Method of comprehensively use of chloronitrobenzene mixture by fluoro-reaction
A technology of monochloronitrobenzene and chloronitrobenzene, applied in the field of comprehensive utilization of o-, m- and p-chloronitrobenzene mixtures, can solve problems such as many steps, resources cannot be well utilized, etc., and achieves simple operation. Effect
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Embodiment 1
[0019] Add 158 grams (1 mole) of a chloronitrobenzene mixture, 15.8 grams of catalyst tetrabutylammonium bromide, and 157 grams (2.7 moles) of anhydrous potassium fluoride into the reaction flask, heat to 200 ° C, react for 5 hours, and filter Solids such as potassium chloride were removed, and 63.5 grams of p-fluoronitrobenzene and 12.7 grams of o-fluoronitrobenzene were separated through rectification in a rectification tower, with a total yield of 90%. The residue was recrystallized from toluene to obtain 60 g of m-chloronitrobenzene with a recovery rate of 95% and a purity of ≥99.5%.
Embodiment 2
[0021] Add 158 grams (1 mole) of a chloronitrobenzene mixture, 1.58 grams of catalyst tetrabutylammonium bromide, and 157 grams (2.7 moles) of anhydrous potassium fluoride into the reaction flask, heat to 150 ° C, react for 15 hours, and filter Solids such as potassium chloride were removed, and 65 grams of p-fluoronitrobenzene and 13 grams of o-fluoronitrobenzene were separated through rectification in a rectification tower, with a total yield of 92%. The residue was recrystallized from toluene to obtain 60 g of m-chloronitrobenzene with a recovery rate of 95% and a purity of ≥99.5%.
Embodiment 3
[0023] Add 158 grams (1 mole) of a chloronitrobenzene mixture, 158 grams of catalyst calix[6]arene, and 476 grams (8.2 moles) of anhydrous potassium fluoride into the reaction flask, heat to 150°C, react for 5 hours, and remove by filtration Potassium chloride and other solids were rectified by a rectification tower to separate 67 grams of p-fluoronitrobenzene and 13.4 grams of o-fluoronitrobenzene, with a total yield of 95%. The residue was recrystallized from toluene to obtain 60 g of m-chloronitrobenzene with a recovery rate of 95% and a purity of ≥99.5%.
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