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Nitrogen-phosphorus expanded type flame retardant and preparation method for application in aqueous polyurethane coating

A nitrogen-phosphorus intumescent, water-based polyurethane technology is used in the preparation of nitrogen-phosphorus intumescent flame retardants, and in the field of nitrogen-phosphorus intumescent flame retardants in the preparation of water-based polyurethane coatings, which can solve the problem of poor compatibility, easy to produce molten droplets, and flames. The problem of high smoke density during burning time can improve the flame retardancy, maintain the original properties, and improve the flame retardancy.

Active Publication Date: 2019-10-18
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its main disadvantage is that its mechanical properties are reduced. This is because its flame retardant is compounded, that is, the inorganic material containing ammonium polyphosphate is mixed with the organic material polyacrylic acid, which is easy to cause poor compatibility. Composite, suitable for melt mixing of polypropylene, not suitable for water-based reaction
Its main disadvantage is that the flame burning time and smoke density of the obtained polyurethane are relatively large, which can easily cause safety hazards
[0013] To sum up, the flame retardancy of water-based polyurethane coatings is poor at present, and the flame burning time and smoke density of existing researches are relatively large. However, as a plastic body, polyurethane is prone to produce molten droplets during combustion, causing secondary hazards.

Method used

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  • Nitrogen-phosphorus expanded type flame retardant and preparation method for application in aqueous polyurethane coating
  • Nitrogen-phosphorus expanded type flame retardant and preparation method for application in aqueous polyurethane coating
  • Nitrogen-phosphorus expanded type flame retardant and preparation method for application in aqueous polyurethane coating

Examples

Experimental program
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Effect test

example 1

[0038] (1) Preparation of nitrogen-phosphorus intumescent flame retardant: add 1 mol of dimethyl phosphite to 1 / 10 weight of the basic catalyst sodium methoxide, then add 0.9 mol of acrylamide, and the reaction temperature is 70 React at ℃ for 3 hours to obtain 3-dimethoxyphosphorylpropionamide, which is intermediate A. Lower the temperature of the intermediate product to 50℃, add 0.9mol of trimethylchlorosilane and 0.1mol of potassium sodium tartrate, and stir at 60℃ React for 2 hours, adjust the pH of the solution with sodium hydroxide during the stirring process to stabilize the pH of the solution at 6.5-7.0, then add 3.1 g of 2,4-dihydroxybenzophenone and 0.2 g of 1,3,5-triazine, Stir and react at 60°C for 2 hours, concentrate until the solid content reaches 90% (not more than 92%), and obtain the nitrogen-phosphorus intumescent flame retardant.

[0039] (2), in the there-necked flask of 500ml that stirring paddle, thermometer, condenser tube are housed, adding molecular w...

example 2

[0043] (1) Preparation of nitrogen-phosphorous intumescent flame retardant: add 1 mol of dimethyl phosphite to 1 / 10 weight of the basic catalyst sodium methoxide, then add 1.2 mol of acrylamide, and the reaction temperature is 90 React at ℃ for 5 hours to obtain 3-dimethoxyphosphorylpropionamide, which is intermediate A. Lower the temperature of the intermediate product to 55℃, add 1.3mol of cyanuric chloride and 0.1mol of sodium nitrilotriacetate, and stir at 80℃ React for 5 hours, adjust the pH of the solution with sodium hydroxide during stirring to stabilize the pH of the solution at 6.5-7.0, then add 8.7 g of itaconic anhydride and 0.4 g of indole-3-acetamide, and stir for 5 hours at 80°C. Concentrate until the solid content reaches 90% (not more than 92%) to obtain the nitrogen-phosphorus intumescent flame retardant.

[0044] (2) In a 500ml three-neck flask equipped with a stirring paddle, a thermometer, and a condenser, add 45g of hexanediol, 24.8g of hexamethylene diis...

example 3

[0047] (1) Preparation of nitrogen-phosphorous intumescent flame retardant: add 1 mol of dimethyl phosphite to 1 / 10 weight of the basic catalyst sodium methoxide, then add 1.05 mol of acrylamide, and the reaction temperature is 80 React at ℃ for 4 hours to obtain 3-dimethoxyphosphorylpropionamide, which is intermediate A. Lower the temperature of the intermediate product to 50℃, add 1.1mol of trimethylolpropane and 0.1mol of p-nitrobenzoic acid, and heat at 70℃ The reaction was stirred for 3.5 hours. During the stirring process, the pH of the solution was adjusted with sodium hydroxide to stabilize the pH of the solution at 6.5-7.0, and then 5.9 g of citraconic acid and 0.3 g of dimethyl 1,4-cyclohexanedicarboxylate were added. Stir and react at 70°C for 3.5 hours, concentrate until the solid content reaches 90% (not more than 92%), and obtain the nitrogen-phosphorus intumescent flame retardant.

[0048] (2) In a 500ml three-neck flask equipped with a stirring paddle, a thermo...

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Abstract

The invention relates to preparation of a nitrogen-phosphorus expanded type flame retardant and a method for application in preparing an aqueous polyurethane coating. The method comprises the following steps: mixing dimethyl phosphate, and alkali catalysts, namely sodium methoxide and acrylamide, performing a reaction so as to obtain an intermediate, adding a charcoal formation agent and a substance A, keeping the pH value of the solution to 6.5-7.0 in the stirring process, further adding a substance B and a substance C, performing a continuous stirring reaction, and performing concentration so as to obtain the nitrogen-phosphorus expanded type flame retardant; and preparing the aqueous polyurethane coating from the nitrogen-phosphorus expanded type flame retardant. By adopting the flame retardant provided by the invention, flame can be rapidly choked, and the flame retardancy of the nitrogen-phosphorus expanded type flame retardant can be improved by releasing smoke, controlling flamecombustion time and controlling densities of charcoal layers. In addition, the nitrogen-phosphorus expanded type flame retardant is grafted with polyurethane, so that the flame retardancy of the polyurethane can be further improved.

Description

technical field [0001] The present invention relates to the preparation method of flame retardant and waterborne polyurethane coating, particularly relate to the preparation method of nitrogen-phosphorus expansion type flame retardant and the method for utilizing nitrogen phosphorus expansion type flame retardant to prepare waterborne polyurethane coating. Background technique [0002] Flame retardants are mainly used in fields such as plastics, rubber, textiles and coatings. Flame retardants mainly include hundreds of varieties such as halogen flame retardants, phosphorus flame retardants, and inorganic flame retardants. Halogen flame retardants have the advantage of high cost performance, but release a large amount of toxic or corrosive gases such as HX during combustion. At the same time, some halogen flame retardants have carcinogenic effects on humans, such as pentabromodiphenyl ether and octabromodiphenyl ether. [0003] Common inorganic flame retardants are magnesia...

Claims

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Application Information

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IPC IPC(8): C09D5/18C09D175/04C08G18/10C08G18/32C08G18/38C08G18/44C08G18/66C08G18/34C07F9/48C07K1/14C07K1/30
CPCC07F9/4883C07K1/30C09D5/185C09D175/04
Inventor 段宝荣王全杰王琦研仇同济
Owner YANTAI UNIV
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