EP2106454B1 - Vorrichtung und verfahren zum behandeln von werkblei - Google Patents

Vorrichtung und verfahren zum behandeln von werkblei Download PDF

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Publication number
EP2106454B1
EP2106454B1 EP07822541A EP07822541A EP2106454B1 EP 2106454 B1 EP2106454 B1 EP 2106454B1 EP 07822541 A EP07822541 A EP 07822541A EP 07822541 A EP07822541 A EP 07822541A EP 2106454 B1 EP2106454 B1 EP 2106454B1
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EP
European Patent Office
Prior art keywords
lead
reaction vessel
oxidant
bath
gas
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.)
Active
Application number
EP07822541A
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German (de)
English (en)
French (fr)
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EP2106454A1 (de
Inventor
Michael Potesser
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.)
Messer Austria GmbH
Original Assignee
Messer Austria 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 Messer Austria GmbH filed Critical Messer Austria GmbH
Priority to SI200730967T priority Critical patent/SI2106454T1/sl
Priority to PL07822541T priority patent/PL2106454T3/pl
Publication of EP2106454A1 publication Critical patent/EP2106454A1/de
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Publication of EP2106454B1 publication Critical patent/EP2106454B1/de
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D1/00—Treatment of fused masses in the ladle or the supply runners before casting
    • B22D1/002—Treatment with gases
    • B22D1/005—Injection assemblies therefor
    • 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

Definitions

  • the invention relates to the use of a device and a method for treating lead lead.
  • the Harris process uses caustic soda and nitric oxide as the oxidant. With a pump, the molten lead to be refined is pumped into an intermediate container, wherein the deposited oxides are obtained in a salt slag. The slag must then be processed consuming consuming.
  • oxygen is introduced with a lance immersed in the lead bath under high pressure in a turbulent flow of liquid lead concentrated to a proportionate volume, relative to the melting vessel.
  • the oxygen-intimately mixed lead enters into a larger volume to calm down, in which the oxides float and are scraped off.
  • the turbulent flow of lead is generated by the strong flow of oxygen from the lance and by a lead pump that pumps the lead into a reaction tube.
  • the reaction tube is arranged in a second cylinder of larger volume, from which the oxides are withdrawn.
  • the lead flows through a bottom outlet port.
  • the oxygen outlet region of a gas nozzle for injecting oxygen into molten lead is enveloped by a protective gas.
  • the protective gas preferably nitrogen (N 2 ), carbon dioxide (CO 2 ) or argon (Ar), is introduced via a separate inert gas supply into an outer tube surrounding the actual oxygen nozzle.
  • N 2 nitrogen
  • CO 2 carbon dioxide
  • Ar argon
  • a lead-free cavity is formed in front of the gas nozzle, and thus the reaction site is displaced from the exit of the gas nozzle into the bath of lead melt.
  • the contact between molten lead and gas nozzle is avoided by the simultaneous formation of a protective gas cushion surrounding at least the outlet region.
  • the gas nozzle is cooled from the outside by the inert shielding gas.
  • the oxidation is improved by the high velocity, preferably sonic velocity, injected into the molten lead gas inert gas, because this the turbulent mixing of lead melt and oxygen is increased.
  • the inert gas is also used as a mixed gas, which is added to the oxygen.
  • the oxygen input is adapted to the sinking offer of antimony in the melt and excessive oxidation of lead is avoided.
  • the US 4,496,394 discloses a solution, but not with a purge stone , A disadvantage of this method is the rather high proportion of non-reacted oxygen flowing through the melt unused. The reaction is therefore slow. An acceleration must be bought with a high consumption of oxygen.
  • the object of the invention is therefore to provide a way to remove antimony, arsenic and tin from lead by means of a gaseous oxidizing agent, in which the efficiency in carrying out the reaction over the prior art method is increased.
  • This object is achieved by a use of the features of patent claim 10 and by a method having the features of claim 1
  • apparatus for removing tin, antimony and arsenic from lead which is equipped with a reaction vessel for holding a bath of liquid lead and a gas supply system for introducing a gaseous oxidant into the reaction vessel, the gas supply system being a sink located in the bottom of the reaction vessel for bubbling the oxidizing agent.
  • the reaction vessel can be structurally separated from a lead-absorbing lead or lead bath. Refining boiler to be installed in or next to this, in each case a flow connection between the two, which allows a continuous or batchwise treatment of the lead from the lead boiler.
  • the device injects gas bubbles from the feed channels of the entry means located in the bottom of the reaction vessel traverse the entire lead bath from bottom to top with the least possible speed.
  • the large surface area of the gas bubbles and the long residence time of the gas bubbles in the bath ensure a very effective oxidation of the foreign metals contained in the lead.
  • a purging plug is used as the insertion device, by means of which it is possible to introduce a gaseous oxidizing agent in the form of the smallest possible gas bubbles distributed as widely as possible in the lead bath, and which is resistant to the molten lead temperatures.
  • Flushing stones for bubbling gases into metallurgical melts are known per se, but have not hitherto been used to treat lead lead.
  • Such purging blocks are made of a gas-permeable and heat-resistant material such as ceramic.
  • a variety of fine, extending through the block of the purging plug through channels allows the bubbling of the oxidant in the form of fine gas bubbles.
  • An overview of different types of purging stones and their applications can be found for example in the WO 92/04473 A1 , In particular, the following types of purging blocks are distinguished, which can also be used in the context of the invention: joint washer, dishwasher with undirected porosity and dishwasher with directed porosity.
  • the formation of gas bubbles of different size, shape and different path movement succeeds in ascending the lead bath.
  • reaction vessel has the shape of a substantially upright cylinder and the insertion device extends over a substantial part of the base surface of the reaction vessel.
  • the entry device can also occupy virtually the entire footprint.
  • the two-dimensional entry of the oxidizing agent causes a particularly large volume of the lead bath to be brought into contact with oxidizing agent.
  • the reaction vessel is equipped with at least one supply line and with at least one lead for molten lead, whereby a continuous operation of the reaction vessel is made possible.
  • a yet further preferred embodiment of the invention provides, the at least one supply line and the at least one discharge vertically from each other spaced to arrange. This makes it possible to produce a directed or rotating, upward or downward flow of the work lead in cocurrent or countercurrent to the gas inlet in the reaction vessel.
  • the desired reaction is further favored; in counterflow, the difference in concentration of the gas bubbles and the lead bath leads to a higher refining depth, in the case of a rectified flow, the contact duration of the lead is prolonged at the surface of the gas bubbles.
  • reaction vessel in the reaction vessel and / or in the supply lines and or discharges tempering for heating or cooling of the molten lead are provided, which ensure a constant temperature in the lead bath or boiler during the treatment of the lead.
  • the object of the invention is also achieved by a process for the removal of tin, antimony and arsenic from lead, in which a lead bath of liquid lead is contacted with a gaseous oxidant in a reaction vessel, metallic lead contained in the lead reacts with the oxidizing agent and the reaction products are subsequently removed, and characterized in that the oxidizing agent is bubbled into the lead bath by means of an introduction device arranged in the bottom region of the reaction vessel in the form of gas bubbles.
  • the supply of the oxidant in the form of as many and as small as possible gas bubbles, which are widely distributed in the volume of the lead bath and ascend as slowly as possible, increases the efficiency of the reaction compared to prior art methods in which the oxidant is introduced by means of lances in the lead bath ,
  • the residence time of the gas bubbles in the lead bath is further increased by the fact that the gas bubbles describe a zigzag or helical trajectory when ascending through the bath of liquid lead.
  • the gas bubbles In order to have the largest possible surface area for the reaction, it is advantageous if the gas bubbles have an approximately hemispherical or elliptical shape.
  • the size and shape of the gas bubbles introduced, as well as the path described by the gas bubbles (hereinafter referred to as "bubble parameters") significantly determined by the entry system and by the purity and the geometric properties of the lead bath. It can be determined empirically or by simulation calculations, which entry system leads when used in each lead bath to which bubble parameters. Thus, the suitable for the particular application system can be determined prior to treatment and installed in the reaction vessel.
  • the gas bubbles have on exit from the entry device on average a volume of less than 500 mm 3 , preferably less than 0.5 mm 3 .
  • the use of the method according to the invention proves to be particularly advantageous in continuous operation, that is to say with continuous supply of work lead with simultaneous removal of treated lead.
  • a certain, compared to the unprocessed lead lead reduced content of tin, antimony and / or arsenic is specified in the reaction vessel and regulated the supply / discharge of lead and / or the amount and / or composition of the oxidizing agent towards these parameters.
  • a preferred embodiment of the method according to the invention provides that the liquid Maschinenblei is passed in countercurrent or direct current to the ascending oxidant through the reaction vessel. Also advantageous is an upward or downward helical guidance of the liquid lead.
  • the production of a correspondingly directed flow in the lead can be carried out by means of suitable arranged in the reaction vessel pumps, agitators o. The like. Or by a continuous supply of liquid Maschinenblei from the outside and a suitable arrangement of one or more merging into the reaction vessel inflows and outlets for the liquid lead.
  • a particularly advantageous embodiment of the invention provides for a recirculation of the work lead including the reaction vessel.
  • the lead is in contact with the oxidant for so long until the content of tin, antimony and arsenic falls below a certain pre-selected limit.
  • Such recirculation may also be combined with continuous feed of lead, with a fixed value for the content of tin, antimony and / or arsenic being defined as the target to be met during continuous operation.
  • the lead supplied to the reaction vessel and / or the amount and / or composition of the oxidant fed to the reaction vessel are controlled.
  • the control is expediently carried out as a function of predetermined values of certain reaction parameters, such as, for example, the temperature in the reaction vessel or the contents of tin, arsenic, and / or antimony in the lead bath or the oxygen content in the oxidizing agent.
  • FIG. 1 shows schematically a device according to the invention for treating lead lead.
  • the device 1 comprises an approximately cylindrical reaction vessel 2 for receiving a lead bath 3 of molten lead.
  • the reaction products formed in the reaction lead to the formation of dross, which accumulates on the surface of the lead bath 3 as a so-called "smear".
  • the supply of liquid Werkblei to the reaction vessel 2 via a supply line 4, which opens laterally in the lower part of the reaction vessel 2 in this.
  • a plurality of leads which are arranged for example at regular angular intervals in the side wall of the reaction vessel 2.
  • the supply line or the supply lines can be arranged such that the liquid Maschinenblei is introduced with a tangential flow component in the reaction vessel 2, to a circular or helical flow in the interior of the reaction vessel 2 to enable.
  • the liquid lead is brought from a lead boiler 5 by means of a lead 4 arranged in the lead pump 7.
  • the lead boiler 5 can also be located above the reaction vessel 2, so that the supply of Maschinenbleis can be done by external gravity even without external energy.
  • a heating device 8 is arranged in the supply line 4, by means of which the work lead can be heated to a predetermined temperature.
  • a discharge 11 is provided which at the same time determines the filling level 10 of the lead bath 3.
  • both treated, ie, antimony, arsenic and tin, at least partially liberated work lead, and also detritus floating on the surface of the lead bath, are removed.
  • the dross is optionally skimmed off and removed by means of a known separation device 12.
  • the treated lead then passes back by its own gravity and / or by means of a conveyor 14 to the lead boiler 5, from where it is either pumped in a recycle again in the reaction vessel 2 or a further treatment step, such as the removal of precious metals, zinc or bismuth ,
  • a cooling device 16 is further provided, in which the Werkblei, which is heated due to the running in the reaction vessel 2 exothermic oxidation reaction can be cooled to a predetermined temperature value, if the temperature differences require it.
  • a supply means 18 for an oxidizing agent or cooling gas is provided in the lower part of the reaction vessel 2.
  • the feed device 18 comprises an entry device 19, which in the exemplary embodiment is a purge stone which extends substantially over the entire bottom surface of the reaction vessel 2, as well as an oxidant supply line 20 operatively connected to the entry device 19.
  • the purge block is for example made of one made of porous, ceramic material. Due to the porosity of the material, gas permeable microchannels extend through the entire body of the purging plug, through which the oxidizing agent flows from the oxidant supply line 20 into the lead bath.
  • the oxidant supply line 20 is connected to gas supply lines 21,22 connected via the oxygen (gas supply line 21) or an inert gas (gas supply line 22), for example nitrogen, from corresponding, not shown pressure vessels into the oxidant supply line 20 can be fed. If the corresponding gases stored in the pressure vessel under high pressure, a here also not shown reducing valve for adjusting the pressure to, for example, 5 bar is provided in the supply lines 21,22.
  • molten Maschinenblei is brought from the lead boiler 5 via the supply line 4 and thereby brought in the heater 8 to the desired reaction temperature of, for example, 700-750 ° C.
  • the desired reaction temperature for example, 700-750 ° C.
  • the reaction vessel 2 is filled to the filling level 10 with molten Maschinenblei.
  • the lead is discharged via the outlet 11, whereby an upward flow is generated in the reaction vessel 2. It is also possible to regulate the temperature and / or the concentration of tin, antimony and / or arsenic in the lead bath 3 via the flow of the added or discharged factory lead.
  • an oxidizing agent is introduced, for example, at a pressure of 5 bar.
  • the oxidizing agent is, for example, oxygen, air or a mixture of oxygen and an inert gas, for example nitrogen.
  • the composition of the oxidizing agent remains the same during the treatment period or is adapted to the requirements of the reaction taking place in the reaction vessel 2.
  • the supply of oxygen and / or nitrogen via valves not shown here in the gas supply lines 21,22 set and, for example, depending on measured parameters, such as the tin antimony and / or arsenic concentration in the lead bath 3 or the temperature of Lead baths 3, to be regulated.
  • the oxidant permeates the Sink 19 and pearls at the lead bath 3 side facing in the lead bath 3 in the form of small gas bubbles 23 a.
  • the oxidizing agent on the surface of the gas bubbles 23 reacts with foreign metals present in the lead bath 3.
  • oxidation takes place with the metals tin, arsenic and antimony.
  • the largest possible reaction surface ie the largest possible number of small and “deformed” (ie non-spherical), gas bubbles 23 and the longest possible duration of residence of the gas bubbles 23 in the lead bath 3 is helpful; ideally, the gas bubbles 23 have an ellipsoidal bubble shape and a diameter of less than 5 mm and rise in the lead bath 3 in a zigzag or helical path. Shape, size and movement of the bubble 23 gas bubbles are determined in particular by the purging plug used, which is selected accordingly for this purpose.
  • the rectified to the upward movement of the gas bubbles 23 flow of Werkbleis in lead bath 23 thereby extends the contact time of the reactants together and thereby favors the reaction.
  • the oxidized metals accumulate in the form of dross on the surface of the lead bath 3 and are skimmed off at the separating device 12, or fed to the lead boiler 5.
  • the unreacted oxidizing agent and any inert gases admixed with the oxidizing agent are collected in a gas space 24 and removed via a gas outlet 25 or the outlet 11. This gas is then available for further utilization and, for example, can also be fed back into the oxidant supply line 20.
  • the lead lead taken from the lead boiler 5 can be circulated until predetermined limits of the concentration of tin, antimony and / or arsenic are reached.
  • concentration of tin, antimony and / or arsenic are reached.
  • levels in the reaction vessel of, for example, 0.02-0.05 mass% Sb and / or 0.003 vol% As being maintained.
  • the invention provides a refining process for lead, improved over the prior art.
  • the process step customary for the refining of lead lead for the removal of tin, antimony and arsenic from the lead is substantially accelerated; the formation of dross is reduced and thus the lead slag is reduced.

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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)
  • Manufacture And Refinement Of Metals (AREA)
EP07822541A 2006-12-16 2007-11-13 Vorrichtung und verfahren zum behandeln von werkblei Active EP2106454B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
SI200730967T SI2106454T1 (sl) 2006-12-16 2007-11-13 Naprava in postopek za obdelavo surovega svinca
PL07822541T PL2106454T3 (pl) 2006-12-16 2007-11-13 Urządzenie i sposób obróbki surowego ołowiu

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006059589A DE102006059589A1 (de) 2006-12-16 2006-12-16 Vorrichtung und Verfahren zum Behandeln von Werkblei
PCT/EP2007/062268 WO2008074575A1 (de) 2006-12-16 2007-11-13 Vorrichtung und verfahren zum behandeln von werkblei

Publications (2)

Publication Number Publication Date
EP2106454A1 EP2106454A1 (de) 2009-10-07
EP2106454B1 true EP2106454B1 (de) 2012-04-25

Family

ID=39278329

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07822541A Active EP2106454B1 (de) 2006-12-16 2007-11-13 Vorrichtung und verfahren zum behandeln von werkblei

Country Status (7)

Country Link
EP (1) EP2106454B1 (pl)
AT (1) ATE555221T1 (pl)
DE (1) DE102006059589A1 (pl)
ES (1) ES2386910T3 (pl)
PL (1) PL2106454T3 (pl)
SI (1) SI2106454T1 (pl)
WO (1) WO2008074575A1 (pl)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104593615A (zh) * 2014-12-30 2015-05-06 河南豫光金铅股份有限公司 一种采用电解析出铅生产合金的装置及工艺

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102015116615B4 (de) 2015-09-30 2023-12-07 Jl Goslar Gmbh Verfahren zum Reinigen einer Bleischmelze
CN115478170A (zh) * 2022-09-06 2022-12-16 湖北大江环保科技股份有限公司 铅冶炼过程中粗氧化锡产出的工艺

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2155545A (en) * 1935-07-13 1939-04-25 American Metal Co Ltd Removal of tin from lead containing tin and other impurities
US2871008A (en) * 1950-11-02 1959-01-27 Air Liquide Apparatus for gas flushing of molten metal
GB1421793A (en) * 1973-06-20 1976-01-21 Electricity Council Injectors for injecting gas into molten metal
IN159763B (pl) * 1982-07-16 1987-06-06 Bnf Metals Tech Centre
DE8906130U1 (de) * 1989-05-18 1989-08-10 Radex-Heraklith Industriebeteiligungs AG, Wien Feuerfester keramischer Spülstein
EP0547080B1 (de) * 1990-09-08 1994-11-30 Veitsch-Radex Aktiengesellschaft für feuerfeste Erzeugnisse Spülstein zum durchleiten von gasen und/oder feststoffen in die schmelze eines metallurgischen gefässes sowie verfahren zu seiner herstellung
DE4322782A1 (de) * 1993-07-08 1995-01-12 Messer Griesheim Gmbh Verfahren zum Entfernen von Zinn, Arsen und Antimon aus schmelzflüssigem Blei
DE19500266C1 (de) * 1995-01-07 1996-02-22 Metallgesellschaft Ag Verfahren und Vorrichtung zur Trennung einer spezifisch leichteren Phase von einer spezifisch schwereren flüssigen Phase

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104593615A (zh) * 2014-12-30 2015-05-06 河南豫光金铅股份有限公司 一种采用电解析出铅生产合金的装置及工艺

Also Published As

Publication number Publication date
DE102006059589A1 (de) 2008-06-19
ES2386910T3 (es) 2012-09-05
SI2106454T1 (sl) 2012-08-31
ATE555221T1 (de) 2012-05-15
WO2008074575A1 (de) 2008-06-26
EP2106454A1 (de) 2009-10-07
PL2106454T3 (pl) 2012-09-28

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