Cryogenically controlled direct fluorination process, apparatus

Details Cryogenically controlled direct fluorination process, apparatus Cryogenically controlled direct fluorination process, apparatus

1976-06-23

1981-07-28

Love, Ethel G.

Organic compounds -- part of the class 532-570 series

Organic compounds

Chalcogen in the nitrogen containing substituent

2603406, 26034816, 26034848, 260543F, 260694, 560129, 562507, 562596, 568411, 568615, 568842, 564118, 564121, 570130, 570134, C07D26530, C07B 900

Patent

active

042811198

ABSTRACT:
An apparatus and process useful in direct fluorination of a variety of compositions, as well as the fluorinated compositions themselves, are disclosed.
The apparatus comprises a cryogenic zone reactor, such as a packed column reactor, suitably divided into a plurality of independently controllable cryogenic temperature zones. Means are also provided to introduce a reactant to be fluorinated as well as to introduce a mixture of fluorine gas and an inert gas.
New fluorinated compounds are also disclosed. These include: perfluoro-2-methoxyethyl ether; perfluoro-1,4-dioxane; perfluoro-2,5-diketohexane; perfluorohexamethylethane; and monohydropentadecafluoroadamantane.
Additionally, new syntheses for trifluoroacetic acid, a commercially significant bulk chemical, are disclosed. One synthesis comprises producing perfluoroethyl acetate by direct fluorination using a cryogenic zone reactor, followed by hydrolysis of perfluoroethyl acetate. Two moles of the acid are produced for each mole of ester. A second synthesis comprises fluorinating an acyl chloride followed by hydrolysis of the resulting acyl fluoride.

REFERENCES:
Maraschin et al., (I), Journ. Amer. Chem. Soc., 94, 24, Nov. 29, 1972, pp. 8601-8603.
Maraschin et al., (II), Inorg. Chem., vol. 12, No. 6, Jun. 1973, pp. 1458-1459.
Maxwell et al., Amer. Chem. Soc., 82, 22, Nov. 1960, pp. 5827-5830.

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