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A kind of preparation method of phosphorus and nitrogen synergistic water-soluble polymer flame retardant

A water-soluble polymer and flame retardant technology, applied in the application field of functional polymer materials, can solve the problems of easy phase separation, difficult to dissolve in solvents, easy to migrate, etc., achieve simple production process conditions, and overcome the deterioration of mechanical properties. , Improve the effect of flame retardant performance

Active Publication Date: 2020-03-24
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of these flame retardants are inorganic and organic small molecules. When used in the flame retardancy of polymer materials, they are prone to poor compatibility, resulting in decreased mechanical properties, thermal stability, and exudation. sexual issues
Therefore, the current flame retardants are also developing towards polymers to solve the problems of poor compatibility between small molecule flame retardants and polymer materials, easy migration, and affecting the mechanical properties and mechanical strength of materials.
On the other hand, polymer intumescent flame retardants are generally difficult to dissolve in solvents, and are prone to phase separation when added to polymer materials, resulting in uneven distribution of flame retardant properties

Method used

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  • A kind of preparation method of phosphorus and nitrogen synergistic water-soluble polymer flame retardant
  • A kind of preparation method of phosphorus and nitrogen synergistic water-soluble polymer flame retardant
  • A kind of preparation method of phosphorus and nitrogen synergistic water-soluble polymer flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) First, 10.4 g of neopentyl glycol and 9.3 mL of phosphorus oxychloride were dissolved in 1,2-dichloroethane, refluxed at 85° C. for 10 hours, rotary evaporated, and dried to obtain white phosphorus-containing intermediate 5, 5-Dimethyl-2-chloro-1,3,2-dioxaphosphocaprolactoyl phosphate;

[0022] (2) Afterwards, 18.5g of 5,5-dimethyl-2-chloro-1,3,2-dioxaphosphacaprolactoyl phosphate obtained in step (1) was dissolved in 9.7g of potassium thiocyanate In acetone solution, reflux at 60°C for 4 hours, remove potassium chloride by filtration, and obtain 5,5-dimethyl-2-isothiocyanato-1,3,2-dioxaphosphacaprolactoyl phosphate filtrate ;

[0023] (3) 5,5-dimethyl-2-isothiocyanate-1,3,2-dioxaphosphacaprolactoyl phosphate filtrate that step (2) obtains adds 10 g molecular weight again and is 600Da large Molecular nitrogen-containing intermediate polyethyleneimine, reacted for 6 hours, suction filtered, and dried to obtain a yellow-brown powdery phosphorus-nitrogen synergistic ...

Embodiment 2

[0025] (1) First, dissolve 10.4g of neopentyl glycol and 18.6mL of phosphorus oxychloride in dichloromethane, reflux at 85°C for 8 hours, rotary steam and dry to obtain the white phosphorus-containing intermediate 5,5-dimethyl -2-Chloro-1,3,2-dioxaphosphacaprolactoyl phosphate;

[0026] (2) Afterwards, 18.5g of 5,5-dimethyl-2-chloro-1,3,2-dioxaphosphacaprolactoyl phosphate obtained in step (1) was dissolved in 9.7g of potassium thiocyanate In 1,2-dichloroethane solution, reflux at 60°C for 6 hours, remove potassium chloride by filtration, and obtain 5,5-dimethyl-2-isothiocyanato-1,3,2-phosphorus dioxide Heterocaprolactoyl phosphate filtrate;

[0027] (3) 5,5-dimethyl-2-isothiocyanate-1,3,2-dioxaphosphacaprolactoyl phosphate filtrate that step (2) obtains adds 15g molecular weight again and is 1800Da macromolecule The nitrogen-containing intermediate, polyethyleneimine, was reacted for 10 hours, suction filtered, and dried to obtain a yellowish-brown powdery phosphorus-nitrog...

Embodiment 3

[0029] (1) First, dissolve 10.4g of neopentyl glycol and 37.2mL of phosphorus oxychloride in acetone, reflux at 85°C for 6 hours, rotary steam and dry to obtain the white phosphorus-containing intermediate 5,5-dimethyl-2 - Chloro-1,3,2-dioxaphosphacaprolactoyl phosphate;

[0030] (2) Afterwards, 18.5g of 5,5-dimethyl-2-chloro-1,3,2-dioxaphosphacaprolactoyl phosphate obtained in step (1) was dissolved in 9.7g of potassium thiocyanate In 1,2-dichloroethane solution, reflux at 60°C for 8 hours, remove potassium chloride by filtration, and obtain 5,5-dimethyl-2-isothiocyanato-1,3,2-phosphorus dioxide Heterocaprolactoyl phosphate filtrate;

[0031] (3) 5,5-dimethyl-2-isothiocyanate-1,3,2-dioxaphosphacaprolactoyl phosphate filtrate that step (2) obtains adds 18g molecular weight again and is 25000Da macromolecule The nitrogen-containing intermediate, polyethyleneimine, was reacted for 12 hours, suction filtered, and dried to obtain a yellow-brown powdery phosphorus-nitrogen synerg...

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Abstract

The invention belongs to the field of applications of functional polymer materials and particularly relates to a preparation method of a phosphorous and nitrogen synergistic type water-soluble polymer flame retardant. According to the method, a phosphorous-containing intermediate is prepared from raw materials including neopentyl glycol and phosphorous oxychloride and then activated with potassium thiocyanate, the activated phosphorous-containing intermediate reacts with macromolecular nitrogen-containing intermediate polyethyleneimine, and the tawny powdery phosphorous and nitrogen synergistic type polymer flame retardant is obtained. The flame retardant is water-soluble and can be well compatible with a polymer material, the molecular weight is adjustable as required, and the flame retardance of the material can be improved. The flame retardant can effectively solve the problem that common phosphorous and nitrogen synergistic type flame retardants are insoluble in water, can be effectively dispersed when applied to preparation of water foam polyurethane materials and the like and cannot migrate and separate out of the materials and the problem of the poor mechanical performance of the materials is solved. The production technology condition is convenient, and the product is high in purity and convenient to use.

Description

technical field [0001] The invention relates to a preparation method of a phosphorus-nitrogen synergistic water-soluble polymer flame retardant. It belongs to the application field of functional polymer materials. Background technique [0002] With the application of polymer materials in various fields such as chemical industry, construction, aviation, automobiles, electrical appliances, etc., especially the increase in the application of foam materials with good thermal insulation, heat insulation, and sound insulation functions, the problem of its flammability has become a problem for people. The focus of the research. At present, polymer materials such as polyurethane and polyethylene are widely used, which contain a large number of flammable hydrocarbon segments and have a low limiting oxygen index. Especially after being prepared as a foam material, the specific surface area is increased, the density is small, and it has high air circulation. Not only is it extremely ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/02C08G73/04C08L75/04C08L79/02C08G18/48C08G18/64
CPCC08G18/4081C08G18/48C08G18/6423C08G73/0206C08L75/08C08L2201/02C08L79/02
Inventor 陈荆晓董晓红贾正仁
Owner JIANGNAN UNIV
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