Process for the preparation of pure, saturated perfluoroalkane-1

Details Process for the preparation of pure, saturated perfluoroalkane-1 Process for the preparation of pure, saturated perfluoroalkane-1

1981-11-09

1983-08-23

Niebling, John F.

Chemistry of carbon compounds

Miscellaneous organic carbon compounds

C-metal

562541, 562605, C09F 700, C11C 300

Patent

active

044003250

ABSTRACT:
Saturated perfluoroalkane-1-carboxylic acids having 6 to 14 C atoms are prepared by reacting the corresponding 1-iodoperfluoroalkanes at temperatures of 100.degree. to 180.degree. C. with fuming sulfuric acid containing 15 to 45% by weight of dissolved sulfur trioxide. The two liquid phases which are formed are separated. The lighter phase is mixed with 0.3 to 6% of its weight of water and is distilled at a pressure of 0.3 to 100 kPa. The heavier phase is mixed with 0.7 to 1.5 moles of water per mole of sulfur trioxide employed and is cooled to 0.degree. to +30.degree. C. and the precipitated iodine is filtered off. After the addition of sulfur trioxide, the liquid filtrate can be re-used.
Perfluoroalkan-1-oic acids are obtained in a high state of purity and the bulk of the iodine is recovered in the elementary form.

REFERENCES:
patent: 2904567 (1959-09-01), Barnhart
patent: 3351644 (1967-11-01), Hauptschein

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