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Phosphorus-containing polyethylene polyamine flame retardant and preparation method thereof

A polyethylene polyamine and flame retardant technology, which is applied in the field of halogen-free flame retardant, can solve the problems of complex preparation process and low flame retardant efficiency, and achieves simple preparation method, improved flame retardant performance, improved weather resistance and mechanical performance. Effect

Pending Publication Date: 2020-02-28
HEFEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a phosphorus-containing polyethylene polyamine flame retardant and its preparation method in order to overcome the defects of complex preparation process and low flame retardant efficiency in the prior art

Method used

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  • Phosphorus-containing polyethylene polyamine flame retardant and preparation method thereof
  • Phosphorus-containing polyethylene polyamine flame retardant and preparation method thereof
  • Phosphorus-containing polyethylene polyamine flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Place 4.68 grams of polyethylene polyamine, 11.75 grams of potassium carbonate, 9.72 grams of tripropylamine and 40 milliliters of tetrahydrofuran in a three-necked flask, and add 27.40 grams of diphenyl chlorophosphate dropwise at 0°C under nitrogen, and the addition is complete Afterwards, the reaction was continued for 1 hour at 0°C and under nitrogen, then the temperature was raised to 30°C, and the reaction was carried out under nitrogen for 24 hours. Finally, the obtained product was filtered to remove the precipitate and then the solvent was removed. The obtained light yellow colloid was the phosphorus-containing polysaccharide Ethylene polyamine flame retardant.

[0023] figure 1 and figure 2 Respectively the target product prepared in embodiment 1 and the proton nuclear magnetic resonance spectrum of raw material polyethylene polyamine used 1 H NMR (400MHz, CDCl 3 ). From figure 1 and figure 2 It can be seen that the most significant difference between ...

Embodiment 2

[0026] Put 1.38 grams of polyethylene polyamine, 0.82 grams of sodium acetate, 1.23 grams of N-methylimidazole and 10 milliliters of 1,4-dioxane in a three-necked flask, and add 2.11 grams of After the addition of diethylphosphorous oxychloride, continue to react at 1°C and nitrogen for 1.5 hours, then raise the temperature to 35°C, and react for 12 hours under nitrogen, and finally filter the obtained product to remove the precipitate and remove the solvent. The yellow colloid is the phosphorus-containing polyethylene polyamine flame retardant of the present invention.

Embodiment 3

[0028] 13.75 grams of polyethylene polyamine, 15.90 grams of sodium carbonate, 16.42 grams of N-methylimidazole and 120 milliliters of dichloromethane were placed in a three-necked flask, and 47.33 grams of diphenylphosphine were added dropwise at 2°C under nitrogen. Acyl chloride, after the dropwise addition, continue to react at 2°C and nitrogen for 2 hours, then raise the temperature to 40°C, and react under nitrogen for 36 hours, and finally filter the product to remove the precipitate and remove the solvent, and the obtained light yellow colloid is the base Invented phosphorus-containing polyethylene polyamine flame retardant.

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Abstract

The invention belongs to the technical field of halogen-free flame retardance, and particularly relates to a phosphorus-containing polyethylene polyamine flame retardant and a preparation method thereof. The molecular structural formula is shown in the specification, wherein R is ethyl, phenyl, ethoxy or phenoxy. The preparation method comprises the following steps: dissolving a polyethylene polyamine into an organic solvent; adding an inorganic base and an organic base, dropwise adding phosphoryl chloride at 0-5 DEG C under the protection of nitrogen, continuously reacting after dropwise adding, heating to react under nitrogen condition, filtering an obtained product to remove precipitate, and removing the solvent to obtain a faint yellow colloid, namely the phosphorus-containing polyethylene polyamine flame retardant. The phosphorus-containing polyethylene polyamine flame retardant is high in phosphorus content and nitrogen content, and a synergistic flame retardant effect between phosphorus and nitrogen is achieved, so that in the heating or combustion process of a composite material, polymer carbonization, and oxygen and heat insulation can be rapidly promoted, and release of combustible gas and toxic flue gas is reduced. Meanwhile, a small amount of flame retardant synergist is matched, so that the flame retardant property of the composite material can be further improved.

Description

technical field [0001] The invention belongs to the technical field of halogen-free flame retardant, and in particular relates to a phosphorus-containing polyethylene polyamine flame retardant and a preparation method thereof. Background technique [0002] With the development of polymer material science and engineering, various polymer composite materials have gradually replaced traditional materials and are used in various fields of social production and life. However, most polymer materials are flammable, and polymer materials will generate a lot of smoke and toxic gases during heating or burning, which brings certain safety hazards to people's production and life. At present, the flame retardants used for polymer materials are mainly halogen-containing systems. Although the flame retardant efficiency of halogen-containing flame retardants is very high, due to the large amount of toxic smoke generated during combustion, some halogen-containing flame retardants Carcinogen...

Claims

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Application Information

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IPC IPC(8): C07F9/24C07F9/36C08K5/5399C08L75/04C08L23/00C08L25/06C08L77/00C08L63/00
CPCC07F9/2458C07F9/242C07F9/36C07F9/2408C08K5/5399C08L75/04C08L23/00C08L25/06C08L77/00C08L63/00C08L2201/02
Inventor 杨伟朱三娥吴菊孙宇鲁红典
Owner HEFEI UNIV
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