US785961A - Manufacture of carbon-tetrafluorid gas. - Google Patents

Manufacture of carbon-tetrafluorid gas. Download PDF

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US785961A
US785961A US17338603A US1903173386A US785961A US 785961 A US785961 A US 785961A US 17338603 A US17338603 A US 17338603A US 1903173386 A US1903173386 A US 1903173386A US 785961 A US785961 A US 785961A
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gas
carbon
anode
manufacture
tetrafluorid
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US17338603A
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John A Lyons
Edward C Broadwell
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B3/00Electrolytic production of organic compounds
    • C25B3/20Processes
    • C25B3/27Halogenation
    • C25B3/28Fluorination

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  • Our invention relates to the process of proro v ducing, by means of electrolysis, carbontetr'afluorid gas from the fiuorids of thehighly-electropositive alkaline, alkaline earth, and earth metals; potass1um,'sod1um, lithium, calcium, barium, strontium, .magnesium, manganese,
  • the object of this present invention is to so combine fiuorln gas and carbon that carbontetrafiuorid gas may be produced at a low cost and rendered.
  • a is a crucible formed'of any suitable metal in common use adapted for the purpose, which rests upon a wall 6, within which may be built a fire (not shown) fdr heating the crucible and keeping its contents inamolten condition.
  • a cover a of'earthenware or other non-conducting material, provided with a central opening d about which, on the un- ..50 (her side ofthe-cover, is attached a partitlon e,
  • a vessel f formed of a suitable non-conducting material, having an open-work bottom-g, a cover IL, provided with I a central opening t', and having an opening j above the crucible e on one side, through which any substance desired may be fed, and
  • afoundationbath wt preferably of sodium and potassium fluorid, although the fluoride of any of the alkaline, alkaline earth, or earth metals may be used, and the fluorid OaFi is named as a suitable and practical fluorid to be used, is'
  • n of charcoal, lampblack, or other suitableiearbonaceous material which surrounds the lower portion of the anode and floats upon the surface of the bath at.
  • the quantity of soft carbonaceous material added is sufiicient tovmake, with the hard carbon or graphite, a perfect anode and to protect the latter from unnecessary disintegration.
  • the electrodes are then connected in circuit to some suitable source of electrical energy, and the bath m is electrolyzed by a low-pressure current, about eight volts having been found suflicient. Thereupon the metal basesodium, calcium,
  • potassium, &c. according to the particular .fluorid that may be used will be deposited alkaline, alkaline earth, or by-product.
  • liuorin gas being liberated at the anode instantly combines with the surroundingcarbonaceous material, producing carbon ctraliuorid gas, which may be led oil through the exit or duct iv to any suitable receives. Since the combination of the lluorin with the carbon is instantaneous, there is practically no free liuorin gas in existence during the process.
  • the reaction talccs place at an approximate temperature of 1,004) ccntigradc.
  • the process of producing carbon-tetralluorid gas which consists in passing an electrolytic current through n'ietallic liuorid in a state of fusion and subjecting the fluorin liberated at the anode to a body of corbonaceous material having an allinity for fluorin immediately surrounding the anode.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electrolytic Production Of Metals (AREA)

Description

I PATENTED MAR. 28, 1905. J. A. LYONS & E. G. BROADWELL.
MANUFACTURE OF CARBON TBTRAPLUORID GAS. APPLICATION FILED SEPT 16, 1903.
alluznfow UNITED STATES Patented March 28, 1905.
PATENT OFFICE.
JOHNn. LYoNs AND EDWARD'C. BRoADWELL, or cmcaeo, ILLINOIS.
MANUFACTURE OF CARBON-TE'TRAFLUORID GAS,
SPECIFICATION forming part of Letters Patent'No. 785,961, dated March 28, 1905.
' Applicatin amuseme t 16.1903. Serial No. 173,386.
.5 (look and State of Illinois, have invented new and useful Improvements in Manufacture of Carbon-Tetrafluorid Ga s, ofwhich thefolloW- ing is a specification.
Our invention relates to the process of proro v ducing, by means of electrolysis, carbontetr'afluorid gas from the fiuorids of thehighly-electropositive alkaline, alkaline earth, and earth metals; potass1um,'sod1um, lithium, calcium, barium, strontium, .magnesium, manganese,
. 1'5 chromium, and aluminium being produced at the same time as by-products.
B le we are aware the fluorids have been used lgiiretofore as a solvent for the oxide of the metals to be obtained electrolytically and thatfluorids without such oxid or other compounds dissolved in them have been decomposed by an electric current, no attempt, to our knowledge, has beeri made to combine the fluorin gas with carbon to obtain the very val-. 2 5 I uable carbon-tetrailuorid gas.
The object of this present invention is to so combine fiuorln gas and carbon that carbontetrafiuorid gas may be produced at a low cost and rendered. commercially available for the cheap production of artificial alcohol, acetic acid, formaldehyde, &c.
For a full description of the invention and the merits thereof and also to acquire a knowledge of the means for effecting the result ref- 3 5 erence is had t o the following description, and
to the accompanying drawing, in which a sectional view of our preferred form of electrolytic cell is shown; but we do not wish to limit ourselves to an y particular form of cell or me- 4o terial.
Referring to the drawing, a is a crucible formed'of any suitable metal in common use adapted for the purpose, which rests upon a wall 6, within which may be built a fire (not shown) fdr heating the crucible and keeping its contents inamolten condition. Upon the crucible rests a cover a, of'earthenware or other non-conducting material, provided with a central opening d about which, on the un- ..50 (her side ofthe-cover, is attached a partitlon e,
of graphite or other suitable material,- not neeessarily porous, which sets down within the crucible and reaches almost to the bottom thereof, as shown. Through the opening (Z in the coverc is slipped a vessel f, formed of a suitable non-conducting material, having an open-work bottom-g, a cover IL, provided with I a central opening t', and having an opening j above the crucible e on one side, through which any substance desired may be fed, and
a branch or exit l2, also above the-crucible a,
for the escape .of -th'e gas to be formed. Through the opening i in the cover It is slipped a stick of carbon or graphite Z,'which reaches to the bottom of the vessel and forms the anode of the electrolytic cell. WVe preferably use the inner lining of the crucible (6 for the cathode, although an extra rod or plate of any "suitable materialmay be suspended therein,
if so desired.
Vile prefer to make all the elements above described circular in section onaccount of. cheapness of construction; but obviously they may be of any cross-section and our rocess be equally well conducted therebys.
in carrying out our invention afoundationbath wt, preferably of sodium and potassium fluorid, although the fluoride of any of the alkaline, alkaline earth, or earth metals may be used, and the fluorid OaFi is named as a suitable and practical fluorid to be used, is'
placed in the crucible a and kept in a molten state by means of any external heat and through the opening j is slipped a quantity n of charcoal, lampblack, or other suitableiearbonaceous material, which surrounds the lower portion of the anode and floats upon the surface of the bath at. The quantity of soft carbonaceous material added is sufiicient tovmake, with the hard carbon or graphite, a perfect anode and to protect the latter from unnecessary disintegration. The electrodes are then connected in circuit to some suitable source of electrical energy, and the bath m is electrolyzed by a low-pressure current, about eight volts having been found suflicient. Thereupon the metal basesodium, calcium,
potassium, &c., according to the particular .fluorid that may be used will be deposited alkaline, alkaline earth, or by-product. At the same time liuorin gas being liberated at the anode instantly combines with the surroundingcarbonaceous material, producing carbon ctraliuorid gas, which may be led oil through the exit or duct iv to any suitable receives. Since the combination of the lluorin with the carbon is instantaneous, there is practically no free liuorin gas in existence during the process. The reaction talccs place at an approximate temperature of 1,004) ccntigradc.
It will be noted thatsurroumling the anode with the carbonacetuis material 1/ protects the comparatively costly anode from unnecessaigv waste, and thus cheapens the cost of produc tion of the gas, besides performing its main function of furnishingcarbon to the lluorin. Also the partition 1' effectually prevents loss arising from the linorin or earlmn-tetrafluorin gas reaehing the deposited metals. The bath may be heptfusml by any suitable means, the lire being shown as one form of such means, and the electric current may be made. strong enough to lllftllltitil'lSllCil state of fusion should it be desired.
llaving thus described our invention. what we claim as new, and desire to secure by Letters Patent, is
l. The. process of producing carbon-tetralluorid gas from the liuorids of the electropositivemetals, consisting in passing of electricity through a fused bath of the lieorid of such metal in the presence of a. cathode l sub ecting the fluorin gas and an anode and liberated at the anode to the action of carbonaceous material immediatelysurrolmdingthe anode.
2. The process of producing carbon-tetra the electrol lluorid gas from the l'luo'rids of positive metals, which consists in passing a earth metals'as a l.
l l l l l l l I l I i I l l i l l i l a current current of electricity through the fiuorid of any of said metals in the presence of a suitable cathode and a carbon anode and subjecting the liuorin gas liberated at the anode to a separate body of carbonaceous material im mediately surrounding the anode, whereby carbon-tetrafiuorid will be instantly pro- -duced and any molecular fiuorin that may be created will be converted to said carbon-tetrafluorid gas, and the be deposited at the cathode.
3. The process of producing carbon-tetraiiuorid gas which consists in passing an electrolytic current through a fused bath of the finorid of one of the clectropositive metals and subjecting the tiuorin gas liberated at the anode to a bodyof carbonaceous material having an alliuity for lluorin.
4. The process of producing carlmn-tetraliuorid gas which consists in passing an electrolytic current through a fused bath of a fluorid of an electropositive metal and subjecting the iluorin liberated at the anode to a mass of carbonaceous material having an aflinitytherefor, and 'rmmediately surrounding the anode.
The process of producing carbon-tetralluorid gas which consists in passing an electrolytic current through n'ietallic liuorid in a state of fusion and subjecting the fluorin liberated at the anode to a body of corbonaceous material having an allinity for fluorin immediately surrounding the anode.
' In testimony whereof we have signed our names to this-specilication in the presence of two subscribing witnesses.
JOHN A. LYONS. EDWARD (J. BRUADWELL. Witnesses:
M A'l"l| i n w M URPHY, LADIMIR Mommy.
metals of the fluorids will
US17338603A 1903-09-16 1903-09-16 Manufacture of carbon-tetrafluorid gas. Expired - Lifetime US785961A (en)

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2924623A (en) * 1957-02-15 1960-02-09 Du Pont Process for preparing carbon tetrafluoride essentially free from other halocarbons
US2952591A (en) * 1959-02-26 1960-09-13 Union Carbide Corp Electrolytic preparation of calcium carbide
US2968599A (en) * 1958-09-02 1961-01-17 Dow Chemical Co Preparation of silicon tetrafluoride
US2970093A (en) * 1956-04-24 1961-01-31 Minnesota Mining & Mfg Process for the production of fluorinecontaining compounds
US2970092A (en) * 1956-04-24 1961-01-31 Minnesota Mining & Mfg Process for the production of fluorinecontaining compounds
US2985568A (en) * 1954-11-26 1961-05-23 Ziegler Electrolytic process for the production of metal alkyls
US2990347A (en) * 1958-06-06 1961-06-27 Du Pont Preparation of carbon tetrafluoride
US3017335A (en) * 1958-02-25 1962-01-16 Du Pont Electrolytic production of fluorocarbons and metallic sodium
US3017336A (en) * 1958-09-02 1962-01-16 Dow Chemical Co Preparation of fluorocarbon nitriles
US3032488A (en) * 1958-06-12 1962-05-01 Minnesota Mining & Mfg Electrolysis of metal fluorides in the presence of a pseudo-halogen
US3033767A (en) * 1958-09-02 1962-05-08 Dow Chemical Co Preparation of fluorocarbons
US3037919A (en) * 1958-07-22 1962-06-05 Dow Chemical Co Preparation of hexafluoroethane and higher fluorocarbons
DE1136993B (en) * 1959-05-08 1962-09-27 Du Pont Process for the production of tetrafluorocarbon along with other saturated fluorocarbons with the simultaneous production of calcium
US3114684A (en) * 1958-09-22 1963-12-17 Dow Chemical Co Preparation of halofluorocarbons
DE1222487B (en) * 1960-06-13 1966-08-11 Dow Chemical Co Process for the production of perhalogenated chloro- and bromofluoromethanes in addition to tetrafluoromethane and higher chloro- and bromofluorocarbons
DE1223355B (en) * 1960-06-14 1966-08-25 Dow Chemical Co Process for the production of hexafluoroethane in addition to tetrafluoromethane and higher fluorocarbons

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2985568A (en) * 1954-11-26 1961-05-23 Ziegler Electrolytic process for the production of metal alkyls
US2970093A (en) * 1956-04-24 1961-01-31 Minnesota Mining & Mfg Process for the production of fluorinecontaining compounds
US2970092A (en) * 1956-04-24 1961-01-31 Minnesota Mining & Mfg Process for the production of fluorinecontaining compounds
US2924623A (en) * 1957-02-15 1960-02-09 Du Pont Process for preparing carbon tetrafluoride essentially free from other halocarbons
US3017335A (en) * 1958-02-25 1962-01-16 Du Pont Electrolytic production of fluorocarbons and metallic sodium
US2990347A (en) * 1958-06-06 1961-06-27 Du Pont Preparation of carbon tetrafluoride
US3032488A (en) * 1958-06-12 1962-05-01 Minnesota Mining & Mfg Electrolysis of metal fluorides in the presence of a pseudo-halogen
US3037919A (en) * 1958-07-22 1962-06-05 Dow Chemical Co Preparation of hexafluoroethane and higher fluorocarbons
US3017336A (en) * 1958-09-02 1962-01-16 Dow Chemical Co Preparation of fluorocarbon nitriles
US2968599A (en) * 1958-09-02 1961-01-17 Dow Chemical Co Preparation of silicon tetrafluoride
US3033767A (en) * 1958-09-02 1962-05-08 Dow Chemical Co Preparation of fluorocarbons
US3114684A (en) * 1958-09-22 1963-12-17 Dow Chemical Co Preparation of halofluorocarbons
US2952591A (en) * 1959-02-26 1960-09-13 Union Carbide Corp Electrolytic preparation of calcium carbide
DE1136993B (en) * 1959-05-08 1962-09-27 Du Pont Process for the production of tetrafluorocarbon along with other saturated fluorocarbons with the simultaneous production of calcium
DE1222487B (en) * 1960-06-13 1966-08-11 Dow Chemical Co Process for the production of perhalogenated chloro- and bromofluoromethanes in addition to tetrafluoromethane and higher chloro- and bromofluorocarbons
DE1223355B (en) * 1960-06-14 1966-08-25 Dow Chemical Co Process for the production of hexafluoroethane in addition to tetrafluoromethane and higher fluorocarbons

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