FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing nicotinic acid by direct gas-phase oxidation of 3-picoline with atmospheric oxygen, in which 3-picoline, air, water and recycle gases are fed into a reactor consisting of tubes with a fixed layer of a granular catalyst washed with a coolant. If the recycle fraction is 80–90 % of the total volume of the reaction mixture, concentration of 3-picoline at the reactor inlet is 0.8–1.1 mol%, and the molar ratio of 3-picoline, oxygen and water is 1:/11–21/:/18–26/. Vanadium-titanium oxide catalyst is used, which contains vanadium oxides 5–20 wt%, modifying additives – cerium oxide or one or more metal oxides selected from group IV and period V of periodic table with total content of oxides of modifying elements within 1.2–10.0 wt%, anatase titanium oxides of not less than 60 wt%. Ratio of size of catalyst granules to inner diameter of tube is 1:/5.8–8.4/, and maximum temperature in catalyst layer is 5–20 °C is higher than coolant temperature. After the reactor, the reaction gases are directed to the stage of nicotinic acid release into the solid phase, after which some gases are separated and recycled, and from the other part of reaction gases either unreacted 3-picoline and 3-pyridine carbaldehyde are separated into the liquid phase and returned to the catalytic process of producing nicotinic acid, or another part of the reaction gases is directed to neutralization and then discharged into atmosphere.
EFFECT: increased removal of nicotinic acid from a unit of weight of the catalyst and increased completeness of using initial 3-picoline.
4 cl, 12 ex
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Authors
Dates
2019-10-24—Published
2019-07-24—Filed