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Construction and Operation of a Vacuum Retort Pilot-Plant for Distillation of Alloys

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Construction and Operation of a Vacuum Retort Pilot-Plant for Distillation of Alloys Scholars' Mine Masters Theses Student Theses and Dissertations 1950 Construction and operation of a vacuum retort pilot-plant for distillation of alloys Robert Frederick Doelling Follow this and additional works at: https://scholarsmine.mst.edu/masters_theses Part of the Metallurgy Commons Department: Recommended Citation Doelling, Robert Frederick, "Construction and operation of a vacuum retort pilot-plant for distillation of alloys" (1950). Masters Theses. 7111. https://scholarsmine.mst.edu/masters_theses/7111 This thesis is brought to you by Scholars' Mine, a service of the Missouri S&T Library and Learning Resources. This work is protected by U. S. Copyright Law. Unauthorized use including reproduction for redistribution requires the permission of the copyright holder. For more information, please contact [email protected]. CONSTRUCTION AND OPERATION OF A VACUUM RETORT PILOT-PUNT FOR DISTILLATION OF ALLOTS BY ROBERT FREDERICK DOELUNO A THESIS submitted to the faculty of tbs SCHOOL OF MINES AND METALLURGY OF THE UNIVERSITY OF MISSOIRI In partial fulfillment of the work required for the Degree o f MASTER OF SCI1NCE, METALLURGICAL ENGINEERING Rolla, Missouri 1950 Dr. A. W. Schlechten, Chairman, Department o f Metal­ lurgical Engineering and Mineral Dressing i t a c m m s BHEiit The author wishes to express his appreciation to the Missouri School of Mines and Metallurgy for the opportunity to carry out the rasearchi The author wishes also to express his appreciation to the fa cu lty members o f the M eta llu rg ica l Engineering Department fo r their suggestions and especially to Dr. A. W. Schlechten for his invaluable advice and assistance. Appreciation ie due, also, to the National Research Carp, of Cambridge, Maes, for their helpful suggestions and for ths diffus­ ion pump. The author wishes to express, also his appreciation to Mr, C. H. Shlh for his suggestions and untiring assistanss CONTENTS Pag* Acknowledgment* .......................................... l i List of Illustrations ........................................... lv List of Tablss . * ............ v i I. Introduction 1 II. Review of Literatur*................... 5 III. Theoretical Considerations .............................. 24 IV . Apparatus and Equipment ....................................... 31 ? . Procedure ................................................................... 3® A. Operation ............................. 3d B. Sampling of Material ........ 39 C. Chemical Analysis ................................... 41 VI. Experimental R esu lts ............................. 42 VII. Discussion...................... 54 A. V ariation o f Tints . ...................... 54 B. Variation of Temperature. ...... 55 C. Amount o f C h a r g e ........................... .... 56 D. Variation of Pressure ........ 57 E. Operational Problems ........ 5® VIII. Conclusions and Commercial Possibilities. , . 6® IX. Summary.................. 72 Bibliography. 74 LIST OF ILLUSTRATIONS Page 1, Pidgeon Process Retort .................................. 8 2 , Pumping Speed o f Pumps ...................................... 10a ■? Pumping Cost o f Various Pumps. 10b Shill* s Results, Variation of Time................ ... 16 Shih’ s Results, Variation of Temperature ..... 16 Shih'a Results, Variation of Pressure . .... 16 Shih's Results, Variation of Partiele Size .... 16 Vapor Pressure and Rates of Evaporation of Zn, Pb, Ag, Cu, Fe ..... ............................... 25 Activity of Zinc in Zn - Pb Alleys , , ................... 30 Composition of Vapor from Bolling Zn-Pb Alloys . 30 Activities in Pb-Ag Alloys . .......... 30 Vacuum Tight R etort 36 Gross Section of Retort in Furnace ........ 37 Residue Composition v s . Time (Herculaneum) .... 50 Residue Composition vs. Time (Bunker H ill) .... 50 Residue Composition vs. Pressure (Bunker H ill) . 51 Residue Composition vs Pressure (Bunker H ill). 51 Residue Composition vs Amount o f Charge (Herculaneum) ....... 52 19, Residue Composition vs Temperature (Herculaneum), 53 20, Residue Composition ve Temperature (Bunker H ill). 53 21, Expected Curves for Residue Composition vs Tima . 54 Distribution of Metal in Condensate, ...... 62 70 Tentative Vacuum System ...................................... XJ3T OF ILLU3mTI0K3, oontimisd Photo 1. SKporinontol Apparatus , , , ................... ... » . 2. Charging Boot* 3. Typlo&I Condons «tos* , . ,,,,,,,,,, vi LIST OP TABLES Table Page 1 . Port P ir ie Continuous Softening ....... 20 2 . Dross in g at Bunker H ill Lead R efinery .... 20 3. Composition of Crusts ............................... ... 42 4. Analyses from Run 1 43 5. Analyses from Run 2 43 6. Analyses from Run 3 44 7. Analyses from Run 4 ....... i ... • 44 S. Analyses from Run 5 ............ 45 9. Analyses from Run 6 45 10. Analyses from Run 6 46 11. Analyses from Run 9 46 12. Analyses from Run 10 47 13. Analyses from Run 19 47 14. Results from Bunker HlH Crusts . 48, 49 1 5 . Evaporation of Lead and Zinc ........ ii. niffstopocTioy m m n m The widespread appearance of large scale vacuum systems operat­ ing commercially in the micron range of pressures has initiated a new field of industrial endeavor, vacuum engineering. The ever in­ creasing number of applications of vacuo in commercial processes and la b ora tory research has stim ulated the design and improvement o f vac­ uum equipment, and at the present time equipment may be obtained to meet practically any need. In turn, the variety of available tools has directed the engineers attention to improving old processes and developing new ones through the utilisation of vacuum techniques. Reduced pressures may be desirable to the metallurgist for any number of reasons. D istillation processes conducted in vacuo may be carried out at lower temperatures or shorter time. Reduction reac­ tions which yield gaseous products may be attained in lower tmnperature ranges or may go mors nearly to completion in a vacuum. The practical absence of atmospheric gases in a high vacuum lessens fire hazards in ( i ) the case of magnesium production or makes possible the production (1) Pidgeon, L.M., and Alexander, W.A., Thermal Production of Magnes­ ium - Pilot-plant Studies on the Retort Ferro silicon Process. Trans. A.IJt.B., Vol. 159, PP. 315*352 (1944). -----------------------------------------------------------------------------------------------------------m m ------------------------ of purer metal in the ease of titanium and zirconium. (2) Iroll, W., The Production of Ductile Titanium. Trans. Bleotro- ehem. 8oc, Vol. 78* PP* 3-47 (1940). (3 ) I r o n , W., Schlechten, A. W., and Terkas, L,A„, Ductile Zircon­ ium from Zircon Sand, Trans. Electroohea, Soc, Vol. 89# PP. 263­ 276 (1946), Pressure raquireciants for the various a plications, of sour so, vary over a rather wide range. In the vaeuusn dezincing of lead a (5 ) pressure of 0.5 on. Mg is maintained. In the Pidgeon process (4) label!, W, T., Vacuum Dezincing in Lead Refining, Metals Tech­ nology, T.P. 2133, April, 1947, (5) Pidgeon, L, op. oit., p* 324. f o r production o f magnesium the pressures are fron 0 ,1 to 0 .2 ram Mg, and in laboratory work pressures of 0,001 m Mg are not unoawnm, Maintaining a vacuum becomes Increasingly difficu lt with lowering of {reeeure} however, pressures down to 0,01 m Hg are commercially pos­ s ib le and p r a c t ic a l. In the metallurgy of argentiferous lead there have been four i*~ (6 ) L id d e ll, 0 , H ,, Handbook o f Nonferrous M etallurgy, V o l. 2 , 2nd ed., 8,1, McGraw-Hill Book Co,, 1945, p. 191, oupellation, Pat tin ecu process, Parkes process, and Bette electrolytic p ro ce ss . The f i r s t two are o b s o le te . The Bette proesss has the advan­ tage of bismuth removal which the Parses process does not) however, the cost is high and silver is not removed as completely as by tbs Parkes process. In the Parkes proecse 1 to 2 per cent of sine le added to the molten bullion and a high sine-silver material is formed, fleets to the t o p , and may be removed. What the mechanism o f the proeoss i s i s mot definitely known. Probably,, two im iselble liquids are formed) a high sine layer saturated with lead and e high lead layer saturated with sine. The sine layer has a mush greater affinity far silver than does the lead and there la a silver buildup In the high sine layer. The high sine material has a relatively lev density and floats to the top. It may then be ladled off as a liquid, or sinoe it has a relatively high malting point, it may be skimmed off aa a mushy material i f the temperature ie low enough. These cruets, as they are called, contain mainly dine, silver, and lead. Many impur­ ities frequently occur in the crusts also. The major ones are copper and ir o n . The sine additions are generally made in two steps. The first skinminge containing from 2000 to 5000 os of silver per ton are retain­ ed for silver recovery. The second which are lower in silver are used for the first addition of sine to a new batch of bullion. The present method o f recoverin g s ilv e r from these cru sts i s a complicated, time-consuming task. The cruets are first distilled at atmospheric pressure to remove the sine. The residues are then cup­ elled to crude silver. Tbs crude silver is generally refined again by recupeUation or melting with silver sulfate to oxidise impurities. This process has a high in itial and operating cost and entails excess­ ive metal losses through oxidation. The possibility of producing a relatively high purity silver in a single step by distilling off the sine and lead in a vacuum was suggested as early as 1912 by H. J. Humphries in discussing a paper (7 ) by Turner but until recently no experimental work on this (7) Turner, T ., The Behavior of Certain Allays When Heated in Vacuo. J. Inst, Metals. No, 1, Vol. VII, P, 120 (1912), possibility had been published. In 1949, experiments were conducted by Mr, C. H, 3hih on the distillation of artificial and commercial (8 )(9 ) cru sts in a small vacuum fu rn ace, Mr. Shih1 s findings more extremely encouraging and it was decided to cany the investigation (3) Shih | C, H.
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