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The method for electrolytic synthesis of anisole

A technology of electrolytic synthesis and anisole, which is applied in the direction of electrolytic components, electrolytic process, electrolytic organic production, etc. It can solve the problems of high toxicity of dimethyl sulfate, expensive methyl iodide, harsh reaction conditions, etc.

Active Publication Date: 2019-04-05
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Among the methyl sources currently used in the route to synthesize anisole with phenol as the starting material, methyl iodide is expensive, dimethyl sulfate is highly toxic, and dimethyl carbonate and methanol are too low in activity. The reaction conditions are harsh.

Method used

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  • The method for electrolytic synthesis of anisole
  • The method for electrolytic synthesis of anisole

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] a. Dissolving phenol and tetramethylammonium chloride in 40% methanol completely in a mass ratio of 1:3, and stirring evenly to obtain an electrolyte;

[0014] b. Connect the two ends of the output of the power supply to platinum electrodes, then immerse the two electrodes in the electrolyte obtained in step a at the same time, and perform temperature-controlled electrolysis under the condition of uniform stirring, the electrolysis voltage is 10 volts, and the temperature of the electrolyte is controlled at 25°C;

[0015] c. After the electricity passing through is 1.2 times of the electricity required for the complete reduction of tetramethylammonium chloride, stop the electrolysis reaction. When the decompression gauge pressure is -0.8 MPa, the temperature is 40 ° C, the solvent methanol is distilled, and the temperature is increased to 120 Continue vacuum distillation at ℃, the gauge pressure of vacuum distillation is -0.8 MPa, and the distillate is anisole.

Embodiment 2

[0017] a. Dissolving phenol and tetramethylammonium chloride in 30% methanol completely in a mass ratio of 1:2, and stirring evenly to obtain an electrolyte;

[0018] b. Connect the two ends of the output of the power supply to platinum electrodes, and then simultaneously immerse the two electrodes in the electrolyte solution obtained in step a, and perform temperature-controlled electrolysis under the condition of uniform stirring, the electrolysis voltage is 15 volts, and the temperature of the electrolyte solution is controlled at 15°C;

[0019] c. After the electricity passing through is 1.5 times of the electricity required for the complete reduction of tetramethylammonium chloride, stop the electrolysis reaction. When the decompression gauge pressure is -0.8 MPa, the temperature is 30 ° C, the solvent methanol is distilled, and the temperature is raised to 100 Continue vacuum distillation at ℃, the gauge pressure of vacuum distillation is -0.8 MPa, and the distillate is a...

Embodiment 3

[0021] a, phenol and tetramethylammonium chloride with a mass ratio of 1:1 are completely dissolved in ethanol with a mass percentage concentration of 20%, and the electrolyte is obtained after stirring;

[0022] b. Connect platinum electrodes to both ends of the output of the power supply, and then simultaneously immerse the two electrodes in the electrolyte solution obtained in step a, and perform temperature-controlled electrolysis under the condition of uniform stirring, the electrolysis voltage is 20 volts, and the temperature of the electrolyte solution is controlled at 50°C;

[0023] c. After the electricity passing through is 1.6 times of the electricity required for the complete reduction of tetramethylammonium chloride, stop the electrolysis reaction, distill the solvent ethanol at a decompression gauge pressure of -0.8 MPa, and a temperature of 35°C, and raise the temperature to 110°C Continue the vacuum distillation, the gauge pressure of the vacuum distillation is ...

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Abstract

The invention relates to a method for electrolytically synthesizing anisole. The method utilizes electrolysis technology, and uses graphite electrodes or platinum electrodes to electrolyze methanol solutions of phenol and tetramethylammonium chloride under normal temperature and pressure conditions. The electrolysis reaction After completion, use vacuum distillation and purification to obtain anisole. Compared with the existing methods, the method has the advantages of low raw material price, mild synthesis conditions and the like.

Description

technical field [0001] The invention relates to a method for electrolytically synthesizing anisole, in particular to a method for synthesizing anisole by using phenol and tetramethylammonium chloride as raw materials by using an electrochemical method. Background technique [0002] At present, the traditional production routes for producing anisole from phenol at home and abroad mainly include the following types: the first one uses methyl iodide as a methyl source. Phenol reacts with methyl iodide to produce anisole under microwave irradiation; the second one uses dimethyl sulfate as the methyl source. Phenol and dimethyl sulfate are catalyzed by aluminum oxide to produce anisole above 130°C; the third type uses dimethyl carbonate as the methyl source. Phenol and dimethyl carbonate produce anisole in the presence of catalysts such as high temperature and high pressure and strontium carbonate. The fourth type uses methanol as the methyl source. Phenol and methanol are cat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/04C25B11/04C25B3/25
CPCC25B11/04C25B3/25
Inventor 张政委王强向迎梅
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI