Phosphorus-nitrogen type fire retardant and preparation method thereof

A flame retardant, diaminodiphenylmethane technology, applied in the field of flame retardants and their preparation, can solve problems such as hazards, flammability of polymer materials, etc., and achieve the effects of wide use, convenient operation, and improved flame retardant performance

Inactive Publication Date: 2017-06-16
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most polymer materials are flammable, and while bringing convenience to people's lives, they also bring great harm

Method used

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  • Phosphorus-nitrogen type fire retardant and preparation method thereof
  • Phosphorus-nitrogen type fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0025] Step 1: Add 3.97g of 4,4'-diaminodiphenylmethane and 1g of glutaraldehyde to a 250ml three-necked flask equipped with a magnetic stirrer, a reflux condenser, a thermometer, a nitrogen inlet tube and an exhaust gas absorption device, and add 20ml Dichloromethane was used as a solvent, nitrogen gas was passed through, the temperature was raised to 30° C., and then reacted for 5 hours. After the reaction was completed, it was cooled to room temperature, and the intermediate was obtained by suction filtration, washing, and drying.

[0026] Step 2: Add 4.61g of intermediates and 4.32g of DOPO to a 250ml three-neck flask equipped with a magnetic stirrer, reflux condenser, thermometer, nitrogen inlet tube and tail gas absorption device, add 20ml of toluene as a solvent, and feed nitrogen to raise the temperature After reaching 50°C, react for 5 hours. After the reaction, cool to room temperature, filter with suction, wash, and dry to obtain a phosphorus and nitrogen type flame ...

example 2

[0028] Step 1: Add 4.36g of 4,4'-diaminodiphenylmethane and 1g of glutaraldehyde to a 250ml three-neck flask equipped with a magnetic stirrer, a reflux condenser, a thermometer, a nitrogen inlet tube and an exhaust gas absorption device, and add 30ml Ethanol was used as a solvent, and nitrogen gas was passed through, and the temperature was raised to 30° C. and then reacted for 6 hours. After the reaction was completed, it was cooled to room temperature, and the intermediate was obtained by suction filtration, washing, and drying.

[0029] Second step: add 4.61g intermediate and 4.75g DOPO to the 250ml there-necked flask equipped with magnetic stirrer, reflux condenser, thermometer, nitrogen inlet pipe and tail gas absorption device, add 40ml xylene as solvent, feed nitrogen, Raise the temperature to 60°C and react for 6 hours. After the reaction, cool to room temperature, filter with suction, wash and dry to obtain a phosphorus and nitrogen type flame retardant.

example 3

[0031] Step 1: Add 4.76g of 4,4'-diaminodiphenylmethane and 1g of glutaraldehyde to a 250ml three-neck flask equipped with a magnetic stirrer, a reflux condenser, a thermometer, a nitrogen inlet tube and an exhaust gas absorption device, and add 30ml Acetonitrile was used as a solvent, and nitrogen gas was passed through, and the temperature was raised to 50° C. and then reacted for 6 hours. After the reaction was completed, it was cooled to room temperature, and the intermediate was obtained by suction filtration, washing, and drying.

[0032] Second step: add 4.61g intermediate and 5.18g DOPO to the 250ml there-necked flask equipped with magnetic stirrer, reflux condenser, thermometer, nitrogen inlet pipe and tail gas absorption device, add 30ml xylene as solvent, feed nitrogen, Raise the temperature to 70°C and react for 7 hours. After the reaction, cool to room temperature, filter with suction, wash and dry to obtain a phosphorus and nitrogen type flame retardant.

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PUM

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Abstract

The invention relates to a fire retardant and a preparation method thereof, and concretely relates to a phosphorus-nitrogen type fire retardant and a preparation method thereof. The structural formula of the phosphorus-nitrogen type fire retardant is shown in the description. Raw materials for preparing the fire retardant comprise 4,4'-diaminodiphenylmethane, glutaraldehyde and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO). The preparation method of the fire retardant comprises the following steps: 1, reacting 4,4'-diaminodiphenylmethane with glutaraldehyde under an inert gas condition to synthesize an intermediate; and 2, reacting the synthesized intermediate with the DOPO, and carrying out filtering, washing and drying treatment to obtain the fire retardant. The fire retardant has the characteristics of no halogen and low toxicity, and can be applied to polymeric materials in order to improve the fire retardation performance of the polymeric materials.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a phosphorus and nitrogen type flame retardant and a preparation method thereof. Background technique [0002] Polymer materials have incomparable properties in many aspects, so they are widely used in many aspects of life, and have become indispensable materials in national defense construction and national economy. However, most polymer materials are flammable, and while bringing convenience to people's lives, they also bring great harm. This has also promoted the rapid development of flame retardants. The halogen-free and low-toxicity of flame retardants has become an inevitable trend in the development of flame retardants in the future. Contents of the invention [0003] The purpose of the present invention is to provide a phosphorus and nitrogen type flame retardant and its preparation method. The phosphorus and nitrogen type flame retardant prepared b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/5313
CPCC07F9/657172C08K5/5313
Inventor 梁兵刘莹
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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