A kind of method for preparing perfluoromethylcyclohexane

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 ...

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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