Method for preparing 2,6-dichloropyridine by pyridine liquid-phase photochlorination
A technology of dichloropyridine and pyridine chloride solution, applied in the directions of organic chemical methods, chemical instruments and methods, separation methods, etc., can solve the problems of large amount of three wastes, blockage of tail gas pipelines, etc., and achieve the effect of low cost and low energy consumption
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Embodiment 1
[0012] Example 1: A method for preparing 2,6-dichloropyridine by liquid-phase photochlorination of pyridine, using pyridine and chlorine as starting materials, using trifluoromethyl chlorobenzene as solvent, at a temperature of 150°C to 210°C and Under the irradiation of ultraviolet light, the chlorination reaction of pyridine and chlorine is carried out continuously, and the pyridine chlorination liquid obtained by cooling the chlorination reaction product and the solvent is:
[0013] Using pyridine and chlorine gas as starting materials, trifluoromethyl chlorobenzene as solvent, continuous feed in the temperature range of 150°C to 210°C under the irradiation of ultraviolet light for liquid phase chlorination reaction, the obtained pyridine chlorination liquid .
[0014] In this embodiment, the weight ratio of pyridine to solvent is 1:0.2-4. At the beginning of the chlorination reaction, a certain amount of solvent is pre-added in the reaction chlorination reactor, heated to...
Embodiment 2
[0017] Embodiment 2: On the basis of Example 1, using pyridine and chlorine as starting materials, taking trifluoromethyl chlorobenzene after heating as solvent, pyridine and chlorine are made under the irradiation of 150 ℃ ~ 210 ℃ temperature and ultraviolet light The chlorination reaction is carried out continuously, and the chlorination reaction product and the solvent are cooled to obtain a pyridine chloride solution. After the chlorination solution is roughly steamed, tar and high boilers are separated, and the distillate is pyridine chloride containing a solvent.
[0018] Preparation of 2,6-dichloropyridine by liquid-phase photochlorination of pyridine (coarsely steamed material) test data
[0019] Reaction temperature °C
Embodiment 3
[0020] Embodiment 3: On the basis of Examples 1 and 2, using pyridine and chlorine as starting raw materials, taking trifluoromethyl chlorobenzene as solvent, pyridine and chlorine are made under the irradiation of 150 ℃ ~ 210 ℃ temperature and ultraviolet light The chlorination reaction is carried out continuously, the pyridine chlorination liquid obtained by cooling the chlorination reaction product and the solvent, the chlorination liquid is subjected to rough steaming, and the tar and high boiling matter are separated, and the distillate obtained is the pyridine chloride containing the solvent. After deducting the solvent, the pyridine The 2,6-dichloropyridine content in the chloride is ≥65%, and the pyridine chloride containing the solvent is purified by rectification to obtain a 2,6-dichloropyridine product with a purity ≥99.0%.
[0021] Experimental test data of preparation of 2,6-dichloropyridine (distillation separation) by liquid-phase photochlorination of pyridine
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