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Method for preparing branched perfluorohexane

A technology of perfluorohexane and dodecafluorodihydrohexane is applied in the field of preparing branched perfluorohexane, and can solve the problems of undisclosed conversion rate or yield, corrosion of electrolytic cells, pipelines and related equipment, fluorination Reagents are difficult to obtain and other problems, to achieve the best conversion rate of raw materials, high hydrogen replacement reaction efficiency, and improved yield per unit time.

Active Publication Date: 2019-04-19
浙江佳汇新材料有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Frohn, Hermann-Josef et al. reported (Journal of Fluorine Chemistry, 131 (10), 1000-1006; 2010) that perfluoroalkenes were fluorinated by perfluoroalkyl iodide hexafluoride, and 100% were converted into perfluoroalkanes, but the Fluorinated reagents are very difficult to obtain
[0008] Chinese patent application CN107604378A discloses a method for preparing perfluorohexane, in which hexafluoropropylene dimer, anhydrous hydrogen fluoride and electrolytic conduction additives are prepared into an electrolyte, which is continuously added to an electrolytic cell for electrolytic fluorination, wherein the electrolytic The conduction aid is potassium fluoride or sodium fluoride. The process is simple and the current efficiency is high, but the specific conversion rate or yield is not disclosed. The disadvantage is that long-term operation will cause corrosion of electrolytic cells, pipelines and related equipment

Method used

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  • Method for preparing branched perfluorohexane
  • Method for preparing branched perfluorohexane
  • Method for preparing branched perfluorohexane

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: the preparation of hydrogenation catalyst

[0032] The chloride of Rh, Pd, Ni or Zn is dissolved in the hydrochloric acid aqueous solution according to metal weight ratio as shown in Table 1, and the metal weight percent content is 8%, and the concentration of hydrochloric acid is 11%; After 48 hours, it was drained, dried at a low temperature of 130°C, and calcined at 500°C to obtain the hydrogenation catalyst.

Embodiment 2～8

[0033] Embodiment 2-8: Synthesis of dodecafluorodihydrohexane

[0034] Catalytic hydrogenation of hexafluoropropylene dimer to prepare dodecafluorodihydrohexane. The test was carried out in a fixed-bed reactor. The reactor was a stainless steel tube with an inner diameter of 20mm and a length of 800mm, filled with 150ml of hydrogenation catalyst, and the reaction temperature was 150°C. The operating pressure is 1MPa, and the space velocity of the raw material hexafluoropropylene dimer is 48h -1 , the flow ratio of hydrogen to hexafluoropropylene dimer is 8.

[0035] The synthetic product was analyzed and tested by gas chromatography, and the product was collected by low temperature condensation. The reaction analysis results are shown in Table 1.

[0036]

[0037]

[0038]

Embodiment 9

[0039] Embodiment 9: Synthesis of branched perfluorohexane

[0040] Put 2.8kg of anhydrous hydrofluoric acid in a 5L small electrolytic cell equipped with a -40°C reflux condensing device and necessary auxiliary agent tanks, and remove water by energizing it with nitrogen to maintain a slight positive pressure until the current drops to 0.5mA , voltage 5.5V, then add 14g of dimethyl disulfide, add 280g of dodecafluorodihydrohexane prepared in Example 3, the current gradually rises to 412mA, maintain the voltage at 5.5-5.8V, and the current density of the anode plate is 40mA / cm 2 The continuous electrolysis time is 72 hours, and the temperature of the electrolyte is kept at around 21°C. The layered material at the bottom of the electrolytic cell is recovered, and 255g of perfluorohexane is obtained through steps such as alkali washing, water washing and rectification.

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Abstract

The invention discloses a method for preparing branched perfluorohexane. The method includes the following steps: (1) reacting a hexafluoropropene dimer adopted as a raw material to a catalytic hydrogenation reaction in a reactor to synthesize dodecafluorodihydrohexane; and (2) introducing the dodecafluorodihydrohexane prepared in the step (1), anhydrous hydrofluoric acid and conductive auxiliarydimethyl disulfide into an electrolytic tank and preparing the branched perfluorohexane by Simons electrochemical fluorination. The method of the invention uses the perfluoropropylene dimer as the rawmaterial, performs the hydrogenation to obtain the saturated hydrofluoroalkane, and then performs electrochemical fluorination to replace the hydrogen to obtain the branched perfluoroalkane. The method for preparing the branched perfluorohexane has the advantages of high hydrogenation conversion rate and good selectivity, and so the electrochemical fluorination efficiency is significantly improved and the production cost is greatly reduced.

Description

technical field [0001] The invention relates to a method for preparing perfluoroalkane, in particular to a method for preparing branched perfluorohexane. Background technique [0002] Branched perfluorohexane is an important fine chemical. Because it is a perfluorinated saturated alkane, it has excellent chemical inertness and physiological inertness, making branched perfluorohexane widely used in high-end cleaning, medicine and special fire extinguishing. Has a wide range of uses. [0003] U.S. Patent US3950235A discloses a method for preparing branched perfluoroalkanes by Simons electrochemical fluorination of branched perfluoroalkenes, wherein the branched perfluoroalkenes come from the oligomerization of perfluoropropylene and perfluoroethylene, and the voltage of electrochemical fluorination is 4 ~6.6 volts, temperature 0~20℃, fluorinating reagent is anhydrous hydrogen fluoride, the yield of main product is 75~78%, but due to the poor compatibility and low conductivity...

Claims

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Application Information

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IPC IPC(8): C25B3/08C07C17/354C07C19/08B01J23/89C25B3/28
CPCC07C17/354B01J23/892B01J23/8953C25B3/28
Inventor 李家才王亮何邦友
Owner 浙江佳汇新材料有限公司
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