US2944950A - Operation and discharge of sodium cells - Google Patents

Operation and discharge of sodium cells Download PDF

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Publication number
US2944950A
US2944950A US685902A US68590257A US2944950A US 2944950 A US2944950 A US 2944950A US 685902 A US685902 A US 685902A US 68590257 A US68590257 A US 68590257A US 2944950 A US2944950 A US 2944950A
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United States
Prior art keywords
sodium
cell
riser pipe
conduit
transfer
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US685902A
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English (en)
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Glenn O Hayes
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Ethyl Corp
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Ethyl Corp
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Priority to US685902A priority Critical patent/US2944950A/en
Priority to DEE16453A priority patent/DE1129714B/de
Priority to FR1210355D priority patent/FR1210355A/fr
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Publication of US2944950A publication Critical patent/US2944950A/en
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/005—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells for the electrolysis of melts
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06—Operating or servicing

Definitions

  • This invention relates to the manufacture of alkali .-metals. More specifically, the invention relates to a new .technique in the preparation of alkali metals, especially sodium, by the electrolysis of fused salts, and to the discharge and delivery of the sodium to subsequent operations.
  • sodium is made: by theelectrolysis of afused .bath consisting of sodium chloride and calcium chloride. This operation is carried out in cells ofthe Downs type, originally disclosed in'the Downs I patent, U'.-S. 1,501,756.
  • the characteristic of the Downs cell operation was the employment of a bottom mounted anode of carbonaceous material, surrounded by-a cylindrical type cathode, forming an annular electrolysis zone .between these two members.
  • This rising sodium stream was received by an inyerted trough or collector, which in turn was connected to an upwardly rising riser pipe projecting from the 'top of the cell.
  • This riser pipe provided for the flow of the, sodium above the top level of the electrolyte bath, into the exterior of the cell under the influence of the greater specific gravity of the fused bath than the molten alkali metal product.
  • a portable transfer vessel is connected to each sodium cell and isprovided to accumulate the product of such a cell for a' period of, say, 24 hours. At the termination of such a period, the transfer vessel is moved adjacent the sedimentation-filtration apparatus of the Gilbert device, and emptied, and later is returned for reattachment to the sodium cell.
  • the transfer vessel is moved adjacent the sedimentation-filtration apparatus of the Gilbert device, and emptied, and later is returned for reattachment to the sodium cell.
  • each cell was provided with an intermediate individual hold-up tank. This tank, or receiving drum.
  • Anobject of the present invention hence is to provide an improved method and apparatus for the receipt of and delivery of sodium from a sodium cell, and for facilitating the delivery thereof to subsequent filtration or sedimentation operations or other purification steps. Another object is to provide a method of operation of a sodium cell, and particularly an improved delivery and discharging technique, which entirely eliminates any intermediate storage treatment of the cell product. A' further object is to provide an improved delivery and transfer technique characterized by much less exposure to contaminating atmospheres or vapors than heretofore possible. A further object is to provide new and novel apparatus for accomplishing the improved delivery operation. Other objects will appear below.
  • the invention includes transfer of the sodium product directly through a transfer conduit to a transport vessel from the riser pipe with no intermediate storage. This is continued until the transport vessel is substantially fully charged, and then the said transfer is interrupted for aninterval and the cell production is accumulated in the cell collector trough for a limited but appreciable period. The accumulation approaches but does not exceed the capacity of the cell collector trough. The accumulation period is followed by reinstatement of the dircet transfer to the transport vessel. During the cumulation period cited above, the transport vessel is removed and emptied to subsequen sedimentation and filtering apparatus.
  • a reheating operation accompanies the direct transfer of the sodium to the transport vessel, the reheating being generally of the order of magnitude of from 25 to F. above the temperature at which the sodium is made available by the riser pipe.
  • a small but positive flow of inert gas is passed concurrently with the sodium product through the transfer conduit, and during the periodic cumulation intervals, a positive pressure of inert gas is maintained on the top of the column of sodium in the riser pipe.
  • FIG. 1 a cell and supplemental equipment arranged for the process of the present invention -iszshown.
  • ilfihearnajor components of thecelldncludem acell SlI1l-.2fl,ljI1ithB form ioftailargetankor'vessel, the walls and bottom thereof being composed of :a refractory material with :a .steel external shell.
  • the anode Surrounding amajor portion of :the anode is:a.cylindrical cathode 22, h-aving cathodearms :or lug arms projecting from thesides thereof and -'through the walls :of the cell.
  • the cathode iselectrically insulated from the cell shell.27 :by means :of appropriate insulating refractory 24 packedaround the cathode arms 23.
  • the :c'athode arms make external connection to bus bars 25 25. :to complete the electrical circuit and an annular electrolysis .zone 32 is .thus formed by the anode-cathode configuration.
  • a metal assembly including in chlorine dome 29 and a collector 11.
  • the collector 11 is an inverted channel corresponding generally in plan configuration to the annular -'electrolysis. space.32.
  • the chlorine 'dome '29 corresponds :in general fplan configuration to the anode 2-1. .
  • a diaphragm 33 is suspended from the chlorine tdome andcollectorassemhlyand aids in directing upward flow of sodium metal and chlorine gas as these products arereleased at the cathode :and anode respectively. 7
  • theriser pipe Connecting to't the collector channel '11is a riser pipe 121 which .extends'vertically :an. appreciable distance above the top'devel .34 .of dire cell bath. for most of this pro- ,jectingidistance, theriser pipe is fitted with extended external .fins 20 which aid in heat dissipation to the atmosphere. 'In most cases, theriseripipe is fitted with 'a :ticklermechanism :17, this being a device for dislodging calcium particles which precipitate on the walls of the of the :riser pipe.
  • the riser'pipe maybe a'uniformcross sectionconduit, .Ibllt i-npreferred apparatus for theinven :tion, an enlarged section .12 comprises "the top terminus of the conduit.
  • the transfer line .13 connects to the riser pipe periphery and provides a continuous channel from the :riserpipeto the'transport vessel.
  • the transfer line 13 is maintained in permanent *fixe'd alignment .by the above mentioned opening connection, and "-nsually'by means of a .brace member .18 connecting the transfer i-line 13' and the riser pipe 1 2.
  • Nearthe bottom end ofthe transfer line 13 is a valve 14, preferably of the plug type.
  • an enlarged crosssection 1-2. conduit surmounts, or comprises the upper portion of the riser pipe.
  • the transferiline 13in such installations'joins the riser pipe assembly at the horizontal shoulder 16 which-connects the enlarged section 12 to the riser pipe proper.
  • thetransfer line 13 connecting in this man ner establishes an elliptical opening (notshown) in the shouiderof the enlarged section.
  • the horizontal dispositionof this opening provides certain advantagesexpl'ained hereafter.
  • .Afurther feature of the *presentenibodiment is an "extension segment 13 having a cap 30 thereon. This segment is ea pipe section closely aligned to form a projected extension of the transferline 13. The purpose of this extensionsection is to allow insertion of a closely .fitting rod, through the extension section 13 and thence through the transfer line for rod out cleaning when necessary.
  • the direct transfer operation is accompanied by a reheating operation.
  • the 'sodium' is heated from .25 to 75" -F. abovethe temperature at which the sodium is delivered at the top of the riser pipe, which is usually about 225 to -250 F.
  • the reason for the efficacy of the heating is not fully understood, inasmuch as it would be expected that merely maintaining the 'temperatureconstant "would assure efiective and continuous flow.
  • the heating can be accomplished by any effective means, for example, by electric strip heaters adjacent the transfer line 13, or by induction heating.
  • the :most preferred embodiments :of the process also include the ,step "of passing :abdry .inert gas through the 'upper part :of the riser zpipe, through the transfer line and into the transport container 28.
  • .clry Ordinarily, .clry
  • nitrogen is themost-economicalinert gas, :and may bein-' troduced by an opening or nozzle (not shown) into the top of "the riser .pipe.
  • 'thecap 30 on the extension .13 can be :a nozzle for a supply-of nitrogen.
  • apositiver-pressure .ofsthetgas is maintainedat the-top of the 1rliserpipe, .but owing to the closure of the transfer line, 'thereJis substantially :no flow of gas.
  • the sodium cell is supported in an opening in the door 19 (of .the shop by support means no't s'hown. Positioned adjacent the cell during the largest segment of operation of the present invention is the transport 'vesse'l 2-8..
  • the transport vessel .28 is, generally, a cylindrical @steel dmrn, provided with heating elements for electrical heating if desired, and usually having appropriate external insulation material.
  • Thenozzle 41 is provided with a half section 15 of the quick connecting coupling, this "being .in correct alignment for matching engagement with .the segment 15 of the quick connecting coupling attached to the transfer line 13.
  • the transport vessel is put :in the position indicated with the termini of the 'no'zzle'41 and the transfer line 13 in abutting position and connection is made by thecouplingelements 15 15 .
  • the flow of-sodium from 111611 861 pipe is allowed to continue without interruption until the vessel has been substantiallyfilled.
  • a stream of dry, inertgas such' as nitrogen or helium.
  • the plug valve -14 isclosed and the coupling elements 15 .15 are disconnected and the transport vessel is removed for-discharging to subsequent sedimentation and filtering operations,., for discharge of the sodium thereto.
  • electrolysis continues and the quantity of sodiunrzremaining within the cell increases. .
  • the production during this period is cumulatedin the .riser ,pipe and in the collector channel 11.
  • the transport vessel is necessarily away from the indicated station for a period ofifrom .15 minutes to -2' hours, and during this period the-collector channel ILpIusithe avail-able i'heightfin the riserpipe suthcient to accommodate full production of sodium in that period.
  • the main portions of the coupling-mechanism include a sleeve 41, a movable member 44 having a spherically shaped segmental seat 45 at the upper extremity thereof.
  • the movable member 44 is generally a short cylindrical conduit adapted to slide snugly within the sleeve member 41.
  • the sleeve member 41 has cut into its wall a cam or slot 42.
  • a pin 46 is affixed to the movable member 44 and has a threaded portion for mounting and engagement of a nut 47. It is seen that rotative movement of the member 44 will result in vertical movement thereof. Upon attainment of any desired vertical positioning, retention thereof is attained by fastening the nut 47 to clamp the movable member 44 in place.
  • Ending the transfer conduit 13 is a short and usually vertical-1y disposed segment 51, this segment having at its lower end a spherical face 52 corresponding in proportions to the spherical seat 45 of the movable member 44.
  • the transport vessel 28 is positioned in the appropriate location adjacent a cell, and the movable member 44 is rotated to cause its upward movement and snug engagement with the spherical face 52 of the terminus of the transfer line '13.
  • this structure provides rapid engaging means for connecting the transport vessel to the delivery means of a cell installation.
  • the use of spherical mating surfaces 45, 52 provides for close, contact and compensation for normal variations in alignment of the transfer line 13, irregularities in the floor of the building structure, etc.
  • Example 1 To demonstrate the benefits of the method of the present invention, a series of cell installations, including the transport and transfer apparatus described above and shown in Figures 1 and 2 were operated for an extended period. During the operation the sodium was heated from about 240 F., the discharge temperature from the riser pipe 13, to about 290 F. or a raise of about 50 F. It was found that a reduction in the number of rodout operations of the order of 65 to 85 percent was accomplished. In addition to this drastic reduction in rodou attention, the process completely eliminated the need for hourly agitation during an intermediate storage step as heretofore required. The benefits of the process and apparatus therefor are thus clear and important.
  • the proportions of the transfer line of the apparatus used are not highly critical, but the size and the position of the transfer line is, nevertheless, important. It is found that a transfer line of only moderate size is highly desirable. Thus, the transfer line conveniently has a cross-sectional area of about one percent of the riser pipe. This is, indeed, greater than the cross-sectional area required for production capacity, but the oversize assures space for a sturdy rod for clean-out purposes.
  • the inclination of the transfer line with respect to the horizontal is also of some significance.
  • the transfer lines should be positioned at an angle of at least 45 to the horizontal to assure sufficiently rapid movement of the sodium through this conduit.
  • a sodium cell having an inverted sodium collection trough for receiving sodium by upward displacement from an electrolysis zone, a riser pipe connecting therewith for upward flow of said sodium to a point above the cell, a transfer conduit connecting to the upper portion of said riser pipe and inclined downwardly at an angle of at least about 45 to the horizontal, heating means associated with said transfer conduit, a valve means in said conduit, and coupling means at the lower terminus of said conduit, said conduit having a transverse area of not over about one percent of the transeverse area of the riser pipe, said coupling means being adapted to couple with coupling means on a movable transport vessel for receiving sodium.
  • a sodium cell having an inverted sodium collection trough for receiving sodium by upward displacement from an electrolysis zone, a riser pipe connecting therewith for upward flow of said sodium to a point above the cell, said riser pipe including an upper segment of enlarged cross section connecting to the lower portion of saidriser pipe by a horizontal shoulder, a transfer conduit connecting to the riser pipe, said connection being at said shoulder, and inclined downwardly at an angle of at least about 45 to the horizontal, heating means associated with said transfer conduit, a valve means in, said c-onduit, and coupling means at the lower terminus of said conduit, said conduit having a transverse area of not over about one percent of the transverse area of the riser pipe, said 0011- pling means being adapted to couple with coupling means on a.
  • movable transport vessel for receiving sodium, and an extension conduit connecting to the enlarged portion of the riser pipe and being aligned with the transfer conduit, and closure means for said extension conduit, whereby an aligning channel is provided for insertion of a clean-out means for the transfer conduit.
  • the improved discharge procedure comprising immediately passing the resultant partly purified sodium metal directly from the upper end of the riser pipe to a transport vessel, said passing being at a higher velocity relative to the upward velocity in the riser pipe and being accompanied by heating of the sodium from about 25 to 75 F. above the discharge temperature from the riser pipe, discontinuing said direct flow to the transport vessel at periodic intervals for disengaging temporarily the transport vessel and accumulating the sodium metal produced in the inverted trough until the transfer vessel is reengaged.
  • the improved discharge procedure comprising immediately passing the resultant partly purifled sodium metal directly from the upper end of the riser pipe to a transport vessel, said passing being at a higher velocity .relative to the upward velocity in the ,riser pipe and being accompanied by heating of .the .50.- -d'i-um from about 25 .to -75?

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
US685902A 1957-09-24 1957-09-24 Operation and discharge of sodium cells Expired - Lifetime US2944950A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US685902A US2944950A (en) 1957-09-24 1957-09-24 Operation and discharge of sodium cells
DEE16453A DE1129714B (de) 1957-09-24 1958-09-19 Downs-Zelle zur Herstellung von Natrium durch Schmelzflusselektrolyse
FR1210355D FR1210355A (fr) 1957-09-24 1958-09-22 Procédé et appareil pour la fabrication de métaux alcalins par électrolyse

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US685902A US2944950A (en) 1957-09-24 1957-09-24 Operation and discharge of sodium cells

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3201229A (en) * 1961-12-20 1965-08-17 Dow Chemical Co Cesium production
US3497447A (en) * 1967-07-21 1970-02-24 Du Pont Tickler assembly for riser pipe of fused salt electrolysis cell for the production of sodium
US3962064A (en) * 1973-09-07 1976-06-08 Commissariat A L'energie Atomique Electrolyzer and a method for the production of readily oxydizable metals in a state of high purity
US4092228A (en) * 1977-03-07 1978-05-30 E. I. Du Pont De Nemours And Company Electrolytic cell
US4744876A (en) * 1985-10-25 1988-05-17 Commissariat A L'energie Atomique Electrolyzer for extracting a substance from an electrolytic bath
US5660710A (en) * 1996-01-31 1997-08-26 Sivilotti; Olivo Method and apparatus for electrolyzing light metals
US5855757A (en) * 1997-01-21 1999-01-05 Sivilotti; Olivo Method and apparatus for electrolysing light metals

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1839756A (en) * 1929-01-30 1932-01-05 Dow Chemical Co Method of electrolysis of fused bath and apparatus therefor
US2130801A (en) * 1934-10-04 1938-09-20 Du Pont Production of light metals

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1501756A (en) * 1922-08-18 1924-07-15 Roessler & Hasslacher Chemical Electrolytic process and cell
US2068681A (en) * 1934-10-04 1937-01-26 Du Pont Apparatus for the production of light metals

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1839756A (en) * 1929-01-30 1932-01-05 Dow Chemical Co Method of electrolysis of fused bath and apparatus therefor
US2130801A (en) * 1934-10-04 1938-09-20 Du Pont Production of light metals

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3201229A (en) * 1961-12-20 1965-08-17 Dow Chemical Co Cesium production
US3497447A (en) * 1967-07-21 1970-02-24 Du Pont Tickler assembly for riser pipe of fused salt electrolysis cell for the production of sodium
US3962064A (en) * 1973-09-07 1976-06-08 Commissariat A L'energie Atomique Electrolyzer and a method for the production of readily oxydizable metals in a state of high purity
US4092228A (en) * 1977-03-07 1978-05-30 E. I. Du Pont De Nemours And Company Electrolytic cell
US4744876A (en) * 1985-10-25 1988-05-17 Commissariat A L'energie Atomique Electrolyzer for extracting a substance from an electrolytic bath
US5660710A (en) * 1996-01-31 1997-08-26 Sivilotti; Olivo Method and apparatus for electrolyzing light metals
US5855757A (en) * 1997-01-21 1999-01-05 Sivilotti; Olivo Method and apparatus for electrolysing light metals

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FR1210355A (fr) 1960-03-08
DE1129714B (de) 1962-05-17

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