Synthetic method of phosphorus-nitrogen intumescent flame retardant

A technology of intumescent flame retardant and synthesis method, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problems of poor flame retardant efficiency, difficult synthesis process, and compatibility In order to avoid problems such as poor stability, achieve the effects of high product purity and yield, simple post-treatment process, and simple production conditions

Inactive Publication Date: 2012-12-19
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, halogen-based flame retardants will produce a large amount of corrosive and toxic gases during use and recycling, which will pollute the environment and seriously affect the performance of precision instrument components. It is urgent to develop new low-smoke, low-toxic halogen-free environmental protection Type flame retardants and flame retardant polymer materials to replace halogenated flame retardants
For halogen-free flame retardants, nitrogen-based flame retardants have the disadvantages of poor compatibility with the matrix resin, which is not conducive to dispersion in the matrix, and poor flame retardant efficiency; and silicon-based flame retardants are a new type of flame retardant There is a problem that the synthesis process is difficult and the research depth is not sufficient; therefore, the research hotspots in recent years have mainly focused on phosphorus-containing structural flame retardants
[0006] However, some phosphorus-based flame retardants that have been developed now still encounter some problems in thermal stability, exudation and processing when they are used in plastic flame retardancy.

Method used

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  • Synthetic method of phosphorus-nitrogen intumescent flame retardant
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Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add phenylphosphorous dichloride (8.950g, 0.05mol) and 100ml chloroform 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. 4,4'-Diaminodiphenylmethane (9.913g, 0.05mol) was dissolved in 50ml of chloroform and added to the constant pressure funnel. Under nitrogen protection and stirring, the 4,4'-diaminodiphenylmethane solution was slowly added dropwise. After the dropwise addition, the temperature was raised to the reflux temperature to continue the reaction for 4 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 100 ml of chloroform, and vacuum-dried at 100° C. for 6 hours to obtain 11.51 g of a light yellow solid with a yield of 75.6%.

Embodiment 2

[0022] Add phenyl phosphorus dichloride (8.950g, 0.05mol) 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 , 4,4'-diaminodiphenylmethane (9.913g, 0.05mol) was dissolved in 50ml of dichloromethane, and added to a constant pressure funnel. Under nitrogen protection and stirring, the 4,4'-diaminodiphenylmethane solution was slowly added dropwise. After the dropwise addition, the temperature was raised to the reflux temperature to continue the reaction for 4 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 100 ml of dichloromethane, and vacuum-dried at 100° C. for 6 hours to obtain 12.04 g of a light yellow solid with a yield of 79.1%.

Embodiment 3

[0024] Add phenyl phosphorus dichloride (26.85g, 0.15mol) and 200ml ethyl acetate to a 500ml four-neck flask equipped with a thermometer, nitrogen gas introduction, 100ml constant pressure dropping funnel, magneton, reflux condenser and tail gas absorption device , Dissolve 4,4'-diaminodiphenylmethane (29.74 g, 0.15 mol) in 100 ml ethyl acetate, and add it to a constant pressure funnel. Under nitrogen protection and stirring, the 4,4'-diaminodiphenylmethane solution was slowly added dropwise. After the dropwise addition, the temperature was raised to the reflux temperature to continue the reaction for 4 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 200 ml of ethyl acetate, and vacuum-dried at 100° C. for 6 hours to obtain 38.57 g of a light yellow solid with a yield of 84.5%.

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Abstract

A synthetic method of a phosphorus-nitrogen intumescent flame retardant relates to a synthetic method of a flame retardant, which comprises the following steps: respectively dissolving raw materials of dichlorophenylphosphine and 4,4'-diaminodiphenylmethane in solvents, introducing inert gas, stirring, slowly and dropwisely adding the 4,4'-diaminodiphenylmethane 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 light yellow powdery phosphorus-nitrogen intumescent flame retardant; the phosphorus-containing monomer and the nitrogen-containing monomer are combined into one compound through condensation polymerization reaction, and thus the flame retardant not only has good flame retardation, but also has the greatest advantage of good compatibility with polymer due to its large molecular weight. 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 method for synthesizing a flame retardant, in particular to a method for synthesizing a phosphorus-nitrogen expansion flame retardant. Background technique [0002] Since the advent of polymer materials, their flammability has become an inevitable defect during their use, and they release a lot of smoke and toxic gases during combustion, causing secondary hazards. However, due to the many excellent properties of polymer materials, people have to use a large number of polymer materials, so how to reduce the flammability of polymer materials has become the focus of people's research. [0003] Improving the flame retardant properties of polymer materials is mainly achieved by adding flame retardants to the composite material system and synthesizing new materials with flame retardant groups, that is, introducing some inorganic substances and chemical elements containing flame retardant chemical elements into the composite materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/02C08G79/02C07F9/50C08L79/02C08L85/02
Inventor 梁兵曹俊王长松洪晓东宁志高
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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