Method for preparing perfluoro(methylcyclohexane)

A technology of perfluoromethyl cyclohexane and anhydrous hydrogen fluoride is applied in the field of preparation of perfluoromethyl cyclohexane, which can solve the problem of accelerating anode corrosion and increasing resinous by-products, increasing the difficulty of post-processing of crude products, and reducing electrolysis. It can solve problems such as the operation cycle of the kettle, and achieve the effect of solving the by-products of resinization, improving the uneven thermal conductivity, and improving the electrolysis efficiency.

Active Publication Date: 2017-09-01
昊华气体有限公司
View PDF6 Cites 9 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
current densityaaaaaaaaaa
Login to view more

Abstract

The invention discloses a method for preparing perfluoro(methylcyclohexane). The method comprises the following steps: (1) sequentially adding electrolyte, an electrolysis additive and anhydrous hydrogen fluoride into a proportioning kettle at 5-10 DEG C; carrying out continuous stirring at normal pressure for 1-1.5h to prepare the electrolyte for standby, wherein the mass ratio of the electrolyte to the electrolysis additive to the anhydrous hydrogen fluoride is equal to (5-30): (2-12) :100; (2) adding the electrolyte into an electrolysis kettle by a circulating pump, and carrying out continuous mechanical stirring at normal pressure; and (3) starting electrolysis, wherein the temperature of the electrolysis kettle is 10 DEG C below zero to 20 DEG C, and the current density is 5-50mA / cm<2>; and discharging at the bottom of the electrolysis kettle, collecting crude products, and purifying the crude products to obtain a perfluoro(methylcyclohexane) product. The method is simple in process, the product purity, the electrolysis efficiency and the corrosion resistance of equipment are high, and the operation period of the electrolysis kettle is long.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap