Cryogenically controlled direct fluorination process, apparatus and products resulting therefrom
AssigneeMassachusetts Institute of Technology
InventorsRichard J. Lagow, James L. Adcock, Norma J. Maraschin
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AssigneeMassachusetts Institute of Technology
InventorsRichard J. Lagow, James L. Adcock, Norma J. Maraschin
Estimating the term…
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.
A direct fluorination process for fluorinating a reactant with elemental fluorine, comprising:
A direct fluorination process comprising contacting, at a first fluorination site, a source of elemental fluorine and a reactant to be fluorinated at a temperature below the condensation point of said reactant and in the presence of fluorination surface capable of removing heat generated during fluorination whereby said reactant is partially fluorinated, warming said first fluorination site to a temperature at which said partially fluorinated reactant volatilizes whereby it is volatilized and passes to a fresh fluorination site, lowering the temperature of said fresh fluorination site below the condensation point of said partially fluorinated reactant and contacting the partially fluorinated reactant, at said fresh site, with a source of elemental fluorine in the presence of a fluorination surface capable of removing heat generated during fluorination.
Dependencies are inferred from the claim text.