A kind of method for preparing perfluoromethylcyclohexane

A technology of perfluoromethylcyclohexane and benzoic acids, which is applied in the field of preparation of perfluoromethylcyclohexane, can solve the problem of accelerating anode corrosion and increasing the by-products of resinization, increasing the difficulty of post-processing of crude products, and reducing electrolysis The problems such as the operation period of the kettle can be solved, and the effect of solving the by-products of resinization, improving the uneven heat conduction and improving the electrolysis efficiency

Active Publication Date: 2019-06-04
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

However, the use of sodium fluoride as a conductive agent in the process of electrolytic fluorination accelerates the increase of anode corrosion and resinized by-products, and the generated polymer slag easily blocks the discharge port at the bottom of the electrolytic kettle, which not only greatly reduces the electrolysis efficiency, Reducing the operable period of the electrolytic kettle also increases the difficulty of post-treatment of crude products, resulting in a lower electrolytic yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Add 2kg of p-aminobenzotrifluoride, 5kg of benzobenzotrifluoride, and 100kg of anhydrous hydrogen fluoride to the batching kettle at 6°C in sequence, and stir continuously for 1.5h under normal pressure to prepare an electrolyte solution for later use;

[0019] 2) The above-mentioned electrolyte is added into the electrolytic kettle through a circulation pump, and mechanical stirring is continued under normal pressure;

[0020] 3) Control the electrolysis voltage to 5.5V, the electrolysis temperature to 5-15°C, and the current density to 25.3mA / cm 2 ; The gas phase obtained by electrolysis is condensed and refluxed to realize the secondary utilization of hydrogen fluoride, and the rest of the gas phase is emptied after being washed with alkali; the crude product is collected through the bottom discharge, and the crude product is purified to obtain perfluoromethylcyclohexane product. The purity of the product is 92%, the yield is 45%, the electrolytic kettle runs cont...

Embodiment 2

[0022] 1) Add 12kg of o-trifluorobenzoic acid, 30kg of trifluorotoluene, and 100kg of anhydrous hydrogen fluoride into the batching kettle at 6°C in sequence, and continue stirring for 1.5h under normal pressure to prepare an electrolyte solution for later use;

[0023] 2) The above-mentioned electrolyte is added into the electrolytic kettle through a circulation pump, and mechanical stirring is continued under normal pressure;

[0024] 3) Adjust the ultrasonic frequency to 25-50KHz, control the electrolysis voltage to 5.5V, the electrolysis temperature to 5-15°C, and the current density to 25.3mA / cm 2 ; The gas phase obtained by electrolysis is condensed and refluxed to realize the secondary utilization of hydrogen fluoride, and the rest of the gas phase is emptied after being washed with alkali; the crude product is collected through the bottom discharge, and the crude product is purified to obtain perfluoromethylcyclohexane product. The purity of the product is 96%, the yie...

Embodiment 3

[0026] 1) At 8°C, add 8kg of p-aminobenzotrifluoride, 10kg of benzobenzotrifluoride, and 100kg of anhydrous hydrogen fluoride into the batching kettle in turn, and continue stirring for 1.5h under normal pressure to prepare an electrolyte solution for later use;

[0027] 2) The above-mentioned electrolyte is added into the electrolytic kettle through a circulation pump, and mechanical stirring is continued under normal pressure;

[0028] 3) Adjust the ultrasonic frequency of the cell to 25-50KHz, control the electrolysis voltage to 5.5V, the electrolysis temperature to 5-15°C, and the current density to 27.0mA / cm 2 ; The gas phase obtained by electrolysis is condensed and refluxed to realize the secondary utilization of hydrogen fluoride, and the rest of the gas phase is emptied after being washed with alkali; the crude product is collected through the bottom discharge, and the crude product is purified to obtain perfluoromethylcyclohexane product. The purity of the product is...

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Abstract

The invention discloses a method for preparing perfluoromethylcyclohexane, which comprises the following steps: (1) sequentially adding electrolyte, electrolytic additives, and anhydrous hydrogen fluoride into a batching kettle at 5-10°C, and continuously Stir for 1-1.5 hours, prepare the electrolyte solution, and set aside; the mass ratio is electrolyte: electrolysis additive: anhydrous hydrogen fluoride = 5-30: 2-12: 100; (2) Add the above-mentioned electrolyte solution into the electrolytic kettle through a circulating pump , continuous mechanical stirring under normal pressure; (3) start the electrolysis, the temperature of the electrolytic kettle is -10-20°C; the current density is 5-50mA / cm2; the crude product is collected by discharging at the bottom of the electrolytic kettle, and the crude product is purified to obtain perfluoromethyl ring Hexane products. The method has the advantages of simple process, high product purity, high electrolysis efficiency, high corrosion resistance of equipment, and long operation period of the electrolysis kettle.

Description

technical field [0001] The present invention relates to the preparation method of perfluoromethylcyclohexane. Background technique [0002] Perfluoromethylcyclohexane has significant chemical inertness and often exhibits excellent thermal stability, high dielectric properties, and excellent thermophysical and electrical properties. As a kind of fluorine-based cleaning agent, perfluoromethylcyclohexane has been widely used in precision instruments, liquid crystal, medical equipment and other production industries. [0003] The synthesis methods of perfluoromethylcyclohexane mainly include metal fluorination and electrochemical fluorination. Among them, the metal fluorination method uses toluene as a raw material to fluorinate cobalt trifluoride to obtain perfluoromethylcyclohexane. Although this method has a high yield, it is difficult to achieve large-scale production because fluorine gas is used to repeatedly activate CoF2 during the gas-solid reaction process, resulting ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/08C25B3/28
CPCC25B3/28
Inventor 牛鹏飞任章顺黄晓磊鲍金强张金彪
Owner 昊华气体有限公司
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