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A kind of preparation method of menadione

A technology of menaquinone and menaquinone, which is applied to the preparation of menaquinone by direct electrolytic oxidation of 2-methylnaphthalene, and the field of the preparation of menaquinone, can solve serious pollution, reduce target product selectivity and product yield , electrode plate deactivation and other problems, to achieve the effect of improving selectivity and conversion, inhibiting polymerization side reactions, and preventing electrode deactivation

Active Publication Date: 2022-01-07
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing production of menadione mainly adopts the joint production process of dichromate oxidation and by-product chrome tanning agent. This process has the disadvantages of large amount of chromium-containing wastewater, serious pollution, and complicated process, especially the treatment of chromium-containing waste liquid. Problems have plagued the industrial production of menadione
[0005] In a mature organic electrochemical system, the polymerization reaction of organic matter on the electrode plate can not only deactivate the electrode plate, but also greatly reduce the selectivity and product yield of the target product. These problems have always plagued the process scale-up of electrosynthesis

Method used

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  • A kind of preparation method of menadione
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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Electrolyte preparation: Prepare 100g of supporting electrolyte solution with 98wt% concentrated sulfuric acid and deionized water according to the mass ratio of about 1:4, LiClO 4Weigh 2.28g and join in the supporting electrolyte solution; 15g of raw material 2-methylnaphthalene is dissolved in 35g of dichloromethane to prepare the raw material solution, and the supporting electrolyte solution is added in the raw material solution to be prepared as an electrolyte, and the composition of the electrolyte obtained is 2 -Methylnaphthalene 10wt%, electrocatalyst LiClO 4 1.5wt%, dichloromethane 23.0wt%, concentrated sulfuric acid 13.1wt%, the rest is deionized water;

[0041] (2) Electrolysis reaction: the anode is made of lead dioxide-coated pole plate, the cathode is made of copper pole plate, and the circuit is connected to form a closed loop with the electrolyte system; the constant temperature water bath is turned on, and the temperature of the water bath is contro...

Embodiment 2

[0047] (1) Electrolyte preparation: Prepare 100g of supporting electrolyte solution with 98wt% concentrated sulfuric acid and deionized water according to the mass ratio of about 1:1, LiClO 4 Weigh 7.5g and add it to the supporting electrolyte solution; 75g of the raw material 2-methylnaphthalene is dissolved in 75g of ethylcyclohexane to prepare the raw material solution, and the supporting electrolyte solution is added to the raw material solution to prepare the electrolyte solution to obtain the composition of the electrolyte solution For: 2-methylnaphthalene 29.1wt%, electrocatalyst LiClO 4 2.9wt%, ethylcyclohexane 29.1wt%, concentrated sulfuric acid 19.4wt%, the rest is deionized water;

[0048] (2) Electrolysis reaction: the anode is made of platinum-coated plate, the cathode is made of lead plate, and the circuit is connected to form a closed loop with the electrolyte system; the constant temperature water bath is turned on, the temperature of the water bath is control...

Embodiment 3

[0051] (1) Electrolyte preparation: Prepare 100g of supporting electrolyte solution with 98wt% concentrated sulfuric acid and deionized water according to the mass ratio of about 1:3, LiClO 4 Weigh 8.3g and add it to the supporting electrolyte solution; 17.4g of raw material 2-methylnaphthalene is dissolved in 48.6g of ethylcyclohexane to prepare a raw material solution, and the supporting electrolyte solution is added to the raw material solution to prepare an electrolyte solution to obtain an electrolyte solution The composition is: 2-methylnaphthalene 10wt%, electrocatalyst LiClO 4 4.7wt%, ethylcyclohexane 27.9wt%, concentrated sulfuric acid 11.5wt%, the rest is deionized water;

[0052] (2) Electrolysis reaction: the anode is made of platinum-coated plate, the cathode is made of lead plate, and the circuit is connected to form a closed loop with the electrolyte system; the constant temperature water bath is turned on, the temperature of the water bath is controlled at 60°...

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Abstract

The invention discloses a method for preparing menadione. The method is prepared by preparing raw material 2-methylnaphthalene and an electrocatalyst into an electrolyte, and then performing a direct electrolytic oxidation reaction of 2-methylnaphthalene under constant current conditions. Menadione; The electrocatalyst is RClO 4 、RPF 6 or RBF 4 One or more of, wherein R is Li + 、Na + 、K + , NH 4 + One of. The electrolytic solution in the present invention can be reused all the time, the method is simple, there is no addition of oxidizing reagents and the generation of three wastes, and the product selectivity of the electro-oxidation reaction reaches more than 95%, which is a green synthesis technology with development prospects, which is very suitable for Environmental protection requirements in the current chemical production process.

Description

technical field [0001] The invention relates to a preparation method of menadione, in particular to a preparation method of direct electrolytic oxidation of 2-methylnaphthalene to prepare menadione, which belongs to the technical field of organic chemical industry. [0002] technical background [0003] Menadione is a fat-soluble vitamin drug, a key intermediate for the synthesis of vitamin K3, an important raw material for fine chemicals, and is widely used in medicine and feed additives. The existing production of menadione mainly adopts the joint production process of dichromate oxidation and by-product chrome tanning agent. This process has the disadvantages of large amount of chromium-containing wastewater, serious pollution, and complicated process, especially the treatment of chromium-containing waste liquid. Problems have plagued the industrial production of menadione. [0004] The document "Cr(IV) Oxidation of 2-Methylnaphthalene to Preparation of 2-Methyl-1,4-Napht...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/07C25B3/23C07C46/10C07C50/12B01J27/06B01J27/24
CPCC07C46/10B01J27/06B01J27/24B01J35/0033C07C50/12
Inventor 初晓东杜旺明刘释水潘亚男李俊平黎源
Owner WANHUA CHEM GRP CO LTD