A method for the indirect electrosynthesis of quinones assisted by ultrasound

An ultrasonic-assisted, compound technology, applied in electrolytic components, electrolytic process, electrolytic organic production, etc., can solve the problems of low yield, high electrolytic production cost, long chemical reaction time, etc., to reduce cell pressure, facilitate circulation, The effect of improving product selectivity

Active Publication Date: 2021-10-15
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problems of long chemical reaction time, low yield and high cost of electrolytic production in single methanesulfonic acid in the prior art, the present invention provides a method for the indirect electrosynthesis of quinone compounds assisted by ultrasound

Method used

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  • A method for the indirect electrosynthesis of quinones assisted by ultrasound
  • A method for the indirect electrosynthesis of quinones assisted by ultrasound
  • A method for the indirect electrosynthesis of quinones assisted by ultrasound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Electrolysis part: see reaction device figure 1 . The prepared 1.2L, 1mol / L Ce 3+ The mixed acid solution (methanesulfonic acid 2mol / L, sulfuric acid 0.4mol / L), the flow rate is controlled by a flow meter and a pump, and it is passed into the anode chamber for circulation, and the same operation is performed for the cathode. The electrolytic flow rate is controlled at 40L / H, and the current density is 20mA / cm 2 , the electrolysis temperature is 40°C, the electrolysis time is 7 hours and 20 minutes, and the Ce is measured by titration after the electrolysis 4+ Ion concentration, Ce 3+ The ion conversion rate is 60%, the current efficiency is 85%, and the voltage is 2.2V. After the reaction is completed, the bypass is opened, the anolyte enters the synthesis reaction chamber, the catholyte enters the anode liquid storage tank, and the liquid obtained by the synthesis reaction is passed into the cathode chamber to continue electrolysis and cycle operation.

[0042] S...

Embodiment 2

[0047] The difference with the electrolysis step of embodiment 1 is: Ce 3+ The ion concentration is 0.8mol / L, the electrolysis time of the electrolysis part is the theoretical time condition, and the rest of the steps are unchanged, using Fe 2+ Titrate to get Ce 4+ Concentration, the conversion rate is calculated to obtain a current efficiency of 69%, and a voltage of 2.1V.

Embodiment 3

[0049] The difference with the electrolysis step of Example 1 is that the current density is 60mA / cm 2 , the electrolysis time of the electrolysis part is the theoretical time condition, and the rest of the steps remain unchanged, using Fe 2+ Titrate to get Ce 4+ concentration, calculate the conversion rate to obtain a current efficiency of 66%, and a voltage of 2.6V.

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Abstract

The invention discloses a method for ultrasonic-assisted indirect electrosynthesis of quinone compounds. The method comprises the following steps: (1) preparing an electrolyte, the electrolyte being Ce 3+ The mixed acid aqueous solution, described mixed acid is made up of methanesulfonic acid and sulfuric acid, wherein Ce 3+ The ion concentration is 0.8~1mol / L, the concentration of methanesulfonic acid is 2 mol / L, and the concentration of sulfuric acid is 0.2~0.6mol / L; (2) The electrolyte prepared in step (1) is respectively passed into the anode of the plate and frame electrolytic cell Chamber and cathode chamber are circulated, electrified for electrolysis to obtain anolyte and catholyte; the catholyte enters the anode liquid storage tank; (3) Use naphthalene, 2-methylnaphthalene or anthracene as the reaction substrate to prepare the raw material solution (4) Mix the anolyte obtained in step (2) with the raw material liquid obtained in step (3), and carry out a catalytic oxidation reaction under the conditions of ultrasonic assistance and mechanical stirring, and obtain a reaction mixture after sufficient reaction, and the reaction mixture is passed through After treatment, the corresponding quinones can be obtained.

Description

technical field [0001] The invention relates to a method for indirect electrical synthesis of 1,4-naphthoquinone, 2-methyl-1,4-naphthoquinone and 9,10-anthraquinone compounds. Background technique [0002] As an important organic chemical intermediate, quinone compounds are widely used in many fields closely related to daily life, such as pesticides, medicines, dyes and flame retardants. [0003] The existing reaction methods for generating quinone compounds are mainly concentrated in the gas phase catalytic oxidation method. Taking 1,4 naphthoquinone as an example, Kawasaki Chemical Industry in Japan first completed the industrial production of this process, but the conversion rate of naphthoquinone is only 100% 20 or so. Domestic chemical companies use chromic anhydride to oxidize naphthalene to synthesize 1,4-naphthoquinone under liquid phase conditions, but there are still shortcomings such as low selectivity, low product yield, large amounts of chromium-containing acid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/07C25B3/23
Inventor 褚有群卢圣达陈赵扬
Owner ZHEJIANG UNIV OF TECH
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