Electrochemical preparation method of benzanthrone

A benzranthrone and electrochemical technology, applied in the field of electrochemical organic synthesis, can solve problems such as environmental pollution, complex synthesis process, etc., and achieve the effects of simple process, mild reaction conditions and easy separation

Pending Publication Date: 2022-05-06
赤峰市恒祥化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the shortcomings of the existing benzothrone synthesis process complex and serious environmental pollution, the purpose of the present invention is to provide a simple process, mild conditions, environmentally friendly electrochemical preparation method of benzoxantrone

Method used

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  • Electrochemical preparation method of benzanthrone
  • Electrochemical preparation method of benzanthrone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 0.048mol of anthraquinone and 50g of 85% sulfuric acid solution into the electrolytic cell with carbon electrodes as cathode and anode, respectively, under nitrogen protection, stir and heat the solution to 100°C at a heating rate of 1°C / min, and energize. , adjust the current to 3A, and dropwise add 0.1mol glycerol for 2h; when the passing electricity reaches 10560 coulombs, stop energizing; dilute the concentration of sulfuric acid solution to 60%, filter and wash the filter cake to pH 6 After ~7, it was dried in a constant temperature oven at 105 °C for 12 h to obtain benzrathranthrone.

Embodiment 2

[0027] Add 0.048mol of anthraquinone and 50g of 85% sulfuric acid solution into the electrolytic cell with platinum electrode as cathode and glass electrode as anode, under nitrogen protection, stir and heat the solution to 80°C at a heating rate of 2°C / min ; Power on, adjust the current to 10A, and add 0.048mol glycerol dropwise at the same time, the dropping time is 1h; when the passing electricity reaches 10560 coulombs, stop the power; Dilute the concentration of the sulfuric acid solution to 60%, filter and wash the filter cake to pH After being 6 to 7, it was placed in a constant temperature oven at 105° C. to dry for 6 hours to obtain benzrathrone.

Embodiment 3

[0029] Add 0.048mol of anthraquinone and 50g of 85% sulfuric acid solution into the electrolytic cell with platinum electrodes as cathode and anode respectively, under nitrogen protection, stir and heat the solution to 120°C at a heating rate of 2°C / min; , adjust the current to 3A, and add 0.48mol glycerol dropwise at the same time for 4h; when the passing electricity reaches 10560 coulombs, stop energizing; dilute the concentration of the sulfuric acid solution to 60%, filter and wash the filter cake to pH 6 After ~7, it was dried in a constant temperature oven at 105°C for 12 h to obtain benzrathrone.

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Abstract

The invention discloses an electrochemical preparation method of benzanthrone, which comprises the following steps: (1) sequentially adding electrolyte and anthraquinone into a diaphragm-free electrolytic tank, inserting a cathode and an anode, and introducing nitrogen; (2) stirring and heating to a reaction temperature, electrifying, dropwise adding glycerol into the electrolytic tank, and reacting at a constant temperature and a constant flow; and (3) after the reaction is completed, diluting the electrolyte until the mass fraction of the acid is 60%, separating out a product, filtering, washing and drying to obtain the benzanthrone. The method has the advantages that 1, the benzanthrone is prepared by adopting an electrochemical method, the process is simple, and the reaction condition is mild; 2, no organic solvent is added in the reaction process, no heavy metal salt is generated, and the method is an environment-friendly organic synthesis reaction; 3, a reaction product is easy to separate, the content of benzanthrone is high, and an additional treatment process is not needed; and 4, main pollutants in the electrolyte are some sulfonates of anthraquinone or benzophenone and are easy to remove, and the purified electrolyte can be recycled.

Description

Technical field: [0001] The invention relates to the technical field of electrochemical organic synthesis, in particular to an electrochemical preparation method of benzranthrone. Background technique: [0002] Benzoanthrone, also known as Benzoanthrone, is an important anthraquinone dye intermediate, which can be used to produce a variety of vat dyes, such as vat dark blue BO, vat brilliant green FFB, vat gray M, vat olive green B, vat Olive green T, reduced black BBN, etc.; its molecular formula is C 17 H 10 O, its molecular structure is as follows: [0003] [0004] The traditional synthesis process of benrazanthrone is as follows: under the condition of concentrated sulfuric acid, anthraquinone and glycerin are synthesized with iron powder or zinc powder as reducing agent and copper sulfate as catalyst. During the reaction, a large amount of heavy metal salts such as ferrous sulfate, ferric sulfate and copper sulfate will be produced. The concentrated sulfuric acid...

Claims

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Application Information

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IPC IPC(8): C25B3/07C25B3/25
CPCC25B3/07C25B3/25
Inventor 周林黄斌
Owner 赤峰市恒祥化工有限公司
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