US3220827A - Distillation of metals - Google Patents

Distillation of metals Download PDF

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Publication number
US3220827A
US3220827A US255548A US25554863A US3220827A US 3220827 A US3220827 A US 3220827A US 255548 A US255548 A US 255548A US 25554863 A US25554863 A US 25554863A US 3220827 A US3220827 A US 3220827A
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US
United States
Prior art keywords
liquid
volatile constituent
evaporating zone
frusto
zone
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Expired - Lifetime
Application number
US255548A
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English (en)
Inventor
Davey Thomas Ronald Albert
Woods Stephen Esslemont
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Metallurgical Processes Ltd
National Smelting Co Ltd
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Metallurgical Processes Ltd
National Smelting Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/04Refining by applying a vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00Obtaining lead
    • C22B13/06Refining
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00Obtaining zinc or zinc oxide
    • C22B19/04Obtaining zinc by distilling
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/04Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated adapted for treating the charge in vacuum or special atmosphere

Definitions

  • zinc is separated from zinc-containing lead under vacuum in a substantially circular vessel in which zinc-containing lead is caused to flow in a thin, even film over the downward and inward sloping side of a frusto-conical spreading means which is concentrically arranged within the vessel so that zinc is evaporated from the lead and condensed on a cooled surface at the centre of the vessel.
  • the lead may be run into a relatively small annular launder or trough surrounding the top of the spreading tube which is maintained level so that the lead overflows evenly and forms a thin uniform film over the spreading tube.
  • This top may be formed with a weir profile as described more fully below.
  • the invention consists in a method of ensuring even distribution of and facilitating evaporation of a volatile constituent from, liquid flowing in a thin film over an inclined spreading means in which movement of the liquid is so controlled that it flows over the top of the spreading means with a transverse component to its motion.
  • the invention further consists in a method of separating zinc from zinc-containing lead by passing the molten zinc-containing lead under vacuum down the inner inwardly tapering surface of a frusto-conical spreading tube in a thin film and collecting the zinc distilled off, in which the movement of the zinc-containing lead is so controlled that it flows over the top of the frusto-conical spreading tube with a transverse, i.e. tangential component to its motion.
  • the tangential component of the motion may be imparted to the liquid either as, or before, it flows over the top of the spreading means.
  • the invention further consists in apparatus for extracting a volatile constituent from a liquid mixture
  • apparatus for extracting a volatile constituent from a liquid mixture comprising a vacuum vessel containing a hollow tapering spreading means with its broad end uppermost and surrounded by a space capable of holding the liquid mixture at the level of the top of the spreading means so that in operation the liquid mixture flows over the inside surface of the hollow tapering means, and means for ensuring that the liquid flow has a tangential component.
  • these means may be a lead supply pipe which enters the lead holding space at such an angle as to impart a circulatory motion to the zinc-com taining lead in the space when the apparatus is in use.
  • the apparatus for separating zinc from zinc-containing lead is a substantially circular vacuum vessel within which is concentrically positioned a frusto-conical spreading tube surrounded by two intercommunicating concentric launders, from the inner of which zinc-containing lead flows down the inner surface of the frusto-conical spreading tube.
  • a tangential flow motion may be brought about by deflecting vanes around the top of the spreading tube which are positioned at an angle to the radii of the tube.
  • the apparatus may comprise means for directing the zinc-containing lead from the outer to the inner launder so that it enters the launder at an angle to a radius and a circulatory motion is set up in the inner launder.
  • This may be effected by tubes (so formed as not to project within the inner launder and impede the circulatory motion set up) in a dividing wall of the inner and outer launders at a low angle to the wall or alternatively by forming the wall as a series of angled plates and thus defining between adjacent plates 21 series of spaces each at an angle to a radius passing through it.
  • the inner launder may be dispensed with and the outer launder be provided with a supply tube for zinc-containing lead at, or at a small angle to, a tangent to the launder.
  • the apparatus described in the four preceding paragraphs may also have a portion of the frusto-conical tube near the top profiled so as to give a Weir of appropriate shape to minimise or eliminate splashing.
  • the velocity of circulation of zinc-containing lead depends upon the difference in zinc-containing lead level in the two launders (or, in the single-launder modification, upon the speed of Zinc-containing lead supply). This in turn depends upon the head over which the vacuum in the vessel has to draw the Zinc-containing lead, and may also be varied, e.g. by supplying the Zinc-containing lead under pressure.
  • FIGURE 1 is a vertical section through part of the apparatus.
  • FIGURE 2 is a section taken through II in FIGURE 1.
  • FIGURE 3 is a section taken in the same plane as FIGURE 2 of a different embodiment for imparting tangential flow.
  • FIGURE 4 is a similar section showing a third embodiment.
  • FIGURE 5 is a section taken through II--II of FIG- URE 4.
  • FIGURE 6 is a similar section to FIGURES 2, 3 and 4 of a fourth embodiment, and
  • FIGURE 7 is a section taken through line III of FIG- URE 6.
  • FIGURE 1 a substantially circular vessel 1 is supported on surrounding wall 1a.
  • cooling coils 2 frusto-conical spreading tube 3, having an upper portion 3a and a top 3b, inner launder- 4 and outer launder 5, the launder 5 being an annular chamber defined between the tube 3 and the wall of the vessel, and launder 4 being defined by the upper portion 3a of tube 3 and a surrounding angled metal sheet 6.
  • Outer launder 5 connects via angled barometric inlet tube 7 with lead-holding bath 8 (it will be appreciated that since the vessel 1 is under vacuum, lead will rise in tube 7 and pass into launder 5) In operation, lead runs uniformly over the circular top 3b of tube 3 and falls in a thin film down the tube, in the process losing the zinc vapour which accumulates as zinc metal upon the cooling coils 2. Such an accumulation is shown at 9.
  • the centrifugal force exerted by the swirling motion at 3b holds the lead film on to the weir and spreading surface, preventing the film from leaping out and splashing.
  • the profile of the weir is chosen so as to give a smooth flow of lead from its horizontal flow over the weir lip to its almost vertical flow down the spreading tube.
  • FIGURE 1 shows one of a series of tubes interconnecting the launders 4 and 5. These tubes pass through the sheet 6 at an angle, as is more clearly shown in FIGURE 2.
  • the lead in outer launder 5 is at a level 5a higher than that of the top 3b of tube 3.
  • This lead passes into the inner launder at an angle, and the whole of the lead in the inner launder in fact circulates around the inner launder because of this. It therefore runs over the top 3b of tube 3 with a tangential component of motion and runs down tube 3 as shown by the arrows in FIGURE 1. It will be observed that tubes 11 do not project into the inner launder 4. This gives a streamlined flow at the dividing wall 6.
  • FIGURE 3 More especially for low flow rates of lead, the arrangement of FIGURE 3 may be adopted.
  • inner launder 4 is not used, but the remaining launder 5 is fed tangentially (via barometric inlet tube 7) from a holding bath such as shown at 8 in FIGURE 1.
  • FIGURES 4 and 5 a further method of ensuring tangential flow is shown.
  • an inner launder 4 is used fed from outer launder 5 by virtue of its higher lead level 5a.
  • lead passes from 5 to 4 via holes 12 which do not impart a tangential motion; the tangential motion is imparted to the lead as it flows over the top 3b of the tube 3 by the deflecting vanes 13 which are welded to the top 3b of tube 3 at an angle with respect to a radius.
  • FIGURES 6 and 7 show an arrangement in which the whole wall of the inner launder 4 is composed of angled plates 14 welded to the launder bottom 15. As will be evident from FIGURES 6 and 7, these plates have the same function as tubes 11 of FIGURES 1 and 2, since they impart a tangential motion to the lead before it passes over the top of tube 3.
  • the slope of tube 3 in the foregoing embodiments is conveniently about 10 in 1. Any slope much gentler than this results in the evacuated vessel 1 being less compact and therefore less able to stand the strain of evacuation.
  • a suitable circumferential velocity for the liquid in the inner launder has been determined for lead as being a little less than one third of the circumference of the upper part of the tube per second.
  • a circumferential velocity for the lead of about 4 ft./sec. is satisfactory. Because of frictional losses, this will require an inlet velocity of about 8 ft./sec. which can be supplied by a 12" potential head drop between the outer and inner launders.
  • Greater angular velocities can of course be produced by providing a greater potential head drop and this, by appropriate arrangement of levels of the holding bath 8 and the vessel, may be even greater than one barometric head of the liquid in question, while using only atmospheric pressure to force liquid through an evacuated vessel, or may, of course, be produced by a pump supplying liquid to the vessel.
  • a contained continuously replenished inner annular 'body of the liquid complex is formed around the exterior upper portion of the frusto-conical evaporating zone
  • a separately contained continuously replenished outer annular body of the liquid complex is formed around the exterior of the inner annular body of liquid complex
  • liquid complex is continuously passed from the outer annular body to the inner annular body, maintaining the level of the outer annular body of liquid complex at a substantially higher level than the top of the frusto-conical evaporating zone and the normal liquid level in the inner annular body to establish a hydro-static head in the outer annular body for accelerating the flow of liquid complex from the outer annular body to the inner annular body, and liquid complex in the inner annular body is flowed continuously under pressure into the evaporating zone at a controlled angular velocity.
  • liquid complex is molten zinc-containing lead, and the zinc is the more volatile constituent and the lead is the less vola tile constituent.
  • liquid complex in the outer and inner annular bodies is molten zinc-containing lead, and the zinc is the more volatile constituent and the lead is the less volatile constituent.
  • apparatus for separating and recovering a relatively volatile constituent from a liquid complex containing the same in association with a less volatile constituent, such as molten zinc-containing lead, the zinc being the more volatile constituent and the lead being the less volatile constituent including a generally circular vacuum chamber, a substantially vertical hollow inverted generally circular frusto-conical distributing tube disposed within and spaced from the side wall of the chamber, the larger end of the frusto-conical tube being uppermost and the smaller end being lowermost, an annular launder for the passage of the liquid complex located between the side wall of the chamber and the exterior of the frusto-conical tube, means for feeding liquid complex continuously into the launder, an upright condenser for the more volatile constituent disposed concentrically in the center portion of the chamber spaced a suitable distanoe from the frusto-conical tube, said condenser being adapted to support on its outer peripheral surface a relatively thick solid cake composed of said more volatile constituent to provide a condensing surface for more vapours of the more volatile
  • the annular launder constitutes an inner laundry immediately adjacent the periphery of the top portion of the frustoconical tube and an outer annular launder surrounding the inner annular launder
  • the associated devices include a plurality of circumferentially spaced upright plates set at an acute angle to the outer periphery of the frustoconical tube and integrally secured to the bottom of the inner launder to separate the two launders in a sub-divided manner, the plates extend upwardly from the bottom of the inner launder substantially above the level of liquid complex normally confined in the two launders, each plate extends part Way into the outer launder and part way into the inner launder, and each plate is oriented in substantially the same general circumferential direction to divert separate streams of liquid complex from the outer annular launder into the inner annular launder and to impart a circulatory flow of the liquid complex in the inner launder, so that the circulating liquid complex may be discharged from the inner launder tangentially into the frusto-
  • the annular launder constitutes an inner launder immediately adjacent the periphery of the top portion of the frustoconical tube, an outer annular launder surrounding the inner annular launder
  • the associated devices include a barometric inlet tube connecting a source of liquid complex with the interior of the outer launder for feeding liquid complex therethrough, a plurality of circumferentially spaced passageways connect the outer launder with the inner launder for the passage of liquid complex the rethrough, the inner and outer walls of the outer annular launder extend substantially higher than the top of the frusto-conical tube so that the outer launder may contain an annular body of the liquid complex with a liquid level substantially higher than the normal liquid level in the inner annular launder to establish a hydrostatic head in the outer annular launder for impelling liquid complex under accelerated velocity through the fit passageways from the outer annular launder to the inner annular launder.
  • Apparatus according to claim 16 in which the passageways connect with inlet tubes extending at an acute angle from the outer exterior wall of the inner annular launder part Way into the interior of the outer annular launder, the inlet end of said inlet tubes opens into the outer launder and the outlet end of the inlet tubes opens tangentially into the inner launder, and each inlet tube is oriented in substantially the same general circumferential direction to accelerate circulation of the liquid complex in its normal direction of How in the inner launder.
  • the associated devices also include a plurality of upright deflecting vanes integrally secured to the top over-flow lip of the frusto-conical tube at an acute angle, a free end of each vane extends from the over-flow lip over the frusto-conical tube, and each deflecting vane is oriented in substantially the same general circumferential direction for discharging liquid complex tangentially into the frusto-conical tube and onto its inner distributing surface.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
US255548A 1962-02-21 1963-02-01 Distillation of metals Expired - Lifetime US3220827A (en)

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Application Number Priority Date Filing Date Title
GB6683/62A GB1014161A (en) 1962-02-21 1962-02-21 Distillation of metals

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DE (1) DE1239101B (cs)
ES (1) ES285299A1 (cs)
GB (1) GB1014161A (cs)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3767381A (en) * 1971-07-28 1973-10-23 Alco Standard Corp Furnace and method of using the same for reclaiming metal

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1688426A (en) * 1927-02-01 1928-10-23 American Smelting Refining Method and apparatus for producing zinc dust
US2032215A (en) * 1934-02-14 1936-02-25 Magnesium Products Inc Method of and apparatus for treating discrete particles and vapors
US2424640A (en) * 1942-10-21 1947-07-29 Rossi Irving Apparatus for casting metals continuously
US2720456A (en) * 1949-08-05 1955-10-11 Broken Hill Ass Smelter Distillation of metals
US2823111A (en) * 1953-07-16 1958-02-11 Broken Hill Ass Smelter Continuous vacuum distillation
US3031296A (en) * 1957-10-18 1962-04-24 Metallurgical Processes Ltd Separation of lead and zinc

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2789308A (en) * 1953-09-17 1957-04-23 Hoover Co Suction cleaning tool having resilient surface engaging fingers

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1688426A (en) * 1927-02-01 1928-10-23 American Smelting Refining Method and apparatus for producing zinc dust
US2032215A (en) * 1934-02-14 1936-02-25 Magnesium Products Inc Method of and apparatus for treating discrete particles and vapors
US2424640A (en) * 1942-10-21 1947-07-29 Rossi Irving Apparatus for casting metals continuously
US2720456A (en) * 1949-08-05 1955-10-11 Broken Hill Ass Smelter Distillation of metals
US2823111A (en) * 1953-07-16 1958-02-11 Broken Hill Ass Smelter Continuous vacuum distillation
US3031296A (en) * 1957-10-18 1962-04-24 Metallurgical Processes Ltd Separation of lead and zinc

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3767381A (en) * 1971-07-28 1973-10-23 Alco Standard Corp Furnace and method of using the same for reclaiming metal

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Publication number Publication date
DE1239101B (de) 1967-04-20
DE1239101C2 (cs) 1967-11-02
GB1014161A (en) 1965-12-22
ES285299A1 (es) 1963-08-01

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