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An electrochemical fluorination electrolyzer

A fluorinated electrolytic cell and electrochemical technology, applied in the field of electrochemistry, can solve the problems of small effective electrolysis area, decreased electrolysis efficiency, and time-consuming, and achieve the effects of large effective electrolysis area, reduced labor intensity, and high space utilization rate

Active Publication Date: 2017-01-25
昊华气体有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Since the electrode stack is mostly square, the cylindrical electrolytic kettle has disadvantages such as low space utilization rate in the kettle and small effective electrolysis area.
During the process of electrolytic fluorination, organic matter breakage and carbonization reactions occur on the surface of the electrode, and solid residues are deposited on the bottom of the electrolytic cell, which may easily lead to blockage of the discharge port at the bottom
The corrosion of the plate and the deposition of solid residues hinder the progress of electrolysis, resulting in a gradual decline in electrolysis efficiency. The electrolysis process needs to be dismantled and inspected regularly, and the surface of the electrode must be polished to ensure that the surface of the electrode is clean
At present, most of the electrode plates are connected by fixed connections, and the electrode plates cannot be disassembled in a single piece. Since the distance between the electrode plates required by the electrolytic fluorination process is very small, it is often necessary to cut off the electrode plates and then weld them during the dismantling process, which is time-consuming and laborious.
[0005] In the prior art, the electrode plate spacing of each electrode group is fixed, but different electrolytic raw materials have different requirements for the electrode plate spacing. To produce different products, different electrode plate spacing needs to be adjusted. In the prior art, the electrode set must be replaced as a whole. The slot is labor intensive

Method used

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  • An electrochemical fluorination electrolyzer
  • An electrochemical fluorination electrolyzer
  • An electrochemical fluorination electrolyzer

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Taking the electrolytic fluorination of methanesulfonyl chloride as an example, 51 nickel electrode plates, nickel beams, rods and nickel nuts with a thickness of 2mm were polished with a wire wheel brush before use. It is divided into 3 groups of electrode groups, one anode conductive beam, one cathode conductive beam, each electrode group has 17 electrode plates (9 anodes, 8 cathodes), and the threaded PTFE fixed shaft 15 The electrode plate is fixed through the center hole 19 of the plate, and the cathode and anode plates are insulated with a 10mm thick annular polytetrafluoroethylene insulating pad 17, and the distance between the electrode plates is 10mm. Fix the electrodes with Teflon insulating nuts 16 at both ends of the fixed shaft, and then pass the electrode screws 20 on the top of the cathode and anode electrode plates through the hollow structure in the middle of the nickel conductive beam 8, and use nickel conductive nuts 18 for fastening, after measuring ...

Embodiment 2

[0027] Taking the electrolytic fluorination of sulfolane as an example to produce perfluorobutylsulfonyl fluoride products, the cell assembly process is the same as in Example 1, the distance between the electrode plates is 5mm, and the electrolysis parameters are controlled: electrolysis concentration 7%, current 4.5-6.5V, current Density 20mA / cm 2 , the temperature is 10°C. During the process, the HF solution of sulfolane with a certain concentration in the proton tank is added through the feeding port, and the perfluorobutylsulfonyl fluoride generated during the electrolysis process is deposited on the bottom, and the crude product is collected through the bottom discharge valve and then washed with alkali, washed with water, dried, Distillation, the product yield reaches 48.7%.

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Abstract

The invention discloses an electrochemical fluorination electrolytic cell, which comprises a cell body (1), a cell cover (2), a temperature control jacket (3) on the side wall of the cell body, a bottom discharge valve (4), and an electrode group (5 ), the anode conductive rod (6), the cathode conductive rod (7), the conductive beam (8), the structure of the electrode group is: the electrode plate is fixed by the fixed shaft (15) passing through the pole plate center hole (19) , the distance between the electrode plates is controlled by an annular insulating pad (17), and the fixed shaft fixes the electrode plates into a group of electrode groups through the insulating nuts (16) at both ends; the conductive beam has a hollow structure, and the electrodes on the electrode plates The screw rod (20) passes through the hollow structure and is fixed on the conductive beam, and the conductive beam is assembled with the tank cover (2) through the negative and anode conductive rods. The electrolytic cell has the characteristics of large capacity, high space utilization rate, and large effective electrolysis area. The electrode plate is movably connected with the conductive beam, which is easy to disassemble and assemble.

Description

technical field [0001] The invention relates to the field of electrochemistry, in particular to an electrochemical fluorination electrolytic cell. Background technique [0002] The electrolytic fluorination method, also known as the Simons method, uses nickel as the anode, nickel or iron as the cathode, dissolves the organic reactant in anhydrous hydrogen fluoride to form a conductive electrolyte, and controls the voltage at a lower temperature to 4.5-6.0V , a method of introducing fluorine into organic molecules by anodic electrochemical fluorination. Electrolytic fluorination is currently widely used in the preparation of perfluorinated compounds. [0003] In the prior art, the Simons type electrolyzer mostly adopts a cylindrical electrolytic kettle with an electrode stack structure, and the electrolyte between the electrodes circulates by natural force during the electrolysis process, in which there is exchange of cold and heat, rising of gas and liquid The drop supplem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/08C25B9/00C25B3/28
Inventor 任章顺李立远袁胜芳黄晓磊张景利许福胜李贤武
Owner 昊华气体有限公司
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