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Preparation method of menadione

A technology of menaquinone and menaquinone is applied in the preparation field of menaquinone and the preparation of menaquinone by direct electrolytic oxidation of 2-methylnaphthalene, which can solve the problem of electrosynthesis process enlargement, complex process, and the amount of chromium-containing wastewater. Large and other problems, to achieve the effect of simple methods

Active Publication Date: 2020-11-06
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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  • Preparation method of menadione

Examples

Experimental program
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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 mixed with the electrolyte solution, and the composition of the electrolyte solution 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 ...

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 preparation method of menadione. The method comprises the steps: preparing an electrolyte from a raw material 2-methylnaphthalene and an electrocatalyst, and carrying out a direct electrolytic oxidation reaction on the 2-methylnaphthalene under a constant current condition to prepare menadione, wherein the electrocatalyst is one or more of RClO4, RPF6 or RBF4, and R is one of Li < + >, Na < + >, K < + > and NH4 < + >. The electrolyte can be repeatedly used all the time, the method is simple, no oxidation reagent is added, no three wastes are generated, the product selectivity of the electrooxidation reaction reaches 95% or above, and the method is a green synthesis technology with development prospects and quite meets the green and environment-friendly 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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IPC IPC(8): C25B3/02C07C46/10C07C50/12B01J27/06B01J27/24
CPCC07C46/10B01J27/06B01J27/24B01J35/33C07C50/12
Inventor 初晓东杜旺明刘释水潘亚男李俊平黎源
Owner WANHUA CHEM GRP CO LTD
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