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 burnin

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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Example Embodiment

[0037] Example one

[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 thermom...

Example Embodiment

[0042] Example two

[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. Reduce 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, and stir for 5h at 80℃. 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 hexa...

Example Embodiment

[0046] Example three

[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 for 4h at ℃ to obtain 3-dimethoxyphosphorylpropionamide, which is intermediate A. The temperature of the intermediate product is lowered to 50℃, and 1.1 mol of trimethylolpropane and 0.1 mol of p-nitrobenzoic acid are added at 70℃. The reaction was stirred for 3.5 hours. During the stirring, 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 1,4-cyclohexanedicarboxylate were added. Stir and react for 3.5 hours at 70°C, and concentrate until the solid content reaches 90% (not exceeding 92%) to obtain the nitrogen-phosphorus intumescent flame retardant.

[0048] (2) In a 500ml three-necked flask equ...

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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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