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Preparation method of perfluorohexane

A fluorohexane and electrolytic fluorination technology, applied in the field of fluoroalkanes, can solve the problems of increased leakage risk of hydrogen fluoride, high pressure of the electrolytic fluorination system, and increased difficulty in purification and separation, etc. Long cycle and the effect of maintaining concentration

Pending Publication Date: 2018-01-19
ZHEJIANG JUSHENG FLUOROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the conductive additives participate in the electrolytic fluorination reaction and generate perfluoroamine or polyfluoroamine impurity compounds, which increases the difficulty of purification and separation
The disadvantage is that the pressure of the electrolytic fluorination system is relatively high, and the corrosive medium hydrogen fluoride increases the risk of leakage
The disadvantage is that there are many steps, the process is complicated, and the yield of each step is low, which makes the whole process uneconomical

Method used

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  • Preparation method of perfluorohexane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Add 35kg of hexafluoropropylene dimer, 65kg of AHF and 1.0kg of sodium fluoride into the electrolyte preparation tank respectively, stir at 5°C and 50rpm for 30min to obtain the electrolyte, and set aside;

[0033] (2) Put the electrolyte obtained in step (1) into the water removal tank for electrolytic dehydration. The initial current of electrolytic dehydration is 10A. After electrolytic dehydration starts, the current is increased at a rate of 10A / 2h. When the current reaches 60A When the electrolytic dehydration is finished, the electrolyte solution after dehydration is obtained for subsequent use;

[0034] (3) The dewatered electrolyte solution obtained in step (2) is continuously added to the electrolytic cell (the anode material is 6# nickel, and the cathode material is carbon steel), and the electrolytic fluorination reaction is carried out at a temperature of 19°C under normal pressure , the electrolysis voltage is controlled to be 6V, and the working curre...

Embodiment 2

[0037] (1) Add 10kg of hexafluoropropylene dimer, 50kg of AHF and 0.5kg of sodium fluoride into the electrolyte preparation tank respectively, stir at 15°C and 80rpm for 5min to obtain the electrolyte, and set aside;

[0038] (2) Put the electrolyte obtained in step (1) into the water removal tank for electrolytic dehydration. The initial current of electrolytic dehydration is 10A. After electrolytic dehydration starts, the current is increased at a rate of 5A / 2h. When the current reaches 50A When the electrolytic dehydration is finished, the electrolyte solution after dehydration is obtained for subsequent use;

[0039] (3) The electrolyte obtained in step (2) after water removal is continuously added to the electrolytic cell (the anode material is 6# nickel, and the cathode material is carbon steel), and the electrolytic fluorination reaction is carried out at a temperature of 20 ° C and normal pressure , control the electrolysis voltage at 5V, working current 60A, the gas pha...

Embodiment 3

[0042] (1) Add 50kg of hexafluoropropylene dimer, 80kg of AHF and 0.3kg of sodium fluoride into the electrolyte preparation tank respectively, stir at 10°C and 70rpm for 10min to obtain the electrolyte, and set aside;

[0043] (2) Put the electrolyte obtained in step (1) into the water removal tank for electrolytic dehydration. The initial current of electrolytic dehydration is 8A. After electrolytic dehydration starts, the current is increased at a rate of 7A / 2h. When the current reaches 52A When the electrolytic dehydration is finished, the electrolyte solution after dehydration is obtained for subsequent use;

[0044] (3) The electrolyte obtained in step (2) after water removal is continuously added to the electrolytic cell (the anode material is 6# nickel, and the cathode material is carbon steel), and the electrolytic fluorination reaction is carried out at a temperature of 15°C under normal pressure , control the electrolysis voltage at 7V, working current 30A, the gas p...

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Abstract

The invention discloses a preparation method of perfluorohexane. The preparation method comprises the following steps that (1) by weight, hexafluoropropylene dimer, anhydrous hydrogen fluoride and electrolytic addition agents are prepared into an electrolyte for standby application; (2) the electrolyte is subjected to electrolytic dehydration for standby application; and (4) the dehydrated electrolyte is continuously added into an electrolytic bath to be subjected to electrofluorination reaction, a gaseous product obtained after electrolysis is condensed and rectified, and thus a perfluorohexane product is obtained. The advantages that the process is simple, the cost is low, the current efficiency is high, the operation cycle is long, and the product quality is stable are achieved.

Description

technical field [0001] The invention relates to the technical field of fluoroalkane, in particular to a preparation method of perfluorohexane. Background technique [0002] Perfluorohexane, CAS: 355-42-0, molecular formula: C 6 f 14 , structural formula: CF 3 CF 2 CF 2 CF 2 CF 2 CF 3 , Molecular mass: 338.04, boiling point: 51-59°C, density at 25°C is 1.66-1.7g / ml, Chinese name: Tetrafluorohexane or perfluorohexane or perfluoro-n-hexane, is a colorless and transparent Liquid, mainly used as heat medium and dielectric. [0003] The preparation of perfluorinated compounds mainly includes two methods: fluorine gas fluorination and electrolytic fluorination. Fluorine gas fluorination prepares perfluorohexane, and the raw material that adopts is hexafluoropropylene dimer ((CF 3 ) 2 CFCF=CFCF 3 ), the catalyst is CoF 3 or CuF 2 , gas-phase fluorination and liquid-phase fluorination processes can be adopted, but fluorine gas fluorination involves fluorine gas preparat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/08C25B3/28
Inventor 任慧芳朱洪吉余考明陈伟峰王志辉李彬
Owner ZHEJIANG JUSHENG FLUOROCHEM
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