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Electrochemical fluorination using interrupted current

An electrochemical, current-level technology, applied in electrolysis components, electrolysis process, halogenation electrolysis, etc., can solve problems such as current blocking, reduction in electrolytic cell conductivity, and increase in resistance

Inactive Publication Date: 2000-05-24
3M CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This problem can become very serious and lead to a situation known as "current blocking", which is manifested by a continuous increase in electrical resistance and a continuous decrease in conductivity in the bath

Method used

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  • Electrochemical fluorination using interrupted current
  • Electrochemical fluorination using interrupted current
  • Electrochemical fluorination using interrupted current

Examples

Experimental program
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Effect test

Embodiment 1

[0064] 97% by weight of anhydrous hydrogen fluoride and 3% by weight of dimethyl disulfide were charged into a 2.5-liter electrochemical fluorination cell as described in US Patent No. 2,713,593. The electrochemical fluorination cell is equipped with an overhead condenser at -40°C, a nickel anode of 0.40 square feet (3.7 square decimeter) and a single control device equipped with a cycle timer. Continue to supply a mixture of octyl sulfonyl fluoride containing 6% (weight) of dimethyl disulfide to the electrolytic cell. The operating conditions of the electrolytic cell are: pressure 30 psig, temperature 54°C, and current controlled at 53 amps / ft. 2 (5.7 Ampere / square decimeter), maintain a relatively constant voltage at 6.0V.

[0065] After the electrolyzer reaches a steady state, increase the current to 58A / ft 2 (6.2 amperes / square decimeter), reduce the electrolytic cell voltage to 3.3V (V r )3 seconds to make the current drop to basically 0 (T e = 27 seconds, T r = 3 seconds), s...

Embodiment 2

[0067] Basically the process used in the circulating current environment as described in Example 1 was used, maintaining the same current circulating process, without adding dimethyl disulfide, and adding octylsulfonyl fluoride. Current control at 56amps / ft 2 (6.0 ampere / square decimeter), a steady-state high voltage with a voltage of 5.6V. The low voltage is 3.3V. Perfluorooctyl sulfonyl fluoride is produced at an average yield of 21 g / 50 ampere·hour.

Embodiment 3

[0069] An electrolyte mixture containing 84% (by weight) of anhydrous hydrogen fluoride and 2.5 pounds of dimethyl disulfide is charged into an electrochemical system with a 27 square foot (251 square decimeter) anode as described in US Patent No. 2,713,593 In the fluorination electrolytic cell. Within 3 days, continue to supply a mixture of octylsulfonyl fluoride containing 94% (weight) of octylsulfonyl fluoride and 6% (weight) of dimethyl disulfide to the electrolytic cell until a stable status. The voltage under non-interrupted current is 5.8 volts. The current is 1521 amperes, and the normalized resistance is 0.028 ohm-square feet (0.26 ohm-decimeter square).

[0070] The above current is interrupted for 8 seconds every 72 seconds (T e = 72 seconds, T r = 8 seconds), so that the voltage of the electrolytic cell is lower than that of the non-intermittent electrolytic cell. This also leads to an increase in current (current density) and a decrease in normalized resistance. The v...

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PUM

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Abstract

A method for electrochemical fluorination of a substrate, the fluorination method comprising the steps of: providing a substrate containing at least one hydrogen bonded by a carbon bond; preparing a reaction solution containing the substrate and hydrogen fluoride; making a sufficient amount of electric current Passing through the reaction liquid so that one or more hydrogens on the substrate are replaced by fluorine, the current is interrupted by cycles defined by current levels including high current and low current; wherein, the current Intermittent in such a way that the resistance of the electrolyzer operated by intermittent current is lower than that of the electrolyzer operated by non-intermittent current.

Description

Invention field [0001] The invention relates to an electrochemical fluorination method for the electrochemical fluorination of organic materials. Background technique [0002] Fluorinated chemicals (for example, fluorinated or perfluorinated organic compounds) are generally useful chemical materials with commercial value. Fluorine-containing chemicals show many useful properties, for example, they are inert, non-polar, and hydrophobic and oleophobic. In this way, fluorine-containing chemicals can be used in a wide range of fields. They can be used as oil-resistant, water-repellent, and rust-resistant chemicals, as well as refrigerants and heat exchangers; alternatively, they can be used as solvents and cleaning agents. Due to the versatility of fluorine-containing chemicals and the increasing demand for these materials, the fluorine-containing chemicals manufacturing industry has put forward continuous requirements for new and improved preparation methods for the preparation of f...

Claims

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Application Information

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IPC IPC(8): C25B3/28
CPCC25B3/08Y02P20/129C25B3/28
Inventor S·D·波尔森J·C·斯潘格勒E·N·华莱士L·M·格鲁比纳G·I·考罗瓦A·E·冈德里纳A·A·克拉西利尼科夫
Owner 3M CO
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