ChemicalBook CAS DataBase List Nonafluorobutanesulfonyl fluoride

Nonafluorobutanesulfonyl fluoride synthesis

9synthesis methods

Product Name:Nonafluorobutanesulfonyl fluoride
CAS Number:375-72-4
Molecular formula:C4F10O2S
Molecular Weight:302.09

Perfluorobutylsulfonyl fluoride is a perfluorinated compound mainly used in the synthesis of fluorocarbon surfactants, fluorinated pesticides, dyes, polycarbonate processing dispersants, etc. Its synthesis method is that butylsulfonyl chloride as raw material, conducts a fluorine replacement reaction on butylsulfonyl chloride such as potassium chloride to prepare butylsulfonyl fluoride, and then conducts a replacement reaction with anhydrous hydrogen fluoride under nitrogen conditions to generate Perfluorobutylsulfonyl fluoride.

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Yield:375-72-4 95.32%

Reaction Conditions:

with hydrogen fluoride at -35 - 15;Large scale;

Steps:

1.1-3.1 Synthesis of perfluorobutanesulfonyl fluoride:

Put 22.23Kg n-butylsulfonyl chloride into a 100L stainless steel reactor, 7.27Kg potassium fluoride, 25Kg acetonitrile and 0.25Kg tetrabutylammonium bromide. The temperature was raised to 68°C with stirring, and the reaction was stirred for 2h. At the end of the reaction, stop stirring and cool to room temperature, filter the side reaction potassium chloride in the electrolytic cell with a volume of 180L, nickel as the anode and iron as the cathode, in a Simons electrolytic cell with an anode plate area of 25000cm2; open the cooling brine of the coil condenser in the electrolytic cell , The tank temperature is reduced to -10 ~ -5 ; recovery of acetonitrile solvent distillation to obtain 20Kg n-butylsulfonyl fluoride ether. Add 140Kg of anhydrous hydrogen fluoride. Slowly add 20Kg of n-butylsulfonyl fluoride from the metering tank to the electrolytic tank, and control the temperature at 12%-15%, and the electrolyte temperature at 515; the silicon controlled rectifier delivers the voltage to the electrode plate group in the tank 5.0V8.5V direct current; the current is controlled at 450A480A, the current density is between 0.017 A/cm20.018A/cm2, the temperature in the cell is maintained at 515; the gas emitted during the electrolysis process passes through Condenser (condenser temperature is controlled at -35-30) buffer; then passes through a pressurized column to keep the system at a pressure of 0.400.42kgf/cm2; Then, the gas is vented; the electrolytic product is insoluble in the electrolyte and sinks in the lower layer of the electrolytic tank, and the crude product is discharged, so it must be discharged after a certain period of time; the discharged electrolytic product is the crude perfluorobutylsulfonyl fluoride; put it into the distillation kettle; , Collect the fraction at 64; Obtained 40.3Kg, yield 95.32%, content 99.02%.

References:

CN112174859,2021,A Location in patent:Paragraph 0022; 0024; 0028; 0032