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EP0800590B1 - Procede et dispositif pour separer une phase specifiquement plus legere d'une phase liquide specifiquement plus lourde - Google Patents

Procede et dispositif pour separer une phase specifiquement plus legere d'une phase liquide specifiquement plus lourde Download PDF

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Publication number
EP0800590B1
EP0800590B1 EP95942152A EP95942152A EP0800590B1 EP 0800590 B1 EP0800590 B1 EP 0800590B1 EP 95942152 A EP95942152 A EP 95942152A EP 95942152 A EP95942152 A EP 95942152A EP 0800590 B1 EP0800590 B1 EP 0800590B1
Authority
EP
European Patent Office
Prior art keywords
suspension
tube
reaction vessel
phase
vessel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP95942152A
Other languages
German (de)
English (en)
Other versions
EP0800590A1 (fr
Inventor
Jürgen HEERING
Thomas Schierle
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.)
Ecobat Resources Stolberg GmbH
Original Assignee
"Berzelius" Stolberg GmbH
Berzelius Stolberg GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by "Berzelius" Stolberg GmbH, Berzelius Stolberg GmbH filed Critical "Berzelius" Stolberg GmbH
Publication of EP0800590A1 publication Critical patent/EP0800590A1/fr
Application granted granted Critical
Publication of EP0800590B1 publication Critical patent/EP0800590B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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 an apparatus for Separation of a specifically easier phase from a specific one heavier liquid phase.
  • the starting material for which a Phase separation takes place is single-phase in the sense of the invention Liquid or melt, in which by adding Reagents form two phases, as well as a liquid-liquid or to understand a solid-liquid suspension.
  • Starting material such as Lead and other contaminated Lead such as used lead and lead alloys contain as Impurities accompanying metals that are used to produce pure Lead must be removed.
  • Impurities that are separated can be like Sb, As, Sn, Tl, Zn, Ca and Mg by introducing reagents into a lead-insoluble specifically lighter phase such as transferred to the oxide phase, the itself on the surface of the specifically heavier liquid Phase such as Lead collects and is subtracted from this phase.
  • the specifically lighter phase can be in liquid or solid Condition.
  • the removal of an oxide phase can be done manually by skimming Perforated trowels or pulling off on an inclined ramp, such as described in DE-PS 33 03 810.
  • CA-PS 10 11 108 From CA-PS 10 11 108 it is known to be a fine-grained Loosen oxide phase and at the same time pneumatically suck.
  • DE-PS 38 31 898 describes a process for removing As, Sn and Sb known, in which in a filled with lead Melting boiler an open tube is arranged, the upper one The end is above the surface of the lead bath and that is a small one Volume, based on the lead bath. In the upper end of the pipe, the lead bath becomes lead in a turbulent flow pumped and technical oxygen introduced at the same time. Around a second larger tube is arranged around this tube, in which the lead intimately mixed with oxygen from the lower End of the small pipe flows.
  • the larger pipe serves as Calming room in which the oxide phase generated from lead is separated and floated to the surface.
  • the severed Lead flows back out of the larger pipe into the lead bath.
  • the floating oxide phase flows out of the larger pipe at the top over a gutter. The reaction occurs in this process of oxygen only in a very small volume of the lead, and there will be no thermodynamic equilibrium as a whole Lead of the melting pot is achieved.
  • EP-A-0 099 711 relates to a process for continuous Removal of tin from a reaction vessel Lead smelting by melting the lead with chlorine and oxygen is added so that a tin-containing slag forms, the mixed with lead near the bottom of the reaction vessel removed and to separate the lead from the tin-containing Slag from a calming zone located in the reaction vessel is abandoned. About process engineering training as well about the removal of the slag in this case, however no further information is disclosed.
  • the invention is based, if possible extensive separation of a specifically easier phase from one specifically heavier liquid phase in economical and technically simple way to enable.
  • the tube immersed in the suspension can be any Cross section such as round, square, polygonal, oval, etc. exhibit.
  • the tube is preferably vertical in the suspension arranged. But it can also be arranged inclined or kinked become.
  • the lower end of the pipe is at least as deep in the suspension arranged that under the in the tube floated specifically easier phase one fluidically calmed separation zone can form, in which is the specifically heavier liquid phase and the segregate specifically the lighter phase.
  • the pipe will preferably arranged on the edge of the vessel and removable.
  • the volume of the pipe is compared to the volume of the vessel is very low and is generally less than 2%. When the suspension is thoroughly mixed the specifically easier phase below the level of the lower edge of the pipe.
  • the suspension is preferably mixed by a mechanical stirrer immersed in the suspension.
  • the process can be continuous, semi-continuous or be carried out discontinuously.
  • the vessel can be from the outside chilled e.g. by blowing air on the outer jacket. Thereby the throughput can be increased.
  • a preferred embodiment of the invention is that the tube is arranged on the edge of the vessel and suspension with a stirrer arranged in the area of the center of the vessel is mixed.
  • a preferred embodiment of the invention is that spatially at least one reagent in the suspension from the tube separated in the downward part by stirring generated flow is initiated.
  • a reagent can be used accelerated phase separation take place or by reaction of the Reagents increased the proportion of the specifically lighter phase become.
  • the Reaction of the starting material with the specific reagents creates lighter phase.
  • oxygen-containing gas exert as little influence as possible on the calming zone in the pipe. This happens because the reagents at one point in the Suspension are initiated in the direction of rotation of the flow the suspension is so far in front of the pipe that the reaction of the Reagent in the suspension is finished when the suspension Tube reached.
  • the introduction of the reagents into the suspension can through a submerged lance, through the hollow shaft of the Stirrer or through a sink with supply line from below respectively. Several lances or sink stones can also be used Initiation of the reagents are arranged.
  • a preferred embodiment of the invention is that the suspension from above into one arranged on the bottom of the vessel in the suspension delimited calming zone occurs, the suspension settles in Separates phases, the specifically lighter phase into the suspension decreases and the specifically heavier liquid phase is continuously withdrawn and starting material is added continuously.
  • the delimited calming zone can e.g. consist of a siphon, one leg arranged vertically with the opening upwards in the suspension and its other leg over the edge of the vessel as Spout is arranged.
  • the suspension flows into the opening of the vertical leg, in which then a reassurance and Phase separation occurs.
  • the specifically easier phase floats occurs and re-enters the suspension in the vessel.
  • the specifically heavier liquid phase sinks and flows over the other leg from the vessel.
  • the delimited calming zone can also be defined by a Pipe formed vertically on the bottom of the vessel into which the suspension enters from above and from which the specifically heavier liquid phase below through the bottom of the Vessel is withdrawn in a controlled amount.
  • a preferred embodiment of the invention is that the tube is inserted into the reaction vessel after the start of the reaction becomes. This measure advantageously ensures that the phase separation only after a required one has been reached Temperature is initiated.
  • a preferred embodiment of the invention is that the tube into the reaction vessel after the Reaction is used. This measure prevents that did not react in sluggish reactions Reagents are withdrawn from the suspension.
  • a preferred embodiment of the invention is that the temperature in the reaction vessel by adding Starting material is kept constant.
  • 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 physical state and 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. Oxygen-enriched gas can also be used.
  • a Device consisting of a reaction vessel with a stirrer, an introduction for reagents and one Pipe with an open upper end and an open lower end, the upper end of the tube above the surface of the suspension is arranged and a trigger device for the specific has lighter phase and the lower end of the tube than Inlet opening is designed for the suspension.
  • the reaction vessel can be a suspension such as e.g. a lead bath be arranged.
  • In the lower part of the tube is one Calming zone for the suspension, in the middle part of the pipe is a separation zone, in the upper part of the tube there is one Collection zone and a deduction device for the specific lighter phase arranged.
  • the suspension such as. Lead has a long residence time in the vessel, the reaction e.g. with oxygen in the entire vessel, oxide phase and Lead phase are constantly mixed and come into contact and therefore work on the thermodynamic equilibrium can.
  • the response speed is high.
  • the Throughput performance is especially with continuous Working very high. That as a separator and trigger for the oxide phase tube is a very simple and failure-prone aggregate and still enables a very good one and quick separation of the two phases. Is in the pipe a small amount of oxide phase, so that even with batch Operation a refined lead with small residual amounts of e.g. Oxide phase occurs.
  • the procedure is among others for Removal of Sb can be used down to ⁇ 0.05%.
  • a preferred embodiment of the invention is that the lower end of the tube is formed with a widening is.
  • a preferred embodiment of the invention is that at the bottom of the reaction vessel into the reaction vessel protruding tube is arranged with a valve.
  • a preferred embodiment of the invention is that a siphon is arranged at the bottom of the reaction vessel, the one leg vertically with the opening up in the Suspension is arranged and the other leg over the Edge of the reaction vessel is arranged as an outlet.
  • the drawing includes FIGS. 1 to 5.
  • Fig. 1 is a longitudinal section through a reaction vessel with a mechanical stirrer arranged in the middle and on the edge arranged pipe according to the invention.
  • Fig. 2 is a longitudinal section through the tube in 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.
  • Fig. 5 is a longitudinal section through a reaction vessel with a tube arranged at the bottom of the reaction vessel a valve.
  • the reaction vessel (1) e.g. a lead smelting boiler (Fig. 1)
  • a suspension (2) e.g. a lead bath.
  • a mechanical stirrer (3) is arranged in the suspension (2), whose direction of rotation is indicated by the arrow.
  • the inlet pipe (4) for one or more Reagents such as oxygen-containing gas, arranged.
  • the tube (5) of the reaction vessel (1) is arranged upper end (6) and lower end (7) are open and the lower End (7) is formed with a widening (10).
  • the top The end of the tube (5) is above the surface (8) of the suspension (2) arranged.
  • the tube (5) is with Spacers (15) (Fig. 2) equipped 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) on the Side of the gutter has an opening.
  • the one in Fig. 3 shown section along the line A-A shows an example the ratio of the cross section of the tube (5) to that Cross section of the widening (10) formed in the lower Area of the pipe (5).
  • 5 shows a reaction vessel (1), the defined calming zone consisting of a siphon (19) there is one leg (20) vertically with the opening is arranged upwards in the suspension and its other Leg (21) over the edge of the reaction vessel (1) as an outlet (22) is arranged.
  • the tube (5) has a length of 110 cm from 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.
  • the Sb content When refining a container with 130 t of lead, the Sb content could be reduced by 0.35% by weight within 60 minutes by using 130 Nm 3 of technical oxygen.
  • the described invention it was possible to draw off 96% by weight of the oxidized antimony as a smear from the kettle.

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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)

Claims (11)

  1. Procédé pour séparer une phase spécifiquement plus légère d'une phase liquide spécifiquement plus lourde, dans lequel une suspension produite au moyen de produits réactifs d'apport est agitée dans une cuve de réaction, la suspension dans la zone de la partie dirigée vers le haut de l'écoulement de suspension provoqué par l'agitation pénètre dans l'extrémité inférieure d'un tube agencé à proximité de la bordure de la cuve et ouvert depuis le bas et depuis le haut, caractérisé en ce que l'extrémité supérieure du tube ainsi qu'un dispositif d'extraction relié à celle-ci sont disposés au-dessus de la surface de la suspension, en ce que les phases se séparent dans le tube, en ce que la phase spécifiquement plus légère est enlevée hors de l'extrémité supérieure du tube, ou respectivement hors du dispositif d'extraction, en ce que la phase liquide spécifiquement plus lourde s'écoule à travers l'extrémité inférieure du tube en retour jusque dans la suspension, et en ce que la phase liquide spécifiquement plus lourde est extraite hors de la cuve de réaction.
  2. Procédé selon la revendication 1, caractérisé en ce que le tube est agencé à la bordure du récipient, et en ce que la suspension est mélangée de façon intime avec un agitateur agencé au milieu de la cuve.
  3. Procédé selon l'une des revendications 1 et 2, caractérisé en ce qu'au moins un produit réactif est introduit dans la suspension de façon séparée dans l'espace par rapport au tube dans la partie dirigée vers le bas de l'écoulement engendré par l'agitation.
  4. Procédé selon les revendications 1 à 3, caractérisé en ce que la suspension pénètre depuis le haut dans une zone de tranquillisation délimitée agencée dans la suspension au fond de la cuve, la suspension se sépare en phases, la phase spécifiquement plus légère est retournée dans la suspension et la phase liquide spécifiquement plus lourde est extraite en continu et du matériau de départ est additionné en continu dans la suspension.
  5. Procédé selon les revendications 1 à 4, caractérisé en ce que le tube est introduit dans la cuve de réaction après le commencement de la réaction.
  6. Procédé selon les revendications 1 à 5, caractérisé en ce que le tube est introduit dans la cuve de réaction après écoulement complet de la réaction.
  7. Procédé selon les revendications 1 à 6, caractérisé en ce que la température dans la cuve de réaction est maintenue constante par addition de matériau de départ.
  8. Procédé selon les revendications 1 à 7, caractérisé en ce que l'on utilise comme matériau de départ du plomb de liquidation ou du plomb avec un ou plusieurs métaux tels que Sb, As, Sn, Ti, Zn, Ca et Mg, et un ou plusieurs produits réactifs tels que des gaz contenant de l'oxygène, des composés contenant de l'oxygène, des gaz contenant du chlore et des composés contenant du chlore.
  9. Appareil pour la séparation d'une phase spécifique plus légère depuis une phase liquide spécifiquement plus lourde, comprenant une cuve de réaction (1) pourvue d'une conduite d'entrée (4) pour des produits de réaction, un dispositif agitateur (3) agencé dans ladite cuve, et un tube (5) ouvert en haut et en bas agencé à proximité de la bordure dans la cuve de réaction, dont l'extrémité supérieure est reliée à un dispositif d'extraction (12), dans lequel une suspension est agitée au moyen du dispositif agitateur dans la cuve de réaction, caractérisé en ce que l'extrémité inférieure (7) du tube (5) présente une section (10) plus forte que la partie restante du tube et le volume du tube est inférieur à 2% par comparaison au volume de la cuve de réaction, et la position du tube est ainsi conçue que la suspension pénètre dans l'extrémité inférieure dans la région de la partie dirigée vers le haut de l'écoulement de suspension, et les phases se séparent dans le tube, la phase spécifiquement plus légère est extraite hors de l'extrémité supérieure (6) du tube, respectivement hors du dispositif d'extraction, et la phase liquide spécifiquement plus lourde s'écoule à travers l'extrémité inférieure (7) du tube en retour dans la suspension.
  10. Appareil selon la revendication 9, caractérisé en ce qu'un tube (17) pénétrant dans la cuve de réaction et pourvu d'une valve (18) est agencé sur le fond de la cuve de réaction (1).
  11. Appareil selon la revendication 9, caractérisé en ce qu'un siphon (19) est agencé au fond de la cuve de réaction (1), dont une branche (20) est agencée verticalement avec l'ouverture vers le haut dans la suspension (2), et dont l'autre branche (21) est agencée au-dessus de la bordure de la cuve de réaction à titre d'évacuation.
EP95942152A 1995-01-07 1995-12-13 Procede et dispositif pour separer une phase specifiquement plus legere d'une phase liquide specifiquement plus lourde Expired - Lifetime EP0800590B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19500266 1995-01-07
DE19500266A DE19500266C1 (de) 1995-01-07 1995-01-07 Verfahren und Vorrichtung zur Trennung einer spezifisch leichteren Phase von einer spezifisch schwereren flüssigen Phase
PCT/EP1995/004941 WO1996021049A1 (fr) 1995-01-07 1995-12-13 Procede et dispositif pour separer une phase specifiquement plus legere d'une phase liquide specifiquement plus lourde

Publications (2)

Publication Number Publication Date
EP0800590A1 EP0800590A1 (fr) 1997-10-15
EP0800590B1 true EP0800590B1 (fr) 2002-04-17

Family

ID=7751072

Family Applications (1)

Application Number Title Priority Date Filing Date
EP95942152A Expired - Lifetime EP0800590B1 (fr) 1995-01-07 1995-12-13 Procede et dispositif pour separer une phase specifiquement plus legere d'une phase liquide specifiquement plus lourde

Country Status (6)

Country Link
EP (1) EP0800590B1 (fr)
AT (1) ATE216434T1 (fr)
DE (2) DE19500266C1 (fr)
ES (1) ES2174974T3 (fr)
NO (1) NO319933B1 (fr)
WO (1) WO1996021049A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006059589A1 (de) * 2006-12-16 2008-06-19 Messer Austria Gmbh Vorrichtung und Verfahren zum Behandeln von Werkblei

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU421598B2 (en) * 1968-03-29 1972-02-21 Monzino Riotinto Of Australia Limited Separation of molten materials
AU475319B2 (en) * 1972-09-29 1976-08-19 Metallgesellschaft Aktiengesellschaft Process and apparatus for removing solids formed in the refining of molten lead
FR2276385A1 (fr) * 1974-06-27 1976-01-23 Tech Ind Fonderie Centre Procede pour le decrassage automatique d'un cubilot a prelevement intermittent de la fonte par piquees et cubilot perfectionne selon ce procede
CA1079979A (fr) * 1975-08-19 1980-06-24 Denby H. Ward Elimination du bismuth contenu dans le plomb
DE3016160C2 (de) * 1980-04-26 1982-12-23 Preussag - Boliden - Blei GmbH, 3380 Goslar Vorrichtung zum Entfernen einer auf einer Schmelze befindlichen Schlackenschicht
GB2115009B (en) * 1982-02-11 1985-08-07 Ass Lead Mfg Ltd An improved method of removing dross from a lead refining pot
CA1199180A (fr) * 1982-02-11 1986-01-14 Duncan Ritchie Methode d'extraction de la crasse d'un pot d'affinage du plomb
IN159763B (fr) * 1982-07-16 1987-06-06 Bnf Metals Tech Centre
DE3831898A1 (de) * 1988-09-20 1990-03-29 Preussag Boliden Blei Gmbh Verfahren und vorrichtung zur entfernung von arsen, zinn und antimon aus werkblei mit sauerstoff
DE4322782A1 (de) * 1993-07-08 1995-01-12 Messer Griesheim Gmbh Verfahren zum Entfernen von Zinn, Arsen und Antimon aus schmelzflüssigem Blei

Also Published As

Publication number Publication date
DE59510176D1 (de) 2002-05-23
EP0800590A1 (fr) 1997-10-15
WO1996021049A1 (fr) 1996-07-11
NO973082L (no) 1997-08-14
DE19500266C1 (de) 1996-02-22
ATE216434T1 (de) 2002-05-15
ES2174974T3 (es) 2002-11-16
NO973082D0 (no) 1997-07-02
NO319933B1 (no) 2005-10-03

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