Preparation method of phosphorus-nitrogen intumescent flame retardant

An intumescent flame retardant, phosphorus-nitrogen technology, applied in the field of flame retardant preparation, can solve the problems of poor compatibility, moisture absorption, large addition amount, etc., achieve good flame retardancy, reduce moisture absorption, weather resistance good effect

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

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Problems solved by technology

[0004] Although the intumescent flame retardant system has incomparable characteristics compared with other flame retardant systems, it also has many problems to be solved: 1. The addition amount is large. In order to obtain the required flame retardant effect, it is necessary to add A large amount of flame retardant is added to the material, which brings a series of problems such as cost and affecting the performance of composite materials; 2. Moisture absorption, becau

Method used

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  • Preparation method of phosphorus-nitrogen intumescent flame retardant
  • Preparation method of phosphorus-nitrogen intumescent flame retardant

Examples

Experimental program
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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 , Dissolve p-phenylenediamine (5.407g, 0.05mol) in 50ml ethyl acetate, and add it to the constant pressure funnel. Under nitrogen protection and stirring, the p-phenylenediamine solution was slowly added dropwise. After the dropwise addition was completed, the temperature was raised to reflux temperature and the reaction was continued for 3 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 5 hours to obtain 9.15 g of lavender solid, with a yield of 85.4%.

Embodiment 2

[0020] Add phenyl phosphorus dichloride (8.950g, 0.05mol) and 50ml of 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 , Dissolving p-phenylenediamine (5.407g, 0.05mol) in 50ml of dichloromethane was added to a constant pressure funnel. Under nitrogen protection and stirring, the p-phenylenediamine 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 dichloromethane, and vacuum-dried at 100° C. for 5 hours to obtain 8.73 g of a lavender solid, with a yield of 81.5%.

Embodiment 3

[0022] Add phenylphosphorus dichloride (26.85g, 0.15mol) 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. p-Phenylenediamine (16.22g, 0.15mol) was dissolved in 100ml of chloroform and added to the constant pressure funnel. Under nitrogen protection and stirring, the p-phenylenediamine 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 200ml of chloroform, and dried in vacuum at 100°C for 5 hours to obtain 25.83g of lavender solid, with a yield of 80.4%.

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Abstract

A preparation method of a phosphorus-nitrogen intumescent flame retardant relates to a preparation method of a flame retardant, and the method comprises the following procedures: respectively dissolving raw materials of dichlorophenylphosphine and p-phenylenediamine in solvents, introducing inert gas, stirring, slowly and dropwisely adding the p-phenylenediamine 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 purple powdery phosphorus-nitrogen intumescent 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 phosphorus-nitrogen expansion type flame retardant. Background technique [0002] With the development of material science and engineering, various new polymers and their composite materials are gradually replacing traditional materials with their excellent comprehensive properties, and are widely used in various fields of social production and life. However, while polymer materials bring great convenience to people's lives, their flammability also brings potential fire safety problems. Most polymers and their composite materials will release a large amount of heat in a fire, producing smoke and toxic and corrosive gases, causing secondary hazards. Therefore, the flame retardant treatment of the polymer makes it difficult to catch fire or has self-extinguishing property, which can effectively reduce the occurrence and spread of fire. [000...

Claims

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Application Information

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IPC IPC(8): C08G79/02C07F9/50C08L101/00C08L85/02C08K5/5399
Inventor 梁兵曹俊洪晓东王长松宁志高
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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