Synthesis process and application of hydroxyl-terminated hyperbranched polyphosphazene flame retardant

A technology of hydroxyl-terminated hyperbranching and polyphosphazene, which is applied in the direction of polyurea/polyurethane coatings, coatings, fireproof coatings, etc. To achieve the effects of enhancing thermal stability and heat resistance, inhibiting the reaction process, and enhancing flame retardancy

Inactive Publication Date: 2022-04-29
雷红军
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Polyurethane water-based coatings are environmentally friendly, less polluting, and have excellent elasticity of the paint film. They are paints and coatings with great development potential. However, traditional polyurethane coatings have poor flame retardancy and heat resistance. Adding additive flame retardancy will cause Affect the performance and mechanical strength of polyurethane paint film, CN102585135B "Reactive Intumescent Flame Retardant for Polyurethane and Its Synthetic Method", reports the synthesis of a new type of intumescent flame retardant containing active group hydroxyl, and polyurethane system Good compatibility, it is a reactive flame retardant that can react with isocyanate. The reactive flame retardant can participate in the polymerization reaction of the polymer, so that the polymer material itself has a flame retardant component, and has a good flame retardant effect , has the advantage of having less impact on the performance of the material

Method used

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  • Synthesis process and application of hydroxyl-terminated hyperbranched polyphosphazene flame retardant
  • Synthesis process and application of hydroxyl-terminated hyperbranched polyphosphazene flame retardant
  • Synthesis process and application of hydroxyl-terminated hyperbranched polyphosphazene flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Add 0.2 g of carboxycyclotriphosphazene to 5 mL of SOCl 2 , pass into N 2 Exhaust the air, heat to 60°C, react for 5 hours, and distill under reduced pressure after the reaction, wash the product with dichloromethane and acetone to obtain cyclotriphosphazene acid chloride.

[0030] (2) Add 0.5% of acid chloride cyclotriphosphazene into xylene solvent, stir to dissolve and then pass into N 2 Exhaust air, add 0.83g dihydroxy DOPO derivative (C 17 h 20 NO 4 P), and 0.08g of catalyst pyridine was added dropwise, heated to 70°C, reacted for 36h, cooled after the reaction, and distilled under reduced pressure, and the product was sequentially extracted by tetrahydrofuran, dichloromethane and acetone to obtain a hydroxyl-terminated hyperbranched polyphosphazene flame retardant.

[0031] (3) The diisocyanate monomer of 3g is mixed with the polyether polyol of 5g, and the dibutyltin dilaurate of 0.1g is added dropwise, in N 2 React at 70°C for 2 hours in the atmosphere...

Embodiment 2

[0033] (1) Add 0.2 g of carboxycyclotriphosphazene to 10 mL of SOCl 2 , pass into N 2 Exhaust the air, heat to 70°C, react for 5h, distill under reduced pressure after reaction, wash the product with dichloromethane and acetone, and obtain cyclotriphosphazene acid chloride.

[0034] (2) Add 0.5% of acid chloride cyclotriphosphazene into acetonitrile solvent, stir to dissolve and then pass into N 2 Exhaust air, add 0.9g dihydroxy DOPO derivative (C 17 h 20 NO 4 P), and 0.1g of catalyst pyridine was added dropwise, heated to 85°C, reacted for 36h, cooled after the reaction, and distilled under reduced pressure, and the product was sequentially extracted by tetrahydrofuran, dichloromethane and acetone to obtain a hydroxyl-terminated hyperbranched polyphosphazene flame retardant.

[0035] (3) The diisocyanate monomer of 3.3g is mixed with the polyether polyol of 5g, and the dibutyltin dilaurate of 0.15g is added dropwise, in N 2 React at 70°C in the atmosphere for 2.5h to ob...

Embodiment 3

[0037] (1) Add 0.2 g of carboxycyclotriphosphazene to 15 mL of SOCl 2 , pass into N 2 Exhaust the air, heat to 70°C, react for 8 hours, distill under reduced pressure after the reaction, wash the product with dichloromethane and acetone, and obtain the acid chloride cyclotriphosphazene.

[0038] (2) Add 0.5% of acid chloride cyclotriphosphazene to 1,4 dioxane solvent, stir to dissolve and then pass into N 2 Exhaust the air, add 1 g dihydroxy DOPO derivative (C 17 h 20 NO 4 P), and 0.12g of catalyst pyridine was added dropwise, heated to 80°C, reacted for 48h, cooled after the reaction, and distilled under reduced pressure, and the product was sequentially extracted by tetrahydrofuran, dichloromethane and acetone to obtain a hydroxyl-terminated hyperbranched polyphosphazene flame retardant.

[0039] (3) The diisocyanate monomer of 3.5g is mixed with the polyether polyol of 5g, and the dibutyltin dilaurate of 0.2g is added dropwise, in N 2 React in the atmosphere at 75°C for...

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Abstract

The invention relates to the technical field of flame retardance of coatings, discloses a hydroxyl-terminated hyperbranched polyphosphazene flame retardant, and synthesizes a novel nitrogen and phosphorus-containing hydroxyl-terminated hyperbranched polyphosphazene flame retardant with a three-dimensional network structure as a chain extender and a reactive flame retardant of polyurethane. A hyperbranched polyphosphazene flame retardant is added into a polyurethane prepolymer, a terminal hydroxyl group of the hyperbranched polyphosphazene flame retardant participates in a chain extension reaction of the polyurethane prepolymer, so that a polyurethane molecular chain is polymerized and cross-linked through the hyperbranched polyphosphazene flame retardant to obtain flame-retardant polyurethane, the influence on the use performance and the mechanical property of the polyurethane is smaller, and the hyperbranched polyphosphazene flame retardant serving as a halogen-free nitrogen-phosphorus flame retardant has a good flame retardant property. The carbon forming property and carbon residue rate of a polyurethane paint film are greatly improved, the thermal stability and heat resistance of the polyurethane paint film are enhanced, the polyurethane paint film can become phosphoric acid derivatives and nitrogen-containing non-combustible gas during high-temperature combustion, and the flame retardance of the polyurethane paint is enhanced.

Description

technical field [0001] The invention relates to the technical field of flame retardant coatings, in particular to a synthesis process and application of a hydroxyl-terminated hyperbranched polyphosphazene flame retardant. Background technique [0002] Paints and coatings can improve the anti-corrosion, anti-pollution and waterproof properties of the substrate. They are widely used polymer materials, such as polyurethane coatings and acrylic resin coatings. They play an important role in the fields of automobile manufacturing, electronic appliances, and furniture decoration. Uses, the development of new paints and coatings, such as flame-retardant coatings, heat-resistant coatings, etc., has become a research hotspot. Adding flame retardants to the coating matrix is ​​an effective method to enhance the flame retardancy of coatings. [0003] Polyurethane water-based coatings are environmentally friendly, less polluting, and have excellent elasticity of the paint film. They are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/025C08G18/64C09D5/18C09D175/08
CPCC08G79/025C08G18/6461C09D175/08C09D5/18
Inventor 雷红军
Owner 雷红军
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