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Electrochemistry fluorination electrolytic bath

A fluorinated electrolytic cell and electrochemistry technology, applied in the field of electrochemistry, can solve the problems of small effective electrolysis area, decreased electrolysis efficiency, hindered electrolysis, etc., and achieve a large effective electrolysis area, high space utilization rate and reduced labor intensity Effect

Active Publication Date: 2015-04-22
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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  • Electrochemistry fluorination electrolytic bath
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  • Electrochemistry fluorination electrolytic bath

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 to fasten, measure the insulati...

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 electrochemistry fluorination electrolytic bath. The electrochemistry fluorination electrolytic bath comprises a bath body (1), a bath cover (2), a bath body side wall temperature control clamping sleeve (3), a bottom discharge valve (4), electrode sets (5), anode conductive rods (6), cathode conductive rods (7) and a conductive cross beam (8). Each electrode set is structurally characterized in that plate electrodes are fixed with fixing shafts (15) penetrating plate electrode center holes (19), the interval between the plate electrodes is controlled by annular insulation pads (17), and the fixing shafts fix the plate electrodes into one electrode set through insulation nuts (16) at the two ends. The conductive cross beam is of a hollow-out structure, electrode screw rods (20) on the plate electrodes penetrate through the hollow-out structure to be fixed on the conductive cross beam, and the conductive cross beam and the bath cover (2) are assembled together through the anode conductive rods (6) and the cathode conductive rods (7). The electrochemistry fluorination electrolytic bath has the advantages of being large in capacity, high in space utilization rate, large in effective electrolytic area and the like. The plate electrodes are movably connected with the conductive cross beam, dismounting is convenient, and assembly is easy.

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 Applications(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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