtain a diradical compound based on p...

Embodiment 3

[0043] Step (1). 6.00g cyanuric chloride is dissolved in 40ml ethyl acetate solution, joins in the ethyl acetate solution 60ml that is dissolved with 2.05g ethanolamine, adds sodium hydroxide 1.30g, in N 2 In the atmosphere, stir at -5°C for 2.5 hours to obtain 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound;

[0044] Step (2). Add 2.05g of hexachlorocyclotriphosphazene in 50m ethyl acetate solution to 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound, add 1.30g of sodium hydroxide , condensed and refluxed for 5.5 hours under stirring at 55°C;

[0045] Step (3). Add 6.90 g of p-phenylenediamine in 25 ml of ethyl acetate solution to the reaction solution; raise the temperature to 55 ° C, stir and condense for 3 hours, continue to raise the temperature to 85 ° C, stir and condense Under conditions, react for 3 hours;

[0046] Step (4). After the reaction, suction filtration, water washing, and drying are performed to obtain a diradical compound based on phosphaze...

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Abstract

The invention discloses a double base compound based on phosphonitrile and triazine group. A preparation method of the double base compound comprises the following steps: introducing a triazine group into phosphonitrilic chloride trimer with intrinsically flame retardant property, and substituting six chlorine atoms on the side chains; further introducing a compound containing diamido or dyhydroxyl into the side chains of the triazine group, so as to obtain the double base compound based on phosphonitrile and triazine group. The compound is enriched in elements N and P; because the compound simultaneously contains the phosphonitrile and triazine group, the compound can achieve a flame-retardant effect in the combustion process by virtue of gas phase flame retardance and condensed phase mechanisms and has an excellent char-forming effect, and the generated carbon layer has the effects of insulating heat and inhibiting oxygen and achieves the effects of intumescent flame retardants. In addition, the phosphonitrile and triazine group have a synergistic flame retardant effect in the matrix combustion process. Moreover, the compound is high in heat stability, char-forming rate and processability and can be widely applied to flame-retardant modification of various high polymer materials.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a flame retardant and a preparation method thereof, in particular to a double-radical compound based on phosphazene and triazine groups and a preparation method thereof. Background technique [0002] Triazine compounds have become the focus of research because of their excellent char-forming properties, easy-to-react molecular characteristics and relatively low price. As early as 1990, CipolliR et al used triazine compounds and phosphides to construct self-extinguishing thermoplastic polymers or elastomers. In 2006, Li Bin et al. optimized the synthesis process of triazine and invented a triazine oligomer containing hydroxyl and diamine groups and applied it to polyolefins. Since then, people have continuously optimized and improved the structure of triazine compounds, and designed and synthesized a series of triazine derivatives. For example, triazine macromolecular co...

Claims

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Application Information

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IPC IPC(8): C07F9/6593C08K5/5399
CPCC07F9/65815C08K5/5399
Inventor 陈雅君钱立军王伟
Owner 杭州志合新材料有限公司
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