Buckling flame retardant containing phosphor-nitrogen macromolecule and preparation method thereof
An intumescent flame retardant and macromolecular technology, applied in fire-resistant coatings and other directions, can solve the problems of easy migration or precipitation, loss of flame retardant performance, small molecular weight, etc., and achieve good application prospects, easy control, and simple preparation methods. Effect
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[0025] Example 1
[0026] Under the protection of nitrogen, 59.4g 2,6,7-trioxo-1-phosphabicyclo-[2,2,2]-octane-1-methoxydichlorophosphate was dissolved in 100ml acetonitrile In a 250ml three-necked flask, heating while stirring. When the dissolution is complete, start to add 40g 4,4'-diaminodiphenylmethane in acetonitrile solution. After the addition is complete, start to add 15ml catalyst pyridine dropwise at 80℃. During the reaction, light yellow powder was continuously formed, reacted for 5 hours, filtered, washed twice with deionized water, and washed twice with absolute ethanol. It was dried in a vacuum oven at 80°C for 12 hours to obtain a pale yellow powder solid with a yield of 85%. Melting point 255-258°C, elemental analysis: C%: 48.1%, H%: 5.0%, N%: 4.83%, O%: 25.8%, P%: 16.27%. The NMR spectrum is shown in Figure 1. The result proves that the compound synthesized by the preparation method of the present invention is basically consistent with the designed phosphorous and...
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[0029] Example 2
[0030] Under the protection of nitrogen, 29.7g 2,6,7-trioxo-1-phosphabicyclo-[2,2,2]-octane-1-methoxydichlorophosphate was dissolved in 80ml acetonitrile In a 250ml three-necked flask, heating while stirring. When the dissolution is complete, start to add 20g 4,4'-diaminodiphenylmethane in acetonitrile solution. After the addition is complete, start to add 10ml catalyst pyridine dropwise at 80℃ During the reaction, light yellow powder was continuously formed. After 2 hours of reaction, it was filtered. The filter cake was washed twice with deionized water and then washed twice with absolute ethanol. It was dried in a vacuum oven at 80°C for 12 hours to obtain a pale yellow powder solid with a yield of 75%. Melting point 255-257°C, elemental analysis: C%: 46.2%, H%: 4.8%, N%: 5.85%, O%: 25.9%, P%: 17.25%.
Example Embodiment
[0031] Example 3
[0032] Under the protection of nitrogen, 59.4g 2,6,7-trioxo-1-phosphabicyclo-[2,2,2]-octane-1-methoxydichlorophosphate was dissolved in 120ml acetonitrile In a 250ml three-necked flask, heat it while stirring. When the dissolution is complete, start to add 42g 4,4'-diaminodiphenylsulfone in acetonitrile solution. After the addition is complete, start to add 20ml catalyst pyridine dropwise at 80℃ During the reaction, light yellow powder was continuously formed, reacted for 4 hours, filtered, washed twice with deionized water, and washed twice with absolute ethanol. It was dried in a vacuum oven at 80°C for 12 hours to obtain a pale yellow powder solid with a yield of 78%. Melting point 256-258°C, elemental analysis: C%: 43.6%, H%: 4.1%, N%: 5.23%, O%: 26.9%, P%: 16.77%, S%: 3.4%.
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