Preparation method of 4,4'-(Hexafluoroisopropylidene) diphthalic anhydride
A technology of hexafluoroisopropenylene and diphthalic anhydride, which is applied in 4 fields and can solve problems such as high reaction temperature, difficulty in industrial production, and high reaction pressure
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Embodiment 1
[0021] 106g (1mol) of o-xylene, 330g (1.5mol) of 2,2-dichlorohexafluoropropane, AlCl 3 200g and 1300g of 1-butyl-3-methylimidazoline tetrafluoroborate, heated to 85°C for 15 hours, cooled to 20°C and poured into 1500L water, extracted twice with 2000L toluene, dried with anhydrous magnesium sulfate, Filtration, toluene was distilled off, and the crude product was distilled under 2 mmHg vacuum to obtain 150 g of 4,4'-(hexafluoroisopropenylene)di-o-xylene after recrystallization from isopropanol, with a yield of 83%. (Melting point: 78-80°C).
Embodiment 2
[0023] 106g (1mol) of o-xylene, 330g (1.5mol) of 2,2-dichlorohexafluoropropane, ZnCl 2 204g and 1300g of 1-butyl-3-methylimidazoline tetrafluoroborate were heated to 85°C for 15 hours, cooled to 20°C and poured into 1500L of water, extracted twice with 2000L of toluene, dried with anhydrous magnesium sulfate, Filtration, toluene was distilled off, the crude product was distilled under 2 mmHg vacuum and recrystallized from isopropanol to obtain 115 g of 4,4'-(hexafluoroisopropenylene)di-o-xylene, with a yield of 64%. (Melting point: 78-80°C).
Embodiment 3
[0025] 106g (1mol) of o-xylene, 330g (1.5mol) of 2,2-dichlorohexafluoropropane, AlCl 3 200g and 1300g of 1-butyl-3-methylimidazoline hexafluorophosphate, heated to 85°C for 15 hours, cooled to 20°C, poured into 1500L water, extracted twice with 2000L toluene, dried with anhydrous magnesium sulfate, filtered , toluene was distilled off, and the crude product was distilled under 2 mmHg vacuum to obtain 61 g of 4,4'-(hexafluoroisopropenylene) di-o-xylene through recrystallization from isopropanol, with a yield of 34%. (Melting point: 78-80°C).
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