Nitrogen-phosphorus intumescent flame retardant and its preparation method for application in waterborne polyurethane coatings

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 for preparing water-based polyurethane coatings, which can solve the problems of poor compatibility, safety hazards, and easy generation of molten droplets. and other problems, to achieve the effect of improving flame retardancy, improving flame retardancy and maintaining original properties

Active Publication Date: 2021-01-08
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. Existing research shows that its flame burning time and smoke density are relatively large. As a plastic body, polyurethane is prone to produce molten droplets during combustion, causing secondary hazards.

Method used

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  • Nitrogen-phosphorus intumescent flame retardant and its preparation method for application in waterborne polyurethane coatings
  • Nitrogen-phosphorus intumescent flame retardant and its preparation method for application in waterborne polyurethane coatings
  • Nitrogen-phosphorus intumescent flame retardant and its preparation method for application in waterborne polyurethane coatings

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, add alkaline catalyst sodium methoxide to 1 / 10 of the weight of dimethyl phosphite, then add 0.9 mol of acrylamide, the reaction temperature is 70 React at ℃ for 3 hours to obtain 3-dimethoxyphosphoryl propionamide, which is intermediate A. Lower the temperature of the intermediate product to 50℃, add 0.9 mol of trimethylchlorosilane and 0.1 mol of potassium sodium tartrate, and stir at 60℃. React for 2h, 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 3.1g of 2,4-dihydroxybenzophenone and 0.2g of 1,3,5-triazine, Stir the reaction at 60°C for 2 hours, and concentrate until the solid content reaches 90% (not exceeding 92%) to obtain the nitrogen-phosphorus intumescent flame retardant.

[0039](2) In a 500ml three-necked flask equipped with a stirring blade, a thermometer and a condenser, add 45...

example 2

[0043](1) Preparation of nitrogen-phosphorus intumescent flame retardant: add 1 mol of dimethyl phosphite, add alkaline catalyst sodium methoxide to 1 / 10 of the weight of dimethyl phosphite, then add 1.2 mol of acrylamide, reaction temperature 90 React at ℃ for 5 hours to obtain 3-dimethoxyphosphoryl propionamide, which is intermediate A. Lower the temperature of the intermediate product to 55℃, add 1.3 mol of cyanuric chloride and 0.1 mol of sodium nitrilotriacetate, and stir at 80℃ React for 5h, 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 8.7g of itaconic anhydride and 0.4g of indole-3-acetamide, stir and react at 80℃ for 5h, It is concentrated to a solid content of 90% (not exceeding 92%) to obtain the nitrogen-phosphorus intumescent flame retardant.

[0044](2) In a 500ml three-necked flask equipped with a stirring blade, a thermometer and a condenser, add 45g of hexanediol, 24.8g of hexame...

example 3

[0047](1) Preparation of nitrogen-phosphorus intumescent flame retardant: add 1 mol of dimethyl phosphite, add alkaline catalyst sodium methoxide to 1 / 10 of the weight of dimethyl phosphite, then add 1.05 mol of acrylamide, and the reaction temperature is 80 React at ℃ for 4 hours to obtain 3-dimethoxyphosphoryl propionamide, which is intermediate A. The temperature of the intermediate product is reduced to 50℃, and 1.1 mol of trimethylolpropane and 0.1 mol of p-nitrobenzoic acid are added at 70℃. Stir the reaction for 3.5 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 5.9 g of citraconic acid and 0.3 g of dimethyl 1,4-cyclohexanedicarboxylate, Stir and react for 3.5 hours at 70°C, and concentrate until the solid content reaches 90% (not more than 92%) to obtain the nitrogen-phosphorus intumescent flame retardant.

[0048](2) In a 500ml three-necked flask equipped with a stirring blade, a t...

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Abstract

The invention relates to a method for preparing nitrogen-phosphorus intumescent flame retardant and applying it to the preparation of water-based polyurethane coatings. Dimethyl phosphite, basic catalyst sodium methoxide and acrylamide are mixed and reacted to obtain an intermediate, and carbon-forming agents and substances are added. A. During the stirring process, the pH of the solution is stabilized at 6.5-7.0, then substance B and substance C are added, and the stirring reaction is continued, and the nitrogen-phosphorus intumescent flame retardant is concentrated to obtain a water-based polyurethane coating. The flame retardant prepared by the invention quickly suffocates the flame, and improves the flame retardancy of the nitrogen-phosphorus intumescent flame retardant from the viewpoints of releasing smoke, controlling the burning time of the flame and the compactness of the carbon layer. In addition, the present invention grafts the nitrogen-phosphorus intumescent flame retardant onto the polyurethane, which further improves the flame retardancy of the polyurethane.

Description

Technical field[0001]The invention relates to a method for preparing a flame retardant and a waterborne polyurethane coating, in particular to a method for preparing a nitrogen-phosphorus intumescent flame retardant and a method for preparing a waterborne polyurethane coating by using a nitrogen-phosphorus intumescent flame retardant.Background technique[0002]Flame retardants are mainly used in the fields of 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 the combustion process. 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 magnesium oxide and aluminum oxide. Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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