Vitamin K3 synthesis method and device

Abstract

The invention relates to a vitamin synthesis method, in particular to a vitamin K3 synthesis method and device, and belongs to the technical field of chemical synthesis. The vitamin K3 synthesis method mainly comprises the following two steps: S1, preparing an intermediate beta-menadione; and S2, adopting co-production to synthesize menadione sodium bisulfite (MSB) and menadione nicotinamide bisulfite (MNB), namely, based on the different water solubility of MSB and MNB, firstly performing sulfonation reaction synthesis and crystallization on the intermediate beta-menadione to obtain MSB, and then performing condensation synthesis on MSB mother liquor to obtain MNB. The method comprises preparation of a key intermediate beta-menadione and synthesis of MSB (menadione sodium bisulfite) and MNB (menadione nicotinamide bisulfite), a co-production process is adopted, namely, based on the different water solubility of MSB and MNB, synthesizing and crystallizing are carried out to obtain MSB, and then MNB is synthesized by utilizing mother liquor.

Description

technical field [0001] The invention relates to a vitamin synthesis method, in particular to a vitamin K3 synthesis method and device, and belongs to the technical field of chemical synthesis. Background technique [0002] Vitamin K3, Chinese name: menadione, menadione sodium bisulfite (MSB) and nicotinamide menadione bisulfite (MNB). Vitamin K3 is a vitamin nutritional supplement, which belongs to procoagulant drugs, and can be used to treat hemorrhagic diseases caused by vitamin K deficiency, such as neonatal hemorrhage, vitamin K deficiency and hypoprothrombinemia caused by intestinal malabsorption Wait. [0003] The domestic production of menadione sodium bisulfite (MSB) and menadione nicotinamide hydrogen sulfite (MNB) generally adopts an independent production system, that is, the production of MSB products is based on the batch reaction of β-methylnaphthalene as raw material to prepare β- Menadione, and then use β-menaquinone to prepare MSB reaction solution in sodi...

AI Technical Summary

Problems solved by technology

The synthesis of MSB needs to be completed in a certain water phase system, but due to the considerable solubility of MSB in water, the recovery rate of MSB products is low, and the amount of ethanol in the synthesis system is not enough to completely dissolve β-menaquinone, and partial synthesis The reaction is a solid-liquid reaction, so that the reaction time is prolonged, the by-products increase, and the MSB conversion rate decreases

However, the solubility of MNB in ​​water is low, and there is ethanol in the reaction system, which will cause the precipitation of inorganic salts in the MNB particles and cannot be washed away, resulting in unqualified MNB content.

[0004] There are also manufacturers that do not add ethanol when making MNB, first synthesize MSB in the water system, β-menadione reacts with sodium bisulfite solution in solid form, the reaction time is long, and the by-product is as high as 12~15%, and because there is no ethanol There will be organic impurities entering MNB, resulting in poor stability of MNB, and a large amount of wastewater will be generated during the production process (about 20 tons of wastewater per ton of MNB)

Images