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EP0007890B1 - Procédé pour la production et le raffinage de plomb brut à partir de matières brutes plombifères contenant de l'arsenic - Google Patents

Procédé pour la production et le raffinage de plomb brut à partir de matières brutes plombifères contenant de l'arsenic Download PDF

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Publication number
EP0007890B1
EP0007890B1 EP79850058A EP79850058A EP0007890B1 EP 0007890 B1 EP0007890 B1 EP 0007890B1 EP 79850058 A EP79850058 A EP 79850058A EP 79850058 A EP79850058 A EP 79850058A EP 0007890 B1 EP0007890 B1 EP 0007890B1
Authority
EP
European Patent Office
Prior art keywords
lead
iron
copper
melt
speiss
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
Application number
EP79850058A
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German (de)
English (en)
Other versions
EP0007890A1 (fr
Inventor
Stig Arvid Petersson
Björn-Eric Lundin
Allan Ferdinand Norrö
Bengt Sune Eriksson
Viktor Samuel Erkki Krogerus
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.)
Boliden AB
Original Assignee
Boliden AB
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Filing date
Publication date
Application filed by Boliden AB filed Critical Boliden AB
Priority to AT79850058T priority Critical patent/ATE1752T1/de
Publication of EP0007890A1 publication Critical patent/EP0007890A1/fr
Application granted granted Critical
Publication of EP0007890B1 publication Critical patent/EP0007890B1/fr
Expired legal-status Critical Current

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Classifications

    • 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
    • C22B13/02—Obtaining lead by dry processes
    • 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

Definitions

  • metallic lead is normally produced from sulphidic lead raw-materials, such as concentrates, it is also produced from metallic, oxidic and sulphatic lead raw-materials, such as dust, ashes and slags.
  • the most common furnace for smelting and reducing lead is the shaft furnace, which is charged with lead raw-materials which may have been pre-sintered or roasted to oxidize the sulphidic sulphur with atmospheric oxygen to a content of less than 2% sulphidic sulphur.
  • This smelting and reduction of lead raw-material can also be effected to advantage in an inclined rotary furnace, such as a furnace of the Kaldo-type as described in SE-A-7317217-3 and 7317219-9, which illustrate processes for producing crude lead from sulphidic and from oxidic and sulphatic lead raw-materials.
  • crude lead is meant here, generally, a lead product which must be subjected to further purifying or refining stages, in order to be retailed as a normal market product.
  • the lead When producing crude lead from different raw-materials the lead will thus practically always contain impurities undesirable in the finished lead. Examples of such impurities include copper, arsenic and antimony.
  • the crude lead will normally also contain gold and silver.
  • crude lead must always be refined in order to obtain a sufficiently pure lead, commercially known as a so-called refined lead.
  • the lead is refined in various chambers or pots specifically designed for such refining work.
  • the copper, and above all the arsenic, present in the crude lead create a particular problem when refining said lead, since these impurities may reach 15% or, in certain cases, even higher, which give very large quantities of more or less solid powderous products, normally called dross, on the surface of the metal bath, thereby rendering handling difficult.
  • the arsenic represents a direct threat to the environment, since a significant amount thereof is fumed-off from the pots or chambers during the refining process.
  • Crude lead from shaft furnaces which are tapped at about 1000­ 1100°C, can contain the aforementioned impurities, present in the lead raw-material, in quantities which, in the case of copper, correspond to the solubility limit in lead, which is about 10% at 1100°C, and in respect of arsenic correspond to the amount of arsenic present in the lead raw-material with the exception of that which is fumed-off during the smelting process.
  • arsenic is soluble in lead to an unlimited degree.
  • the said method does not solve the problem of the copper which is dissolved in the lead at the temperatures in question, about 1000°C.
  • Refining of crude lead from shaft furnaces is, as with the aforedescribed process, very time-consuming, since different refining stages must be incorporated at which work is carried out at different temperatures and at different redox potentials.
  • considerable time is taken up in the cooling of the crude-lead melt; from the temperature obtained after the melting process to a temperature suitable for a subsequent refining stage operating at a considerably lower temperature, for example the copper segregation stage.
  • JP-B-1974-28520 there is described a method for removing arsenic from molten lead, in which iron in the form of iron powder, sponge iron or iron filings is charged to the melt.
  • iron in the form of iron powder, sponge iron or iron filings is charged to the melt.
  • more than 1% iron is charged at a temperature above 450°C, whereafter the lead melt is stirred mechanically.
  • treatment is carried out in a crucible at temperatures above 450°C and up to 800°C, wherein a finely-divided solid speiss, for example in powder form or in the form of coarse grains, is removed from the melt.
  • the present invention substantially eliminates the aforedescribed problems. Moreover, the method according to the invention enables extremely rapid reaction sequences to be obtained whilst requiring a relatively low energy input, which are important and decisive factors in respect of the economy of the process.
  • the lead raw-material may be of the metallic, sulphidic, oxidic or sulphatic type, and may comprise, for example, various dust products and powderous products obtained from non-ferrous metallurgical processes.
  • the lead raw-material is melted in a furnace, in which turbulence of the content can be created, in the presence of a slag former, and a reducing agent is supplied to reduce the resultant lead-containing slag, whereafter the slag is drawnoff, said method being characterized by the fact that subsequent to drawing-off the slag, there is charged in a surplus to the furnace at a temperature of 800-1200°C under strong turbulence, iron in a metallic, finely-divided form, or iron is caused to be formed in situ, optionally before drawing-off the slag, whereafter the insoluble liquid iron speiss formed in the lead melt is separated therefrom in immediate conjunction with a gravitational separation of speiss and crude lead.
  • iron in a finely-divided form is meant metallic iron in a form such as to present a relatively high specific surface area to the lead melt and such that the iron can be charged to the lead melt in a simple manner.
  • the lead raw-material is charged to the furnace prior to or during the melting process, together with a slag former.
  • the crude lead is reduced chemically in a known manner and the resultant lead-containing slag is chemically reduced, suitably with coke for example, until the lead content of the slag is sufficiently low, for example less than 2%.
  • the slag, purified from lead is then tapped off.
  • further lead raw-material can then be charged to the furnace and the slag reduced to a lead content of less than 2% and the slag tapped-off, in a repeated number of operations.
  • a "speiss” is a compound of arsenic and/or antimony with iron metals and/or copper, i.e. a “speiss” may comprise arsenides and/or antimonides of one or more of the metals copper, iron, nickel and cobalt.
  • Formed iron-arsenic-speiss is practically insoluble in a lead melt, and hence it readily separates, floats to the surface and lies above the lead melt and can be poured therefrom in a liquid state at a temperature of 800-1150°C.
  • a temperature range of 950-1000 0 C is preferred, due to the viscosity of the speiss, which enables rapid separation and tapping.
  • the iron charged to the furnace may conveniently comprise an iron alloy containing more than about 60% iron.
  • any copper impurities present are then suitably frozen out from the lead melt during turbulence thereof in said furnace, by adding a coolant to the melt to cool the same to a temperature of between 400 and 600°C, whereafter crude lead is tapped-off, said lead being free from copper and arsenic.
  • the coolant may conveniently have the form of an oxidic or sulphatic lead raw-material or a crushed iron- silicate slag.
  • a rapid and effective cooling effect is obtained when the coolant is water, which is injected directly into the furnace in a liquid, finely-divided form.
  • it may also be suitable for the coolant to comprise a slag former intended for a subsequent melting operation.
  • copper-freezing step it is possible to leave the copper-freezing step until several charges of lead raw-materials have been melted and treated with iron, and thus to retain the frozen-out copper or copper and speiss in the furnace during at least one further melting cycle.
  • Copper can also be removed from the crude-lead melt as a copper speiss.
  • a copper speiss is formed when the temperature is lowered to less than 1100°C.
  • the whole ratio between copper and free arsenic must be between 1.17 and 4.43.
  • iron is suitably added to form an iron speiss in order to raise the mole ratio, to enable segregation of a copper speiss when cooling. Further arsenic can then be removed, by charging more iron to the furnace.
  • the melt also contains recoverable quantities of tin
  • iron is suitably charged in an amount which will ensure that sufficient arsenic remains in the melt to form copper speiss, for example Cu 3 As.
  • copper speiss for example Cu 3 As.
  • the tin content will exist in a metallic solution in the lead melt, which can be retailed in the form of tin-containing lead, which can demand a higher price on the market.
  • iron can be caused to form in situ in the melt, preferably by adding silicon, silicides, carbon, carbides or ferro-alloys containing carbon and silicon in such quantities that iron present in the slag is reduced out in metallic form prior to removing the slag.
  • the melting capacity of the furnace can be utilized to the maximum, since the formation of speiss in a charge of about 30-40 tons is obtained already after 30 minutes and, when cooling, the heat content of the lead can be recovered by, as aforementioned, using as the coolant a quantity of slag former intended for a subsequent process, said slag former thus being preheated in readiness for said subsequent process. If so desired, the melt of lead raw-material can also be cooled by charging a part of a subsequent charge of lead raw-material.
  • the melting process, and also the formation of speiss and the segregation of copper, are effected in a furnace in which the melt can be treated whilst being strongly agitated.
  • a furnace in which the melt can be treated whilst being strongly agitated.
  • One suitable furnace in this respect is a topblown 'rotary converter, known as a TBRC converter or a Kaldo furnace.
  • a TBRC converter or a Kaldo furnace can be rotated at a speed of from 10 to 60 r.p.m., the choice of suitable rotary speed being controlled by the diameter of the furnace.
  • a suitable turbulence or agitation can be obtained when the inside of the furnace moves at a peripheral speed of 0.5-7 m/s, preferably 2-5 m/s, which enables the melt to accompany the rotating inner surface of the furnace and fall down onto the surface of the bath in droplet form, which results in extremely good contact between solid phase, liquid phase and gas phase. Good contact is a prerequisite of rapid chemical and physical sequences, such as reduction sequence, cooling and separation.
  • the formation of dust is avoided to a surprisingly high degree, owing to the fact that the shower of droplets falling down onto said surface drive down that dust which would otherwise leave the furnace with the reaction gases.
  • the slag and the crude-lead bath were chemically reduced with 1.3 tons of coke until the lead content of the slag was about 1.5% at a temperature of about 1000°C, whereafter the slag was tapped-off. 3.0 tons of iron filings were then charged to the furnace, the arsenic content of the melt during rotation of the converter at a speed of about 30 r.p.m. falling from 7.3% to less than 0.01%.
  • it is extremely important that the speiss formation is effected with good contact between the iron and lead phase with an iron surplus of at least 20% above the stoichiometric value.
  • the temperature during the formation of spiess was in excess of 1000°C.
  • the formed and separated speiss phase was tapped-off immediately the converter stopped rotating, since in a stationary crude-lead bath some arsenic will redissolve in the crude-lead melt from the speiss.
  • Example 1 30 tons of oxidic-sulphatic pellets of the kind and composition recited in Example 1 were melted in a manner similar to that described in Example 1, with 9 tons of fayalite slag and 2.25 tons of limestone in a Kaldo converter, whilst burning oil with oxygen. Subsequent to melting the pellets, the slag and crude lead were chemically reduced at a temperature of 1000°C with 1.3 tons of coke, until the lead content of the slag was about 1.5%, whereafter about 70% of the slag was tapped-off from the converter. About 1.5 tons of silicon iron, FeSi, were then charged to the converter, to reduce the remainder of the slag and to form a speiss.
  • the converter was rotated at a speed of about 25 r.p.m., whereupon the arsenic content fell from an original 5%, firstly to about 1.3% and then, during the rotation of the converter for about one hour and subsequent to the charge of silicon iron, to about 0.4%.
  • Oxidic-sulphatic pellets mixed with pellets of metallic and sulphidic type were melted with fayalite slag and limestone in a manner similar to that described in Example 1. Resulting in a crude-lead melt of about 15 tons having the following composition: lead 84.4%, copper 2.7%, arsenic 5.5% and tin 1.4%.
  • the melt was rolled at 1100°C and 1200 kg of iron filings were added and rolling of the melt continued at 30 r.p.m. for some minutes, an iron speiss being formed.
  • the speiss was tapped-off and the resultant lead melt had the following composition: lead 86.1 %, copper 2.4%, arsenic 1.1 %, tin 1.3%.
  • the mole ratio of copper to arsenic was 2.6.
  • the melt was then cooled to 450°C by injecting water thereinto whilst the furnace was rotating, a copper-speiss-copper- dross segregating out.
  • the resultant lead melt had the following composition: lead 96.3%, copper 0.1 %, arsenic 0.01% and tin 1.3%.
  • Example 3 it will be evident from Example 3 that by limiting the iron charge in a manner such as to obtain in the crude-lead melt a copper/arsenic mole ratio of 2.6, it is possible to avoid losing the tin content to speiss phases in the form of copper-tin-compounds from which tin is not readily recoverable.
  • a lead which contains tin has a very high commercial value.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Saccharide Compounds (AREA)
  • Seasonings (AREA)
  • Steroid Compounds (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Treatment Of Steel In Its Molten State (AREA)

Claims (13)

1. Procédé de fabrication et de raffinage de plomb brut à partir de matières brutes plombifères contenant de l'arsenic de nature métallique ou sous la forme d'oxyde, de sulfate ou de sulfure, dans lequel la matière brute plombifère est fondue dans un four en présence d'un agent de formation de scorie, ce four étant du type dans lequel une turbulence peut être créée dans le contenu de celui-ci, et dans lequel un agent de réduction est amené pour réduire la scorie contenant du plomb résultante, la scorie étant ensuite extraite, caractérisé en ce que l'on amène du fer sous une forme finement divisée, métallique sous la forme d'un surplus dans la masse fondue avant l'extraction de la scorie ou en ce qu'on y provoque sa formation in situ, éventuellement avant l'extraction de la scorie, à une température de 8000-12000C au cours d'une turbulence intense de la masse fondue, après quoi le speiss de fer insoluble formé dans la masse fondue de plomb est séparé sous forme liquide de la masse fondue précitée immédiatement conjointement à une séparation par gravitation du speiss et du plomb brut.
2. Procédé suivant la revendication 1, caractérisé en ce que le fer amené au four est sous la forme de limailles de fer, de poudre de fer ou de morceaux finement divisés.
3. Procédé suivant la revendication 1, caractérisé en ce que le fer comprend un alliage de fer contenant plus de 60% de fer.
4. Procédé suivant la revendication 1, caractérisé en ce que l'on provoque la formation du fer in situ dans la masse fondue par addition de silicium, de siliciures, de carbone, de carbures ou de ferro-alliages contenant du carbone et du silicium en des quantités telles que le fer dans la scorie est réduit sous forme métallique avant l'évacuation par coulée de la scorie.
5. Procédé-suivant la revendication 1, caractérisé en ce que le speiss est évacué par coulée à une température de 950°-1000°C.
6. Procédé suivant l'une quelconque des revendications 1 à 5, caractérisé en ce que les éventuelles impuretés de cuivre sont séparées par solidification de la masse fondue de plomb après la séparation d'arsenic pendant la turbulence de celle-ci dans le four précité, par addition d'une matière de refroidissement pour refroidir la masse fondue à une température se situant entre 4000-6000C, le plomb brut étant ensuite évacué par coulée.
7. Procédé suivant la revendication 1, caractérisé en ce que lorsque du cuivre est présent dans la masse fondue de plomb brut et lorsque le rapport molaire entre le cuivre et l'arsenic libre se situe entre 1,17 et 4,43, on forme un speiss de cuivre avant la formation du speiss de fer précité, par refroidissement de la masse fondue à une température en dessous de 1100°C, le speiss de cuivre formé étant ensuite évacué par coulée.
8. Procédé suivant la revendication 7, caractérisé en ce que l'on introduit du fer dans la masse fondue de plomb en une quantité suffisante pour élever le rapport molaire entre le cuivre et l'arsenic libre entre 1,17 et 4,43 avant d'abaisser la température pour former le speiss de cuivre précité, ledit speiss de cuivre étant ensuite évacué par coulée et du fer supplémentaire étant amené au four pour séparer complètement l'arsenic.
9. Procédé suivant la revendication 6, caractérisé en ce que la matière de refroidissement utilisée est une matière brute plombifère sous la forme d'oxyde ou de sulfate ou une scorie de fer-silicate broyée.
10. Procédé suivant la revendication 6, caractérisé en ce que la matière de refroidissement utilisée est l'eau, qui est injectée directement dans le four sous une forme finement divisée, liquide.
11. Procédé suivant la revendication 6, caractérisé en ce que la matière de refroidissement utilisée comprend un agent de formation de scorie pour une fusion ultérieure de la matière brute plombifère.
12. Procédé suivant la revendication 6, caractérisé en ce que le cuivre ou le cuivre et le speiss séparés par solidification est ou sont retenus dans le four pendant au moins un nouveau cycle de fusion.
13. Procédé suivant la revendication 1, caractérisé en ce que les procédés de fabrication et de raffinage sont effectués dans un four incliné, rotatif du type Kaldo.
EP79850058A 1978-06-29 1979-06-15 Procédé pour la production et le raffinage de plomb brut à partir de matières brutes plombifères contenant de l'arsenic Expired EP0007890B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT79850058T ATE1752T1 (de) 1978-06-29 1979-06-15 Verfahren zur gewinnung und reinigung von rohblei aus arsen enthaltenden blei-rohmaterialien.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE7807357A SE412766B (sv) 1978-06-29 1978-06-29 Forfarande for framstellning och raffinering av rably ur arsenikhaltiga blyravaror
SE7807357 1978-06-29

Publications (2)

Publication Number Publication Date
EP0007890A1 EP0007890A1 (fr) 1980-02-06
EP0007890B1 true EP0007890B1 (fr) 1982-11-03

Family

ID=20335338

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Application Number Title Priority Date Filing Date
EP79850058A Expired EP0007890B1 (fr) 1978-06-29 1979-06-15 Procédé pour la production et le raffinage de plomb brut à partir de matières brutes plombifères contenant de l'arsenic

Country Status (8)

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EP (1) EP0007890B1 (fr)
AT (1) ATE1752T1 (fr)
DE (1) DE2963968D1 (fr)
DK (1) DK148810C (fr)
FI (1) FI68265C (fr)
NO (1) NO152516C (fr)
PL (1) PL117462B1 (fr)
SE (1) SE412766B (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE436045B (sv) * 1983-05-02 1984-11-05 Boliden Ab Forfarande for framstellning av rably ur svavelinnehallande oxidiska blyravaror
IN160772B (fr) * 1983-05-05 1987-08-01 Boliden Ab
DE3922073A1 (de) * 1989-07-05 1991-01-17 Metallgesellschaft Ag Verfahren zum entfernen von thallium aus werkblei
US5223021A (en) * 1992-02-13 1993-06-29 E. I. Du Pont De Nemours And Company Iron as a co-additive in refining crude lead bullion
US5183497A (en) * 1992-02-13 1993-02-02 E. I. Du Pont De Nemours And Company Iron and a copper speiss as co-additives in refining crude lead bullion
US5183496A (en) * 1992-02-13 1993-02-02 E. I. Du Pont De Nemours And Company Copper speiss as a co-additive in refining crude lead bullion
RU2364639C2 (ru) * 2007-03-16 2009-08-20 Байкальский институт природопользования Сибирского отделения Российской академии наук (БИП СО РАН) Способ переработки труднообогатимой окисленной свинцовой руды
CN116949291B (zh) * 2023-06-12 2025-11-18 中国恩菲工程技术有限公司 一种高砷多金属危废的综合回收方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1283427A (en) * 1915-05-06 1918-10-29 Fred A Stief Refining lead alloys and alloys containing lead, tin, copper, or antimony.
US4017308A (en) * 1973-12-20 1977-04-12 Boliden Aktiebolag Smelting and reduction of oxidic and sulphated lead material
DE2454756A1 (de) * 1974-11-19 1976-05-26 Hermetic Pumpen Gmbh Spaltrohrmotorpumpe
BE841411A (fr) * 1976-02-27 1976-09-01 Fusion electrique de residus de sulfates de plomb
DE8317214U1 (de) * 1983-06-13 1984-09-13 Jagenberg AG, 4000 Düsseldorf Bahntrennvorrichtung an wickelmaschinen

Also Published As

Publication number Publication date
PL216607A1 (fr) 1980-03-24
DE2963968D1 (en) 1982-12-09
SE412766B (sv) 1980-03-17
ATE1752T1 (de) 1982-11-15
NO152516B (no) 1985-07-01
DK271379A (da) 1979-12-30
DK148810C (da) 1986-03-24
NO792174L (no) 1980-01-03
DK148810B (da) 1985-10-07
FI792060A7 (fi) 1979-12-30
SE7807357L (sv) 1979-12-30
PL117462B1 (en) 1981-08-31
FI68265C (fi) 1985-08-12
NO152516C (no) 1985-10-09
EP0007890A1 (fr) 1980-02-06
FI68265B (fi) 1985-04-30

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