Production of CC12F2, Ib./cu. ft. 50 70 90 reactor/hr. 15 44 440tion, the rate of production over a longer period would be somewhat lower, depending upon the fraction of the total time spent in regeneration.The recycling of triehlorofluoromethane has been shown to be feasible in process III. This variation of the process requires essentially no change in conditions, causes no appreciable change in yield or utilization of hydrogen fluoride, and causes a slight increase in the rate of production of dichlorodifluoromethane.
fluorination of a hydrocarbon. Much less heat is evolved per mole of fluorinated product so that reaction control is less critical.The greater thermal stability of fluorocarbons as compared to hydrocarbons permits the use of higher boiling feed materials for reaction without thermal cracking; this corresponds to fluorocarbon products of considerably higher molecular weight. All the reacted fluorine appears as carbon fluoride, and the absence of hydrogen fluoride as a product permits the use of simpler isolation procedures. Ethylenic bonds in fluorocarbons are easily attacked by fluorine under moderate conditions of reaction, in contrast to the last few hydrogens in a hydrofluorocarbon which became increasingly difficult to replace. This makes the complete fluorination of olefins relatively easy.
VAPOR-PHASE FLUORINATION WITH COBALT TRIFLUORIDEThe vapor-phase method for indirect fluorination was developed as a means of saturating perfluoro-olefins without dimerization. The experiments were principally with cobalt trifluoride. This salt is easily regenerated from cobalt trifluoride with free fluorine and does not form low melting fluoride complexes between the lower and higher valent salts as do the silver fluorides. Most of the runs were made with CsFi-2, the thermal dimers of perfluorobutadiene.The experimental setup was very similar to that used by Fowler (4) in extensive vapor-phase cobalt trifluoride work with hydrocarbons. The C3F12 was introduced dropwise as a liquid and vaporized into a rotating nickel oven containing a 200-250% excess of cobalt trifluoride heated to approximately 180-200°C. by gas flames. After each run the cobalt trifluoride was regenerated by passing in free fluorine.The following fractions were obtained from a typical run using 187 grams of CsFu passed through the oven at 200°± 5°C. at a rate of 12.5 grams per hour with a 2-to-l nitrogen-to-CsFi2 dilution: (1) 7.7 grams, b.p. 78-88°C .; (2) 26,0 grams, b.p. 88-92°;(3) 83.3 grams., b.p. 92-94°; Í4) 32.9 grams, b.p. 94-98°; (5) 11.1 grams, b.p. 98-104 °; (6) 23.5 grams, b.p. 104-106°; (7) 2.3 grams of residue. The average molecular weight of fraction 3 was 397 and of fraction 6, 415, as determined by vapor density.
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