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Triazine ring structure containing caged organic phosphate and preparation method thereof

A technology of caged phosphate ester and triazine ring, which is applied in the field of caged phosphate ester containing triazine ring structure and its preparation, can solve the problems of large amount of mixed intumescent flame retardants and poor water resistance, and achieve improved material The effect of deterioration of mechanical properties, improvement of compatibility, improvement of char formation and flame retardancy

Active Publication Date: 2013-05-22
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The amount of mixed intumescent flame retardant is generally large, generally more than 20% (mass fraction) of the flame retardant material, and the water resistance is poor

Method used

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  • Triazine ring structure containing caged organic phosphate and preparation method thereof
  • Triazine ring structure containing caged organic phosphate and preparation method thereof
  • Triazine ring structure containing caged organic phosphate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Under the protection of high-purity nitrogen, add 92.2 g of cyanuric chloride and 800 mL of dioxane to a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser, and a dropping funnel, and stir for 30 minutes to disperse the cyanuric chloride Evenly, add 21.5g of piperazine, control the temperature in the ice bath at 0~5°C, react for 4 hours, then add PEPA180.1g, heat up to 25°C, continue to stir and react for 6 hours, then add 151.8g of triethylamine The amine was heated to 70° C., and the reaction was continued for 2 hours. After filtering, washing and drying, the final product, a caged phosphate ester DTPTP containing a triazine ring structure, was obtained.

Embodiment 2

[0036] Under the protection of high-purity nitrogen, add 92.2 g of cyanuric chloride and 800 mL of N,N-dimethylformamide to a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser, and a dropping funnel, and stir for 30 minutes to make The cyanuric chloride is evenly dispersed, then add 21.5g of piperazine, control the temperature in an ice bath at 0~5°C, and react for 6 hours, then add PEPA180.1g, heat up to 30°C, continue to stir and react for 8 hours, Add 177.1 g of triethylamine and raise the temperature to 80° C., continue the reaction for 4 hours, filter, wash and dry to obtain the final product, the caged phosphate DTPTP containing a triazine ring structure.

Embodiment 3

[0038] Under the protection of high-purity nitrogen, add 92.2 g of cyanuric chloride and 800 mL of N,N-dimethylacetamide to a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser, and a dropping funnel, and stir for 30 minutes to make The cyanuric chloride is evenly dispersed, then add 21.5g of piperazine, control the temperature in an ice bath at 0~5°C, react for 4 hours, then add PEPA180.1g, heat up to 25°C, continue to stir and react for 6 hours, 118.7g of pyridine was added and the temperature was raised to 70°C. After the reaction was continued for 2 hours, the final product was filtered, washed and dried to obtain the caged phosphoric acid ester DTPTP containing a triazine ring structure.

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Abstract

The invention discloses a triazine ring structure containing caged organic phosphate and a preparation method of the caged organic phosphate. Cyanuric chloride, piperazidine and 1-oxo-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo[2,2,2]octane (PEPA) are used as main raw materials to prepare the triazine ring structure containing caged organic phosphate, and the preparation method has the characteristics of accessible raw materials, simple, convenient and easy process, safe production and operation, and the like. According to the triazine ring structure containing caged organic phosphate disclosed by the invention, three components, namely, a carbon source, an acid source and a gas source are integrated in one molecular structure, phosphorus-nitrogen synergy and compatibility charring effect in the same molecule is exerted, charring performance and flame retardant performance of a flame retardant system are greatly improved, and in addition, the triazine ring structure and a caged structure both exist in the molecular structure so that the caged organic phosphate has extremely good thermal stability, can be used as a flame retardant in most polymer materials, and has good application prospect.

Description

technical field [0001] The invention relates to a cage-like phosphoric acid ester, in particular to a cage-like phosphoric acid ester containing a triazine ring structure and a preparation method thereof. Background technique [0002] With the development of polymer materials and the improvement of flame retardant requirements for materials, the research, production and application of flame retardants and flame retardant materials have also developed rapidly. Although halogen-based flame retardants have high flame retardant efficiency, they do not meet the current requirements for flame retardants for smoke suppression and environmental protection due to the large amount of smoke generated, and the released hydrogen halide gas is highly corrosive and has potential secondary hazards. The current development trend of flame retardants is low toxicity, low smoke, non-polluting halogen-free high-efficiency flame retardants, while intumescent flame retardants do not contain haloge...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/527C08L55/02
Inventor 彭治汉谭逸伦孙柳邵偲淳赵海珠周易
Owner DONGHUA UNIV
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