A kind of preparation method of β-menaquinone

Abstract

The invention discloses a preparation method of β-menadione, comprising the following steps: step 1, dissolving ceric sulfate in a sulfuric acid solution to obtain a ceric sulfate solution, dissolving β-methylnaphthalene in an organic solvent, Obtain the β-methylnaphthalene organic solution; Step 2, add the ceric sulfate solution and the β-methylnaphthalene organic solution into the reaction kettle at the same time, keep the temperature and stir for the reaction, after the reaction, cool down and crystallize, and obtain the finished product β-methylnaphthalene through filtration Menadione; step 3, separating the cerium sulfate solution and the organic solvent in the liquid phase obtained by filtration, recycling the organic solution after distillation and recycling, and recycling the cerium sulfate solution after electrolytic oxidation of the diaphragm. The preparation method of β-menadione of the present invention completely replaces the oxidation of chromium, so that the product does not contain hexavalent chromium, and β-methylnaphthalene is dissolved in the organic phase for reaction. The material contact area is larger, and the reaction rate is faster. β ‑ Menadione will not peroxidize and the product is of high purity.

Description

technical field [0001] The invention belongs to the technical field of preparation of organic compounds, and relates to a preparation method of β-menadione. Background technique [0002] β-menadione, bright yellow crystal, has a very slightly pungent smell. Stable in air and decomposed in sunlight. 1g β-menadione is dissolved in about 60ml ethanol, 10ml benzene, 50ml vegetable oil, dissolved in chloroform and carbon tetrachloride. not soluble in water. The adduct of β-menadione and sodium bisulfite is water-soluble menadione sodium bisulfite, that is, vitamin K3. β-menadione is the active ingredient of K3. It is mainly used as a feed additive and can promote The liver of livestock and poultry synthesizes prothrombin, and promotes the synthesis of plasma coagulation factors in the liver, acting as a hemostatic agent. [0003] At present, the industrial production method of β-menadione is mainly based on the liquid phase oxidation method, mainly using the chromium salt oxi...

AI Technical Summary

Problems solved by technology

The productive rate that obtains beta-menaquinone with this method is about 70%, but can produce a large amount of chromium-containing waste water, and environmental pollution is very serious

At the same time, the product contains hexavalent chromium, which is a heavy metal, which will have a significant impact on the quality of the product

[0004] Patent document CN105839134A discloses a method for preparing β-menadione by indirect electrooxidation. Although this process uses cerium salt oxidation, it needs complex treatment of cerium salt solution before electrolysis can be carried out, and β-menaquinone After heating, it becomes an oil phase, while the cerium salt solution is a water phase, the two-phase reaction contact surface is small, the reaction time is long, and it is easy to cause partial β-menadione peroxidation

The process is complicated, not conducive to industrialization, and the cost is high