Purification method of 4, 4 '-dinitrodiphenyl ether
A technology of dinitrodiphenyl ether and purification method, which is applied in the field of purification of 4,4′-dinitrodiphenyl ether, can solve the problems of complicated and complicated purification methods, and achieves environmental friendliness, low energy consumption, and low VOC. Effect
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[0036] In the present invention, the 4,4'-dinitrodiphenyl ether crude product is preferably self-made, and the preparation method of the 4,4'-dinitrodiphenyl ether crude product preferably includes the following steps: Phenylbenzene, sodium p-nitrophenolate, nitrobenzene and a catalyst are mixed for an etherification reaction to obtain a crude product of 4,4'-dinitrodiphenyl ether. In the present invention, the molar ratio of nitrochlorobenzene to sodium p-nitrophenolate is preferably 1:0.94-1, more preferably 1:0.96-0.98. In the present invention, the catalyst preferably includes a potassium salt catalyst and / or a sodium salt catalyst, the potassium salt catalyst preferably includes potassium chloride and / or potassium carbonate, and the sodium salt catalyst preferably includes sodium chloride and / or carbonic acid Sodium; the mass ratio of the nitrochlorobenzene to the catalyst is preferably 1:0.07-0.15, more preferably 1:0.08-0.12. In the present invention, the ratio of the ...
Embodiment 1
[0050] Under stirring conditions, add 600kg of crude 4,4'-dinitrodiphenyl ether (purity: 98.95%), 1800kg of pure water and 1.8kg of carbon aerogel into a 3000L glass-lined reactor for mixing, and heat up to 155°C Then heat-preserve and absorb for 0.5h, and filter while hot to obtain the liquid component; add 180g of 3,3′,4,4′-diphenyl ether tetracarboxylic acid to the liquid component and extract at 155°C for 0.5h to obtain The extract was cooled at a rate of 0.15°C / min to 120°C for crystallization, centrifuged while hot, and the obtained solid component was washed twice with 85°C hot pure water (300kg of hot water each time), and then heated at 110°C After drying for 3 hours, 4,4'-dinitrodiphenyl ether was obtained (light yellow crystals, 591kg, yield 98.5%, purity 99.93%).
Embodiment 2
[0052] Under stirring conditions, add 600kg of crude 4,4'-dinitrodiphenyl ether (purity 98.95%), 4200kg of pure water and 9kg of carbon aerogel into a 6300L glass-lined reactor for mixing, and heat up to 145°C Insulate and absorb for 1.5h, filter while hot to obtain liquid components; add 1.5kg of 3,3′,4,4′-biphenyl ether tetracarboxylic acid to the liquid components, and then extract at 155°C for 1.5h to obtain The extract solution was cooled to 90°C at a rate of 0.5°C / min to crystallize, centrifuged while hot, and the obtained solid component was washed with hot pure water at 95°C for 2 times (300kg of hot water each time), and then heated at 100°C After drying for 3 hours, the fine product of 4,4'-dinitrodiphenyl ether (light yellow crystals, 594.6kg, yield 99.1%, purity 99.96%) was obtained.
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