Method for preparing beta-menadione and derivative menadione sodium bisulfate of beta-menadione by taking Ce < 4 + > as oxidant

Abstract

The invention relates to a method for preparing beta-menadione by using Ce < 4 + > as an oxidant, which comprises the following steps: step 1, preparing an electrolyzed ceric methanesulfonate solution, and dissolving beta-methylnaphthalene in a first organic solvent to obtain a beta-methylnaphthalene organic solution; step 2, adding a part of the ceric methanesulfonate solution into a reaction kettle as a priming solution; 3, carrying out a three times of constant temperature reaction, and 4, after the reaction is finished, filtering to obtain a beta-menadione filter cake; layering a filtrateto obtain an organic solvent oil phase layer and a cerium methanesulfonate water phase layer; and 5, extracting the beta-menadione filter cake with a first organic solvent, filtering, and layering thefiltrate to obtain a beta-menadione organic solution oil phase layer and a cerous methanesulfonate water phase layer. According to the method, a high-speed shearing emulsifying machine is adopted inthe oxidation process to strengthen mass transfer, so that the use of an emulsifying agent is avoided, and the problems of foam, electrolytic efficiency and long-term cyclic utilization enrichment inthe oxidation residual liquid aftertreatment and electrolysis process are solved.

Description

technical field [0001] The present invention relates to a kind of chemical synthesis method, particularly a kind of Ce 4+ The method for preparing β-menadione and its derivative sodium bisulfite menadione as an oxidizing agent belongs to the technical field of chemical synthesis. Background technique [0002] The chemical name of β-menadione is 2-methyl-1,4-naphthoquinone. The pure product is bright yellow crystal or crystalline powder with a special pungent smell. Insoluble in water, soluble in ethanol, benzene, chloroform, carbon tetrachloride and vegetable oils. Stable in air, easy to deteriorate and decompose when exposed to light, alkali and reducing agent. Used as a feed additive raw material, the main function is to promote the synthesis of prothrombin in the liver of livestock and poultry, and to promote the synthesis of plasma coagulation factors in the liver, as a hemostatic agent. [0003] MSB (menaquinone sodium bisulfite) obtained by the addition reaction of...

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Problems solved by technology

However, an emulsifier is added during the oxidation process to enhance mass transfer and speed up the reaction rate, but the emulsifier cannot be completely and effectively decomposed and removed during the post-treatment of the oxidation residue and the electrolysis process. A large amount of foam is generated, which makes it difficult to operate normally and the electrolysis efficiency is reduced, and it will gradually accumulate during the long-term recycling process, which will eventually make the cerium solution unable to continue to be applied.

[0011] Therefore, considering various factors, the synthesis process commonly used in industrial production is the "chromium method" route, but in order to solve the problem of a large amount of chromium-containing wastewater produced by the chromium series oxidant process, high-yield, environmentally friendly β-menaquinone is being developed both at home and abroad. Research on synthetic technology has never stopped, but the results are not high

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