Method for treating fluorine ions in m-aminotrifluorotoluene
A technology of m-aminobenzotrifluoride and aminobenzotrifluoride, which is applied in the field of treatment of fluoride ions in m-aminobenzotrifluoride, can solve the problems of difficulty in popularization and application, limited application range, high processing cost, etc., and achieves remarkable economic benefits, The effect of a wide range of sources and a simple process
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Embodiment 1
[0019] In the first step, a crude product of m-aminobenzotrifluoride is synthesized by using trifluorotoluene as a raw material, nitrated with mixed acid, and catalytic hydrogenation reduction under normal pressure, and the crude product contains more than 10 ppm of fluoride ions.
[0020] In the second step, 1600 kg of crude m-aminotrifluorotoluene and 1.6 kg of lime essence (the main component of calcium oxide CaO) were mixed and stirred in proportion. The stirring rate was 100 rpm, and the stirring reaction was carried out at 40 ° C for 3 hours. Fluorine The ions combine with the calcium ions of calcium oxide to form calcium fluoride (CaF 2 ), the precipitate was removed by filtration, and the obtained m-aminobenzotrifluoride had a fluoride ion content of ≤10 ppm; the same method was repeated once, and the fluoride ion content was ≤5 ppm; finally, the m-aminobenzotrifluoride was dried , you can get refined m-aminotrifluorotoluene, the yield ≥ 99.9%.
Embodiment 2
[0022] First, synthesize the crude product of m-aminobenzotrifluoride according to the first step method in Example 1, then mix and stir 1600 kg of the crude product of m-aminobenzotrifluoride with 9.6 kg of lime essence (the main component calcium oxide CaO) in proportion, and the stirring rate is 30 rev / min, stirring and reacting at 20°C for 6 hours, the fluoride ions will combine with the calcium ions of calcium oxide to form calcium fluoride (CaF 2 ), the precipitate was removed by filtration, and the obtained m-aminobenzotrifluoride had a fluoride ion content of ≤5 ppm; the same method was repeated once, and the fluoride ion content was ≤1 ppm; finally, the fluoride-removed m-aminobenzotrifluoride was dried , you can get refined m-aminotrifluorotoluene, the yield ≥ 99.9%.
Embodiment 3
[0024] First synthesize the crude product of m-aminobenzotrifluoride according to the first step method in Example 1, then mix and stir 1600 kg of the crude product of m-aminobenzotrifluoride with 2.5 kg of lime essence (the main component calcium oxide CaO) in proportion, and the stirring rate is 75 Turn / min, stirring reaction at 30 ℃ for 5.5 hours, fluoride ions and calcium ions of calcium oxide will combine to form calcium fluoride (CaF 2 ), the precipitate was removed by filtration, and the obtained m-aminobenzotrifluoride had a fluoride ion content of ≤8 ppm; the same method was repeated once, and the fluoride ion content was ≤3 ppm; finally, the m-aminobenzotrifluoride was dried , you can get refined m-aminotrifluorotoluene, the yield ≥ 99.9%.
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