Preparation method of polymeric phosphorus-nitrogen flame retardant

A phosphorus-nitrogen flame retardant, a polymerized technology, is applied in the field of the preparation of polymerized phosphorus-nitrogen flame retardants, and can solve the problem of mechanical properties such as elongation at break, tensile strength, etc. The effect is not obvious and other problems, to achieve the effect of simple post-processing process, simple production conditions, high product purity and yield

Inactive Publication Date: 2015-01-21
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since polyolefin is a non-polar material, it has poor compatibility with highly polar inorganic flame retardants, resulting in uneven dispersion of flame retardants, and the flame retardant effect is not obvious, and the addition of a large amount of inorganic flame retardants will make the material Decreased mechanical properties such as elongation at break and tensile strength

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add phenylphosphorous dichloride (8.950g, 0.05mol) and 50ml ethyl acetate to a 250ml four-neck flask equipped with a thermometer, nitrogen gas introduction, 100ml constant pressure dropping funnel, magneton, reflux condenser and tail gas absorption device , Dissolving m-xylylenediamine (6.870g, 0.05mol) in 50ml ethyl acetate was added to a constant pressure funnel. Under nitrogen protection and stirring, m-xylylenediamine solution was slowly added dropwise. After the dropwise addition, the temperature was raised to the reflux temperature to continue the reaction for 5 hours, and after the reaction was completed, the nitrogen was continued. 2 Bring to room temperature. Then the mixture was suction-filtered under reduced pressure, and the filter cake was washed with 100 ml of ethyl acetate, and vacuum-dried at 100° C. for 6 hours to obtain 10.63 g of a white solid, with a yield of 87.3%.

Embodiment 2

[0020] Add phenylphosphorous dichloride (8.950g, 0.05mol) and 50ml chloroform to a 250ml four-necked flask equipped with a thermometer, nitrogen gas introduction, 100ml constant pressure dropping funnel, magneton, reflux condenser and tail gas absorption device. m-Xylylenediamine (6.870g, 0.05mol) was dissolved in 50ml of chloroform and added to the constant pressure funnel. Under nitrogen protection and stirring, m-xylylenediamine solution was slowly added dropwise. After the dropwise addition, the temperature was raised to the reflux temperature to continue the reaction for 6 hours, and after the reaction was completed, the nitrogen was continued. 2 Bring to room temperature. Then the mixture was suction-filtered under reduced pressure, and the filter cake was washed with 100 ml of chloroform, and vacuum-dried at 100° C. for 6 hours to obtain 9.31 g of a white solid, with a yield of 76.5%.

Embodiment 3

[0022] Add phenyl phosphorus dichloride (26.85g, 0.15mol) and 100ml dichloromethane to a 250ml four-neck flask equipped with a thermometer, nitrogen gas introduction, 100ml constant pressure dropping funnel, magneton, reflux condenser and tail gas absorption device , m-xylylenediamine (20.61g, 0.15mol) was dissolved in 100ml of dichloromethane, and added to a constant pressure funnel. Under nitrogen protection and stirring, m-xylylenediamine solution was slowly added dropwise. After the dropwise addition was completed, the temperature was raised to reflux temperature and the reaction was continued for 7 hours, and the N was continued after the reaction was completed. 2 Bring to room temperature. Then the mixture was suction-filtered under reduced pressure, and the filter cake was washed with 200ml of dichloromethane, and vacuum-dried at 100°C for 6 hours to obtain 28.53g of white solid, with a yield of 78.1%.

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Abstract

A preparation method of a polymeric phosphorus-nitrogen flame retardant relates to a preparation method of a flame retardant, and the method comprises the following procedures: respectively dissolving dichlorophenylphosphine and m-xylylenediamine in solvents, introducing inert gas, stirring, slowly and dropwisely adding the m-xylylenediamine solution into the dichlorophenylphosphine solution, after dropwise addition, performing reflux reaction for 2-10 hours, cooling, performing suction filtration, washing, and drying to obtain the white powdery polymeric phosphorus-nitrogen flame retardant; the compound can be used as a flame retardant additive for various polymers to improve the flame retardation of the polymers. According to the invention, the production process condition is simple; the product purity and yield are high; and the post-treatment process is simple.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of a polymeric phosphorus nitrogen flame retardant. Background technique [0002] Combustion of polymers is a very complex and violent thermal oxidation process, often accompanied by flames, thick smoke, poisonous gas, etc.; during combustion, polymers are violently thermally decomposed to produce volatile combustible substances. When the substances reach a certain temperature and concentration, It will catch fire again, release heat continuously, decompose more polymers or difficult-to-decompose substances, and produce more combustibles, such a vicious circle, the result is that the combustion continues to expand, causing fires and endangering people's lives and property . With the wider application of polymer materials in aviation, transportation, electrical appliances and other fields, their flame retardancy has become the key reason for limit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/02C07F9/50C08K5/5399C08L85/02
Inventor 梁兵曹俊洪晓东王长松宁志高
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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