Massachusetts Institute of Technology

The United States of America As Represented by the Department of Energy

Other

Electric Power Research Institute Incorporated

University of Tennessee Research Foundation

James L Adcock

Richard J Lagow

Norma J Maraschin

Loucas G Christophorou

Marshall O Pace

Shoji Inoue

Ehrengard B Renk

This invention discloses novel compounds 3-hydryl-F-oxetane and 3,3-dihydryl-F-oxetane, for use as refrigerants or solvents. The compounds will serve as close replacements for CFC's R-11 and R-113.

3-hydryl-F-oxetane and 3,3-dihydryl-F-oxetane compounds useful as

An apparatus for aerosol direct fluorination is disclosed in which a material to be fluorinated is formed into an aerosol prior to fluorination by introducing a vapor stream of the material to be fluorinated centrally into converging flows of carrier particles suspended in a gas and condensing the vapor onto the particles. Fluorine is contacted with the aerosol in an elongated fluorination reactor having microporous walls providing a substantially continuous influx of fluorine-containing gas which creates an increasing fluorine concentration gradient as the aerosol moves through the reactor and provides a barrier to prevent contact of the aerosol with the microporous walls. A photochemical stage includes an elliptical reflector with a light source of one focus and a flow of aerosol and fluorine at the others.

High efficiency apparatus for aerosol direct fluorination

A contaminant trap for a gas-insulated electrical conductor is provided. A resinous dielectric body such as Kel-F wax, grease or other sticky polymeric or oligomeric compound is disposed on the inside wall of the outer housing for the conductor. The resinous body is sufficiently sticky at ambient temperatures to immobilize contaminant particles in the insulating gas on the exposed surfaces thereof. An electric resistance heating element is disposed in the resinous body to selectively raise the temperature of the resinous body to a molten state so that the contaminant particles collected on the surface of the body sink into the body so that the surface of the resinous body is renewed to a particle-less condition and, when cooled, returns to a sticky collecting surface.

Contaminant trap for gas-insulated apparatus

Electrical breakdown of a gas insulator in high voltage apparatus is preved by placing an electrical insulative coating on contaminant particles in the gas insulator.

Method for minimizing contaminant particle effects in gas-insulated

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 perfluorooethyl 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.

Cryogenically controlled direct fluorination process, apparatus and

A method and apparatus for improving direct fluorinations are disclosed in which the material to be fluorinated is formed into an aerosol prior to fluorination.

Aerosol direct fluorination method and apparatus

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.

Perfluorinated functionalized materials are disclosed which are prepared by simultaneous perfluorination and functionalization. A wide variety of materials can be used including polymers and other branched or straight chain hydrocarbons. The material to be perfluorinated is placed in a direct fluorination apparatus and a mixture of fluorine and oxygen is passed over the material using La-Mar direct fluorination techniques. With materials such as polyethylene or polypropylene, pendant alkyl groups are converted to either acid fluoride groups or perfluoroalkyl groups, with the exact ratio of each being dependent upon the specific fluorine-to-oxygen ratio used.

Perfluorinated functionalized materials

An apparatus and process useful in direct fluorination of a variety of compositions, as well as the fluorinated compositions themselves. The apparatus comprises a cryogenic zone reactor, such as a packed column reactor, 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. The direct fluorination process is carried out in the reactor as described above. At least the first zone of the reactor is chilled to a temperature below the freezing point of the reactant to be fluorinated. The reactant is then introduced into the reactor wherein it condenses upon a suitably provided fluorination surface, such as copper column packings. A mixture of fluorine gas and an inert gas, with the fluorine gas initially comprising a very small percentage of the mixture, but gradually increasing as fluorination proceeds, is then introduced into the reactor. After some degree of fluorination has been achieved in the first zone, it is allowed to warm whereas other zones in the reactor are cooled. The resulting temperature gradients cause the partially fluorinated materials to volatilize and move along the column. As the volatilized, partially fluorinated materials enter the subsequent chilled zone, they condense on a fresh fluorination surface and are further fluorinated. The temperature gradients are repeated as necessary to achieve the degree of fluorination desired. 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 are disclosed. One synthesis comprises producing perfluoroethyl acetate by direct fluorination using a cryogenic zoner reactor, followed by hydrolysis of perfluoroethyl acetate. A second synthesis comprises fluorinating an acyl chloride followed by hydrolysis of the resulting acyl fluoride.

Growing community of inventors

Knoxville, TN, United States of America

James L Adcock