Preparing method for beta-menadione

Abstract

The invention discloses a preparing method for beta-menadione. The preparing method includes the following steps that 1, ceric sulfate is dissolved in a sulfuric acid solution, a ceric sulfate solution is obtained, the beta-methylnaphthalene is dissolved in an organic solvent, and a beta-methylnaphthalene organic solution is obtained; 2, the ceric sulfate solution and the beta-methylnaphthalene organic solution are simultaneously added into a reaction kettle, the mixture is stirred and reacted at the constant temperature, the reaction is ended, cooling crystallization is carried out, and the finished-product beta-menadione is obtained through filtering; 3, the filtered cerous sulfate solution in a liquid phase is separated from the organic solvent, the organic solution is distilled and recycled to be reused, and the cerous sulfate solution is subjected to electrolytic oxidation through a diaphragm to be reused. Chromium oxidation is thoroughly replaced with the preparing method for thebeta-menadione, hexavalent chromium does not exist in the product, the beta-methylnaphthalene is dissolved in an organic phase and reacted, the contact area of the material is larger, the reaction rate is higher, peroxidation of the beta-menadione can be avoided, and the product purity is high.

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. Insoluble 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 oxida...

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