Results of research on removal of lead from synthetic and industrial Cu-Pb-Fe alloy with argon barbotage are presented. For examinations was taken a synthetic alloy and industrial alloy coming “Glogow II” Copperworks. As basic research equipment was used a pipe resistance furnace enabling heating of samples up to 1 473 K. Examinations were made in 2 test series. The 1 series was performed on the synthetic alloy, while in 2 series was used an industrial alloy. All series were conducted at 1 473 K and with gas fl ow 5,55•10-6, 6,94•10-6, 8,33•10-6, 9,72•10-6 m3•s-1

B. Oleksiak

G. Siwiec

Results of research on removal of lead from synthetic and industrial Cu-Pb-Fe alloy with argon barbotage are presented. For examinations was taken a synthetic alloy and industrial alloy coming “Glogow II” Copperworks. As basic research equipment was used a pipe resistance furnace enabling heating of samples up to 1 473 K. Examinations were made in 2 test series. The 1 series was performed on the synthetic alloy, while in 2 series was used an industrial alloy. All series were conducted at 1 473 K and with gas fl ow 5,55•10-6, 6,94•10-6, 8,33•10-6, 9,72•10-6 m3•s-1

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25 METALURGIJA 51 (2012) 1, 25-27B. OLEKSIAK, G. SIWIEC REMOVAL OF LEAD FROM THE INDUSTRIAL AND SYNTHETIC Cu-Pb-Fe ALLOY WITH ARGON BARBOTAGEReceived – Prispjelo: 2011-01-12Accepted – Prihvaćeno: 2011-03-28Original Scientifi  c Paper – Izvorni znanstveni radISSN 0543-5846METABK 51(1) 25-27 (2012)UDC – UDK 669.2/:669.4:669.3:621.694:546.293=111Results of research on removal of lead from synthetic and industrial Cu-Pb-Fe alloy with argon barbotage are pre-sented. For examinations was taken a synthetic alloy and industrial alloy coming “Glogow II” Copperworks. As basic research equipment was used a pipe resistance furnace enabling heating of samples up to 1 473 K. Examinations were made in 2 test series. The 1 series was performed on the synthetic alloy, while in 2 series was used an indus-trial alloy. All series were conducted at 1 473 K and with gas fl  ow 5,55·10-6, 6,94·10-6, 8,33·10-6, 9,72·10-6 m3·s-1.Key words: metallurgy, barbotage, copper, refi  ning, alloyOdstranjivanje olova iz industrijske i sintetičke Cu-Pb-Fe legure argonskim pročišćavanjem. Daju se rezul-tati istraživanja odstranjivanja olova iz sintetičke i industrijske Cu-Pb-Fe legure argonskim pročišćavanjem. Za ispitiva  nje odabrana je sintetička industrijska legura iz tvrtke za bakar “Glogow II”. Osnovni uređaj za istraživanje je cje  vasta peć sa mogućnošću zagrijavanja uzoraka iznad 1 473 K. Ispitivanja su provedena u 2 serije. Prva serija je provedena na sintetičkoj leguri, a druga serija na industrijskim legurama. Sve serije su izvedene na 1 473 K sa stru-jom plina 5,55·10-6, 6,94·10-6, 8,33·10-6, 9,72·10-6 m3·s-1.Ključne riječi: metalurgija, pročišćavanje, bakar, refi  nacija, leguraINTRODUCTIONOne of products of the single step copper smelting of concentrate in ﬂ  uidized-bed furnace in Glogow Cop-perworks is the slag containing up to 20 % wt. copper. This material is then submitted to a decopperizing proc-ess in electric furnace. As a product in this technology the Cu-Pb-Fe alloy containing over 20 % wt. of lead and the dusts containing up to 40 % wt. of this element are obtained [1, 2].Cu-Pb-Fe alloy is processed in the converter to ob-tain copper suitable for the ﬁ  re reﬁ  ning process, i.e. containing below 0,3 % wt. of lead. At the same time, this technology is aimed to removal of possible highest quantity of lead in dusts and obtainment of low concen-tration of arsenic in copper. As result of this process, approx. 70 % wt. of lead contained in this alloy is pass-ing to dusts, and the remaining part is collected in con-verter slag. Because the copper content in slag (even above 35 % wt.) is higher than that of lead, this material is returned back to electric furnace. It can be assumed then, that the lead contained in converter slag is circu-lating in the process cycle [3-6].B. Oleksiak, G. Siwiec - Silesian Technical University, Department of Metallurgy, Katowice, PolandRESEARCH EQUIPMENT AND MATERIALSThe research work was made on synthetic alloy Cu-Pb-Fe and on industrial alloy provided by „Glogow” Copperworks. The synthetic alloy was manufactured from deoxidized copper M0B grade, lead PbO grade and Armco iron with melting of the metallic compo-nents together in vacuum-type induction furnace IS/III mark Lebold Heraus, in argon atmosphere and. in SiC crucible. The alloy was poured into preheated graphite moulds, to ingots in form of rods – 0,023 m dia. After extraction from moulds, the rods were cleaned and cut into cylindrical samples of 0,022 m dia. and h = 0,07 m. The chemical composition of alloys used in examina-tions is presented in Table 1.Table 1 Chemical composition of tested alloysType of alloy Contents of alloy basic parts / % wt.Cu Pb Fe As S AgSynthetic 74,8 22,5 4,6 --- --- ---Industrial 70,4 21,5 2,9 3,4 1,7 0,0025A sketch of the equipment used in tests is showed in Figure 1. The main component was a pipe-type resist-ance furnace, enabling heating of sample up to 1 473 K. In the furnace was placed a ceramic protective retort accommodating the crucible and the sample. The proc-ess temperature was measurmed with a thermocouple Pt-PtRh10 of 0,006 m dia. placed directly in liquid al-loy. The gas was introduced into metallic bath through 26   METALURGIJA 51 (2012) 1, 25-27B. OLEKSIAK et al.: REMOVAL OF LEAD FROM THE INDUSTRIAL AND SYNTHETIC Cu-Pb-Fe ALLOY WITH ARGON...an Al2O3 lance immersed to the depth 0,005 m to the crucible bottom. Gas ﬂ  ow was controlled by manual valves and rotameters. Whole system was closed with a ceramic cover and asbestos seal.METHODOLOGY OF RESEARCHA prepared alloy sample put in alundum crucible was introduced into ceramic retort placed in the furnace heated to required temperature.In the course of melting stage, an inert gas was intro-duced into working chamber through a lance located above crucible to the protect the metal against oxida-tion. When predetermined temperature was achieved in the furnace, a lance was introduced in and appropriate gas ﬂ  ow was adjusted. At the set time intervals the alloy specimens were sampled with quartz pipes. During this operation the ﬂ  ow of gas through metallic bath was un-interrupted, a possibility of adverse metal delamination was prevented. Having completed the tests, the lance was withdrawn off crucible, furnace supply was swit-ched off and the system was cooled down with inert gas blowing. After sample withdrawal, the slag and metallic fractions were separated and the samples were weighed up. In case of metallic samples, they were wholly dis-solved in appropriate solution of nitric acid and the re-sultant solutions were analyzed with the help of atomic absorption spectrometer Unicam, model Solar M6.SCOPE OF RESEARCHExaminations were carried out in 2 measurement se-ries. The Ist series was executed with use of synthetic alloy, while the IInd series used an industrial alloy from “Glogow II” Copperworks. All series were conducted at of the temperature 1 473 K, with gas ﬂ  ow of 5,55·10-6, 6,94·10-6, 8,33·10-6, 9,72·10-6 m3·s-1. In Table 2 are shown the basic test parameters for measurement series.Table 2 Basic test parametersSeriesNo. Alloy typeAppliedgasTest duration / sSample weight/gI synthetic Ar 10800 490±10II industrial Ar 10800 490±10Measurement series are designated as follows: alloy type – process temperature– ﬁ  rst three ﬁ  gures deﬁ  ne the gas ﬂ  ow. For example, the test designation S-1 473-5,55-1 means, that this examination is related to the ﬁ  rst measurement series executed at 1 473 K temperature, with argon ﬂ  ow 5,55 ·10-6 m3·s-1, test 1.TEST RESULTSTest results of all experiments concerning ﬁ  nal con-centration of lead and its degree of removal in liquid Cu-Pb-Fe alloy are presented in Table 3. In Figure 2 and 3 are shown exemplary variations of lead concentration depending on process duration achieved in experiments series 1 and 2.Table 3  Final concentrations of lead and its elimination degree achieved in tests series 1No. Test designationFinal concen-tration of lead in alloy / % wt.Lead removal degree / % wt.1 S-1473-5,55-1 21,62 3,912 S-1473-5,55-2 21,64 3,823 S-1473-6,94-1 21,42 4,794 S-1473-6,94-2 21,46 4,625 S-1473-8,33-1 21,23 5,656 S-1473-8,33-2 2,.33 5,217 S-1473-9,72-1 21,24 5,598 S-1473-9,72-2 21,04 6,489 P-1473-5,55-1 21,24 1,2610 P-1473-5,55-2 21,30 0,9811 P-1473-6,94-1 20,99 2,4212 P-1473-6,94-2 21,02 2,2813 P-1473-8,33-1 20,88 2,9314 P-1473-8,33-2 20,86 3,0215 P-1473-9,72-1 20,53 4,5616 P-1473-9,72-2 20,49 4,74The variations of lead mole fraction in metal bath for test series 1 and 2 are correlated with the function:  XPb = A · t + B (1)with:XPb – lead mole fraction,t – process duration time/ sA – equation constant / s-1B – equation constant.Figure 1   Sketch of equipment used in tests: 1 - lance, 2 – asbestos seal, 3 – ceramic shield, 4 – crucible with alloy, 5 – furnace heating components, 6 – thermocouple, 7 – gas supply system.27 METALURGIJA 51 (2012) 1, 25-27B. OLEKSIAK et al.: REMOVAL OF LEAD FROM THE INDUSTRIAL AND SYNTHETIC Cu-Pb-Fe ALLOY WITH ARGON...In Table 4 are presented exemple values of parame-ter A equation (1), its standard deviation and the values of correlation factor of obtained test results for test se-ries 1.CONCLUSIONSThe results of tests and their analysis provide the grounds to formulate the following conclusions:1.   Increase of gas ﬂ  ow intensity and temperature of the process will raise the degree of lead removal from tested alloys.2.  Maximum lead removal degree at parameters used for tests was to 6,8 % wt for the synthetic alloy and 4,74 % wt for the industrial alloy.3.  Low speed of barbotage process would not allow to apply this technology as the ﬁ  rst stage of convert-ing Cu-Pb-Fe alloy. It is possible to use this tech-nology as an auxiliary operation. Such operation can be applied in the second converting stage, when the lead content in copper is dropping to 2 %.REFERENCES[1]  A. Piestrzyński, A. Jasiński, J. Kotarski & others: Mono-graph KGHM Polska Miedź S.A., Cuprum Sp. z.o.o., Lu-blin (1996).[2]  M. Kucharski: Pyrometallurgy of Copper, Wyd. Nauk. – Dydakt., Kraków (2003).[3]  L. Blacha, J. Łabaj, B. Oleksiak: 12-th International Metal-lurgical and Materials Conference “Metal 2003”, Czech Republic (2003).[4]  B. Oleksiak: Metalurgija, 48 (2009)2, 87-90.[5]  H. S. Sohn, T. Fukunaka: Metall. Trans. B 35B (2004), 651.[6]  K. Okumara, M. Ban: ISIJ Int. 35(1995), 832.Note:   P. Nowak is responsible for English language, Katowice, PolandFigure 2  Variation of lead concentration in Cu-Pb-Fe synthetic alloy depending on process timeFigure 3  Variation of lead concentration in Cu-Pb-Fe industrial alloy depending on process timeTable 4  Results of correlation of mole fraction changes of lead in Cu-Pb-Fe alloy in function of process duration time for test series 1Test designation -A·106/s -1Standard deviation, /S(A)·106Standard deviation/S(B)·104Correlation factor/ rS-1473-5,55-1 0,097 0,006 1,16 0,986S -1473-5,55-2 0,110 0,015 2,78 0,942S -1473-6,94-1 0,120 0,007 1,38 0,987S -1473-6,94-2 0,117 0,010 1,78 0,978S -1473-8,33-1 0,137 0,012 2,05 0,978S -1473-8,33-2 0,127 0,012 2,17 0,972S -1473-9,72-1 0,139 0,017 2,97 0,958S -1473-9,72-2 0,172 0,014 2,53 0,979

Removal of lead from the industrial and synthetic Cu-Pb-Fe alloy with argon barbotage

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