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Ethylenediamine bicyclo-tetra methylenemelamine phosphonate compound and preparation method thereof

A technology of ethylenediamine bicyclic tetramethylene phosphonic acid melamine salt compound and ethylenediamine tetramethylene phosphonic acid, which is applied in three fields, can solve the problems that cannot meet the requirements of environmental protection, the reaction process is complicated, and the product purity is not high. Achieve the effects of improving carbon formation and flame retardancy, simple and controllable reaction, and easy access to synthetic raw materials

Inactive Publication Date: 2012-09-19
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the traditional phosphorus-based flame retardants have defects such as volatility and easy hydrolysis. Therefore, the development of phosphorus-based flame retardants with low volatility and low hydrolysis is the focus of future development.
Chinese patent CN101429438A describes a phosphorus-nitrogen intumescent flame retardant 5,5-dimethyl-4-p-chlorophenyl-1 prepared by reacting p-chlorobenzaldehyde, isobutyraldehyde, phosphoric acid and melamine as raw materials , the method of melamine salt of 3,2-dioxaphosphorinyl phosphate, its reaction needs three steps to carry out, and reaction process is more numerous and diverse, and product purity is not high, and the flame retardant that makes contains halogen, still can't meet the requirement of environmental protection Require

Method used

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  • Ethylenediamine bicyclo-tetra methylenemelamine phosphonate compound and preparation method thereof
  • Ethylenediamine bicyclo-tetra methylenemelamine phosphonate compound and preparation method thereof
  • Ethylenediamine bicyclo-tetra methylenemelamine phosphonate compound and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0020] Dissolve ethylenediaminetetramethylenephosphonic acid in water, add melamine, the molar ratio of melamine to ethylenediaminetetramethylenephosphonic acid is 1:0.20, adjust the temperature to 60°C and stir, and continue to react for 6 hours. After completion, filter and dry to obtain the reaction intermediate ethylenediamine tetramethylene phosphonic acid melamine salt. The temperature of the above-mentioned reaction intermediate is raised to 180°C, and the reaction is continued for 10 hours, and the intermediate is subjected to a dehydration reaction to obtain the final product ethylenediamine bicyclic tetramethylene phosphonic acid melamine salt compound, whose structural formula is

[0021]

[0022] Its thermal decomposition temperature is determined to be 283±2°C.

Embodiment 2

[0024] Dissolve ethylenediaminetetramethylenephosphonic acid in water, add melamine, the molar ratio of melamine to ethylenediaminetetramethylenephosphonic acid is 1:0.31, adjust the temperature to 100°C and stir, and continue to react for 2 hours. After completion, filter and dry to obtain the reaction intermediate ethylenediamine tetramethylene phosphonic acid melamine salt. The temperature of the above-mentioned reaction intermediate was raised to 160° C., and the reaction was continued for 16 hours to dehydrate the intermediate to obtain the final product ethylenediamine bicyclic tetramethylene phosphonic acid melamine salt compound.

[0025] Its thermal decomposition temperature is determined to be 285±2°C.

Embodiment 3

[0027] Dissolve ethylenediaminetetramethylenephosphonic acid in water, add melamine, the molar ratio of melamine to ethylenediaminetetramethylenephosphonic acid is 1:0.50, adjust the temperature to 20°C and stir, and continue to react for 8 hours. After completion, filter and dry to obtain the reaction intermediate ethylenediamine tetramethylene phosphonic acid melamine salt. The temperature of the above-mentioned reaction intermediate was raised to 210° C., and the reaction was continued for 2 hours to dehydrate the intermediate to obtain the final product ethylenediamine bicyclic tetramethylene phosphonic acid melamine salt compound.

[0028] Its thermal decomposition temperature is determined to be 287±2°C.

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Abstract

The invention relates to an ethylenediamine bicyclo-tetra methylene melamine phosphonate compound and a preparation method thereof, in particular to a novel ethylenediamine bicyclo-tetra methylene melamine phosphonate for polymer flame retardance and the preparation method thereof. The compound synthesized by a two-step method has the characteristics of high phosphor / nitrogen content, high thermal stability, good hydrolysis resistance and the like, wherein due to triazine ring and phosphor-oxygen-nitrogen six-membered heterocyclic ring in the molecular structure, the thermal stability of the compound is greatly improved, the decomposition temperature of the compound is higher than 280 DEG C; and the charing property and flame retardance of a flame retarding system can be greatly improved due to the triazine ring structure in the molecular structure, and the excellent synergetic flame retarding effect of organic phosphor and six-membered heterocyclic ring can be represented. The compound synthesized by the invention can be widely applied to flame retardance of various synthetic materials and textiles such as polyolefin, polyurethane, nylon and polyester; raw materials for synthesizing the compound are easy to obtain, the production process is simple, and is suitable for industrial production and application.

Description

technical field [0001] The invention relates to an ethylenediamine bicyclic tetramethylene phosphonic acid melamine salt compound and a preparation method thereof, in particular to a novel ethylenediamine bicyclic tetramethylene phosphonic acid melamine salt compound which can be used for polymer flame retardancy and its preparation The method specifically relates to an ethylenediamine bicyclic tetramethylene phosphonic acid melamine salt compound containing a triazine ring and a phosphorus oxynitrogen six-membered heterocyclic ring and a preparation method thereof. Background technique [0002] Since the 1980s, flame retardants have become the largest additives used in synthetic materials next to plasticizers. With the development of the economy, people's awareness of environmental protection and safety has greatly improved, and they are more concerned about the ecological environment and the value of life. Traditional halogen-based flame retardants are widely used in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6587C07D251/56C08K5/5357
Inventor 彭治汉游丽华惠银银谭逸伦孙柳邵偲淳
Owner DONGHUA UNIV
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