Classifications

• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F27—FURNACES; KILNS; OVENS; RETORTS
  • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
  • F27D27/00—Stirring devices for molten material
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
  • C22B13/00—Obtaining lead
  • C22B13/06—Refining
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
  • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
  • C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
  • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
  • C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F27—FURNACES; KILNS; OVENS; RETORTS
  • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
  • F27D3/00—Charging; Discharging; Manipulation of charge
  • F27D3/15—Tapping equipment; Equipment for removing or retaining slag
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F27—FURNACES; KILNS; OVENS; RETORTS
  • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
  • F27D3/00—Charging; Discharging; Manipulation of charge
  • F27D2003/0034—Means for moving, conveying, transporting the charge in the furnace or in the charging facilities
  • F27D2003/0054—Means to move molten metal, e.g. electromagnetic pump

Definitions

• the invention relates to a method and a device for separating a specifically lighter phase from a specifically heavier liquid phase.
• the starting material in which phase separation takes place is understood to be a single-phase liquid or melt in which two phases are formed by adding reagents, and a liquid-liquid or a solid-liquid suspension.
• Starting material such as Lead and other contaminated lead such as used lead and lead alloys contain accompanying metals as contaminants, which must be removed in order to produce pure lead.
• Contaminants that can be separated e.g. Sb, As, Sn, Tl, Zn, Ca and Mg are formed by introducing reagents into a specifically lighter phase which is not very soluble in lead, e.g. transferred to the oxide phase that forms on the surface of the specifically heavier liquid phase, e.g. Lead collects and is subtracted from this phase.
• the specifically lighter phase can be obtained in the liquid or solid state.
• DE-PS 30 16 160 describes a deduction by means of a screw conveyor.
• the invention has for its object to enable the greatest possible separation of a specifically lighter phase from a specifically heavier liquid phase in an economically and technically simple manner.
• the object is achieved according to the invention by a process for separating a specifically lighter phase from a specifically heavier liquid phase, a suspension being stirred in a reaction vessel, suspension entering the lower end of a tube open at the top and bottom, the upper end of the tube lies above the surface of the suspension, the phases separate in the tube, the specifically lighter phase is removed from the upper end of the tube, the specifically heavier liquid phase flows back into the suspension through the lower end of the tube and specifically heavier ones liquid phase is withdrawn from the reaction vessel.
• the tube immersed in the suspension can have any cross-section, e.g. have round, square, polygonal, oval, etc.
• the tube is preferably arranged vertically in the suspension. But it can also be arranged inclined or kinked.
• the lower end of the tube is arranged at least so deep in the suspension that a demixing zone calmed in terms of fluid mechanics can form under the specifically lighter phase floating in the tube, in which the specifically heavier liquid phase and the specifically lighter phase separate.
• the tube is preferably arranged on the edge of the vessel and is removable.
• the lower end of the tube is preferably formed with an enlarged cross section.
• the volume of the tube is very small compared to the volume of the vessel and is generally less than 2%.
• the suspension is preferably mixed by a mechanical stirrer immersed in the suspension.
• the process can be carried out continuously, semi-continuously or batchwise.
• the vessel can be cooled from the outside, e.g. by blowing air on the outer jacket. This can increase the throughput.
• a preferred embodiment of the invention is that the tube is arranged on the edge of the vessel and suspension is intimately mixed with a stirrer arranged in the region of the center of the vessel.
• a stirrer arranged in the middle of the A characteristic optimal flow is achieved in the suspension, the suspension being drawn down in a funnel shape in the middle of the kettle to the stirrer, flowing to the bottom and flowing upward in the region of the wall.
• the suspension executes a rotational movement in the vessel around the stirrer, which is based on the rotational movement of the stirrer. Due to the arrangement of the tube on the edge of the vessel, the lower opening of the tube lies in the upward flow of the suspension.
• a preferred embodiment of the invention is that at least one reagent is introduced into the suspension spatially separated from the tube in the downward part of the flow generated by the stirring. If a suspension is present, the addition of the reagents can accelerate the phase separation or the proportion of the specifically lighter phase can be increased by reacting the reagents. In the case of a single-phase starting material, the reaction of the starting material with the reagents produces the specifically lighter phase.
• at least one reagent such as, for example, an oxygen-containing gas into the downward part of the flow, the oxygen content of the gases is largely used for the oxidation because the residence time of the oxygen in the suspension is longer.
• the introduction is preferably carried out in such a way that the reagents, for example oxygen-containing gas, have as little influence as possible on the cleaning zone in the tube.
• the reagents for example oxygen-containing gas
• the reagents can be introduced into the suspension through an immersed lance, through the hollow shaft of the stirrer or through a sink with a feed line from below.
• Several lances or flushing stones can also be arranged to introduce the reagents.
• a preferred embodiment of the invention is that the suspension enters from above into a delimited calming zone arranged in the suspension, the suspension separates into phases, the specifically lighter phase returns to the suspension and the specifically heavier liquid phase is continuously withdrawn and starting material continuously is added.
• the delimited calming zone can consist, for example, of a siphon, one leg of which is arranged vertically with the opening upward in the suspension and the other leg of which is arranged as an outlet over the edge of the vessel.
• the suspension flows into the opening of the vertical leg, in which a calming and phase separation then occurs.
• the specifically lighter phase floats and re-enters the suspension in the vessel.
• the specifically heavier liquid phase sinks and flows out of the vessel via the other leg. This arrangement also results in an automatic level control of the suspension in the vessel.
• the delimited calming zone can also be formed by a tube arranged vertically on the bottom of the vessel, into which the suspension enters from above and from which the specifically heavier liquid phase is drawn off in a controlled amount through the bottom of the vessel
• a preferred embodiment of the invention is that the tube is inserted into the reaction vessel after the start of the reaction. This measure advantageously ensures that phase separation is only initiated after a required temperature has been reached.
• a preferred embodiment of the invention is that the tube is inserted into the reaction vessel after the reaction is complete. This measure prevents unreacted reagents from being withdrawn from the suspension during sluggish reactions.
• a preferred embodiment of the invention is that the temperature in the reaction vessel by adding Starting material is kept constant.
• the amount of heat released in an exothermic reaction, for example, and the corresponding increase in temperature in a suspension is absorbed by adding starting material with a correspondingly low temperature. This enables the throughput of the vessel to be optimized.
• a preferred embodiment of the invention consists in the fact that the starting material is lead or lead with one or more metals such as Sb, As, Sn, Tl, Zn, Ca and Mg and one or more reagents such as oxygen-containing gases, oxygen-containing compounds, chlorine-containing gases and chlorine-containing compounds be used.
• the term "lead" is to be understood in addition to lead any other contaminated lead such as lead and lead alloys.
• the impurities consist of all metallic elements to be separated, for example by oxidation of lead, such as Sb, As, Sn, Zn, Ca and Mg.
• the oxide phase of the impurities can be liquid and flow off automatically from the upper part of the immersed tube.
• the invention can also have a solid, small-sized aggregate state and can be removed pneumatically or mechanically from the upper opening of the immersed tube.
• the invention is particularly suitable for removing Sb, Sn or As from lead, whereby the oxide product, which is produced in liquid form by the procedure, flows off automatically.
• the invention is particularly suitable for post-refining to remove Ca, Mg or Zn with NaOH 3 .
• Technically pure oxygen is used in particular as the oxygen-containing gas. Oxygenated gas can also be used.
• a device consisting of a reaction vessel with a stirring device, an introduction for reagents and a tube with an open upper end and an open lower end, the upper end of the tube being arranged above the surface of the suspension and a withdrawal device for the specific Lighter phase and the lower end of the tube is designed as an inlet opening for the suspension.
• a suspension such as a lead bath can be arranged in the reaction vessel.
• In the lower part of the tube there is a calming zone for the suspension, in the middle part of the tube there is a separation zone, in the upper part of the tube there is a collecting zone and a discharge device for the specifically lighter phase.
• the suspension e.g. Lead
• the reaction e.g. with oxygen in the whole vessel, oxide phase and lead phase are constantly mixed and come into contact and therefore work can be done on thermodynamic equilibrium.
• the response speed is high.
• the throughput is very high, especially when working continuously.
• the tube which serves as a separating device and extraction device for the oxide phase, is a very simple and failure-prone unit and nevertheless enables a very good and quick separation of the two phases.
• There is a small amount of oxide phase in the tube so that even in batch operation, a refined lead with small amounts of e.g. Oxide phase occurs.
• the method can be used to remove Sb down to ⁇ 0.05%.
• a preferred embodiment of the invention is that the lower end of the tube is formed with a widening.
• a preferred embodiment of the invention consists in that a tube with a valve protruding into the reaction vessel is arranged at the bottom of the reaction vessel.
• a preferred embodiment of the invention is that a siphon is arranged at the bottom of the reaction vessel, one leg of which is vertical with the opening upward in the Suspension is arranged and the other leg is arranged as an outlet over the edge of the reaction vessel.
• the drawing includes FIGS. 1 to 5.
• 1 is a longitudinal section through a reaction vessel with a mechanical stirrer arranged in the middle and a tube according to the invention arranged on the edge.
• Fig. 2 is a longitudinal section through the tube on a larger scale.
• FIG. 3 is a cross section according to A-A in FIG. 2.
• Fig. 4 is a longitudinal section through a reaction vessel with a siphon arranged at the bottom of the reaction vessel.
• 5 is a longitudinal section through a reaction vessel with a tube with a valve arranged at the bottom of the reaction vessel.
• the reaction vessel (1) for example a lead smelting boiler (Fig. 1)
• a suspension (2) for example a lead bath.
• a mechanical stirrer (3) is arranged in the middle of the suspension (2), the direction of rotation of which is indicated by the arrow.
• the introduction tube (4) for one or more reagents, such as, for example, oxygen-containing gas, is arranged in the suspension (2).
• the tube (5) is arranged at the edge of the reaction vessel (1), the upper end (6) and lower end (7) of which are open and the lower end (7) of which has a widening (10).
• the upper end of the tube (5) is arranged above the surface (8) of the suspension (2.
• the rotation of the propeller (11) of the stirrer (3) is indicated by the arrows and dashed lines characteristic flow generated in the suspension.
• the suspension rotates around the stirrer (3) in the direction of the rotating movement of the stirrer (3).
• the lower opening of the tube (7) lies in the rising part of the flow, and a suspension of a specifically heavier liquid phase and a specifically lighter phase such as a suspension emerges Lead and oxide phase in the lower end (7).
• the entered suspension is calmed down in the zone of the tube (5) designated (a).
• Zone (b) segregates the specifically heavier liquid phase and the specifically lighter phase.
• a removable cover (13) with a line (14) for connection to a suction device (9) is arranged on the reaction vessel (1).
• the tube (5) is equipped with spacers (15) (Fig. 2) which rest on the inner wall of the reaction vessel (1).
• the upper open end (6) of the tube (5) can be covered by a hood (16) which has an opening on the side of the drainage channel.
• the section shown in FIG. 3 along the line AA shows, by way of example, the ratio of the cross section of the tube (5) to the cross section of the widening (10) in the lower region of the tube (5).
• reaction vessel (1) shows a reaction vessel (1), the delimited calming zone being formed by a pipe (17) arranged vertically on the bottom of the vessel (1) and the drainage channel of the pipe (17) having a valve (18).
• 5 shows a reaction vessel (1), the delimited calming zone consisting of a siphon (19), one leg (20) of which is arranged vertically with the opening facing upwards in the suspension and the other leg f21. Arranged as an outlet (22) over the edge of the reaction vessel (1). is.
• a reaction vessel (1) equipped as a lead smelter has a diameter of 3.0 m, a height of 2.5 and contains approx. 140 t of lead smelter.
• the tube (5) has a length of 110 cm from the lower end (7) to the upper end (6).
• the diameter of the tube (5) is 20 cm and the diameter of the widening (10) is 50 cm.

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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)
• Extraction Or Liquid Replacement (AREA)
• Treatment Of Liquids With Adsorbents In General (AREA)
• Physical Or Chemical Processes And Apparatus (AREA)

Priority Applications (4)

Applications Claiming Priority (2)

Publications (1)

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Citations (9)

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• 1995
  • 1995-01-07 DE DE19500266A patent/DE19500266C1/de not_active Expired - Lifetime
  • 1995-12-13 ES ES95942152T patent/ES2174974T3/es not_active Expired - Lifetime
  • 1995-12-13 AT AT95942152T patent/ATE216434T1/de not_active IP Right Cessation
  • 1995-12-13 DE DE59510176T patent/DE59510176D1/de not_active Expired - Lifetime
  • 1995-12-13 WO PCT/EP1995/004941 patent/WO1996021049A1/de active IP Right Grant
  • 1995-12-13 EP EP95942152A patent/EP0800590B1/de not_active Expired - Lifetime
• 1997
  • 1997-07-02 NO NO19973082A patent/NO319933B1/no not_active IP Right Cessation

Patent Citations (11)

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