eo MINERAL PROCESSING The application of residence time distributions to flotation and mixing circuits J.E. NESSET Mattabi Mines Ltd. Ignace, Ontario ABSTRACT This paper discusses the importance of considering residence time distribution (RTD) in the design of flotation and mixing circuits and in the analysis of operating problems, The experi- fences and successes of Brunswick Mining in this area are covered and include: the development of @ practical RTD ‘measurement technique using pulp conductivity, baffle installa tion o improve the RTD of existing process equipment, and the ‘method in which RTD considerations have been used to design the newest flotation and conditioning operations. Introduction ‘The use of residence time distributions (RTDs) in the design and analysis of unit operations is well understood by the chemical engineering profession' while mineral processing engineers hhave tended to rely on empirical and rule-of-thumb factors. For example, in scale up from laboratory and pilot test results to full size flotation plant design, empirical rules are often used to establish residence time and number of cells in the bank. Cole- rman® suggests a factor of at east 2, and up to $ for gold ores, be applied to laboratory determined flotation times. This is fur- ther illustrated in Table 1, taken from Denver equipment”). ‘The number of cels in Series to achieve the required retention time while minimizing shor-cicuiting has generated a variety of conclusions” (Table 2). Obviously there is less than complete ALE. Nesset Jan Baward Nesset recived ¢ BEng. (metallurgical) from McGill University stitution in I9BD. From 1979 1986 Jan [Nesset was employed with Norands's Brunswick Mining. operation near Bathurst, New Brunswick, as concen- ‘rator metallurgis, project meallurgst and senior metallrgst. Since 1987 he has Bee wil superintendent at Noranda's Mattabi Mines oper ation near Ignace, Ontaria, ‘Mr. Nesset has authored numerous papers relating to magnetic property measurement and high gradient magnetic separation of {aconites and sulphides, pressure filtration of concentrates, ss well a5 trinding and flotation operations, “He ise member of CIM, Keywords: Mineral processing, Flotation, Residence time dstibuton ‘agreement on the subject. Young notes that a clear difference of opinion has emerged and cites as extremes, () the publica- tions of Outokumpu® showing unimpaited recovery for its largest machines (38 m') compared to equivalent retention times for numerous smaller machines, and (i) the experiences of Eastern European countries where the practice iso install banks ‘of 30 units or more, operating in series, often with unit retention times of only a fraction of a minute. ‘The empirical factors used by engineers presumably account for other than tested feed conditions, inefficiencies in large con- tinuous machines, inevitable day-to-day circuit disruptions, sradual equipment deterioration and any other safety factor the engineer feels compelled to incorporate. An understanding of RTD concepts and techniques should help the practicing mineral engineer to develop more soundly based factors. This paper relates the experiences of Brunswick Mining in using RTD tech- niques in the unit operations of flotation and mixing. Theoretical Aspects Consider a process vessel of volume V, being fed a slurry at a volumetric flowrate, Q. The slurry mean residence time in the vessel, s gven by: i- vg ‘The Muid and mineral particles do not all stay in the vessel the same length of time; some may exit after a very short time (resulting in short-cireuiting) and others remain for a much Tonger time. This can be represented by a “residence time distribution”* or RTD, which is simply a probability function against time. ‘The simplest method of determining the RTD of a vessels by the stimulus-response method in which a tracer is introduced to the vessel infet stream at time zero. The outlet stream is ‘monitored either continuously or discretely to detect how passage through the vessel has distributed the input signal. The simplest response to analyze is from a pulsed input, Figure | shows an RTD curve, resulting from a pulsed input, measured concentration, C, "in the vessel exit stream. ‘An RTD curve is characterized by it first two moments, i the ‘mean residence time, and ot, the variance. The mean residence time reflects mass transport phenomenon in that it defines the relationship between the vessel volume (V) and volumetric feedrate (Q). The variance, in turn, reflects the degree of mix- ing which occurs within the vessel. Both may be readily deter- ‘mined from discrete measurement values by the following Approximations. Measured concentrations are fist normalized so that the total area under the curve equals unity, ie. Paper reviewed and approved for publication by the Canadian Mineral Processors Division of CIM. CCIM Bulletin, November 1988 8eel pulse npat Tracer cutout et euve Ke ator ZEA where CC = normalized concentration E = measured concentration 24, time interval ‘The mean residence time is found from: where fea ecm ge abit! Fea * EG 3% av = Ey Cay since EC abe “The variance is found from: _ fice 4 EG ay cee ca = ERG ay - 2 discrete time value srete concentration value For several closed vessels in series, the over-all mean residence TABLE 1. Typical flotation residence times compar- ing laboratory and industrial conditions (Ret. 3) Usual industial Denver lab col Material flotation times (min) {Hlotable form) times (min)* _ (0:2 or 0-12 cel) Bante B40 45 Coal 35. 23 Copper 13.16 oa Effluents e12 a5 Fluorspar B10 a5 Feldspar 8:10 34 ‘Lead 68 35 Molybdenum 1420 87 Nickel 1014 67 oil 48 23 Phosphate 48 23 Potash 48 23 Sand (impurity flotation) 7.8 34 Silica (ron ore) 810 35. a (phosphate) 45 23 Tungsten B12 56 ‘ine. B12 86. “For roughing applications; fr cleaning, he rotenton time ie between ‘6087880 ofthe roughing time fora particular mineral, thee Side 15 50%-05% ofthe normal roughing soli 6 FIGURE 2. RTD cures for varios degrees of dspesion as ‘measured by the D/UL parameter (rom Levenspe) time and variance are simply the sum of the individual values: pred = Ee It is sometimes convenient to express these parameters in dimensionless time units: G =i a y= “(the reative variance) with the mean dimensionless residence time equal to unity by Sefinition: ‘There are two types of ideal flow; plug flow in which the ‘uid stream passes through the vessel without mixing with the vessel contents, and fully mixed flow in which the fluid ele ments are immediately dispersed throughout the tank volume. ‘Actual flow has components of both types of ideal low. Most modelling of RTD curves has made use of either dis persion or tanks-in-series models. A thorough discussion of the various models and their applicability is covered in the text bby Levenspiel\0. The degree of mixing has been quantified by Levenspiel for closed vessels through the application of @ dispersion model and a dimensionless group called the "vessel dispersion number", D/UL, a parameter which measures the ‘extent of axial dispersion and where D = axial dispersion coefficient L = length of vessel U = anil id velocity in vest For elosed ves, Levens! found og = So zorwL-210/UL PA - et-ULID) forthe famly of curves shown in Figure 2. 'A plot of the preceeding equation appears in Figure 3 and may be sed determine B/UL values for experimental RTD caves one tro have bom cst” Aword of can isin order thse relaonsip ar for closed vessel (id Eaters and eaves solely by pug ow) and lose thee apical: iy where very lage amounts of dispersion sre preset Volume 81, No. 919FIGURE 3, The relative variance asa function of D/UL after Levenspid, Nevertheless, itis possible to use the D/UL parameter to predict the extent of reaction (or recovery) which will occur. Figure 4 has been developed by Levenspiel, assuming first- order reaction kinetics, and relates the real to plug flow (or batch) volume, V/V,, D/UL and the extent of the reaction, Xq (expressed in the figure as I-X,), An Example: Lime Slaking I it has been determined in the laboratory that batch lime slaking requires 15 minutes forthe reaction to go to 98% com- pletion, what mean residence time should be designed for two Inseries mixers in a continuous plant operation so as to achieve the same extent of reaction? Assuming that through cither prior RTD measurement on single mixers or reference ‘material one knows that o,, the relative variance, is 0.8, use is ‘made of the additive nature of the variances to calculate the expected og? for two units, namely 0.4. Use is then made of Figure 3 to obtain the corresponding D/UL (=0.3). For an Xq of 0.95 and a D/UL of 0.3, Figure 4 shows that a real to plug flow volume (or time) ratio of approximately 1.8 will be re- 4uired. The two plant mixers should, therefore, be designed to provide a total mean residence time of 27 minutes (1.8 x 15 minutes). Dobby and Finch” have applied the preceeding method of reactor scale-up, assuming frst order kinetics, to column flo- tation with considerable success. The reader is again referred to the text by Levenspiel which covers the concepts and appli- FIGURE 4. Comparison of real vs eal flow (ue. plug flow) equieed volumes, V/Vp, (rom LevenspieD. cations of RTDs in detail and with great clarity. His chap- ter on diagnosing ills of operating equipment should prove particularly enlightening to plant operators. In sum- ‘mary, it need only be said that RTD concepts are easy to grasp and apply and that the results can be interpreted both qualita- tively as well as quantitatively. At Brunswick Mining much of this work has been carried out by engineering students Measurement of Residence Time Distribution Measurement Techniques RTD measurement involves the introduction of a tracer to the vessel feed stream and either periodic sampling (discrete ‘method) or continuous monitoring (continuous method) of the tracer in the vessel discharge. In a processing plant one is most often concerned with the behaviour of the solids. The use of solid tracers, though by no means impossible, does tend to add to both the complexity and cost of the test. The practice at Brunswick Mining has been 10 use liquid phase tracers and to ‘make the assumption thatthe liquid phase ofthe slurry closely approximates the behaviour of the solids phase. Dobbyt!® has shown thatthe validity of this approximation is a function of Particle size and improves with decreasing particle diameter. At the very fine sizes present in the Brunswick flotation circuit, TABLE 2. Literature sampling on the required number of flotation cells in series Recommended number of Publication calls ‘Additional Roterence et In sories Comments Sutherland, O.N. ‘A study of the optimization of the arrange 68 Usually sufficient ment of flotation circuits (4) Churchill, M Large flotation machine development and 78 For typical sulphides Degner, WA. ‘operation (8) Abiter, Ny Design of flotation cells an circuits (6) 1244 12 minimum Weiss, N, Wilson, R.A. 1218 12 minimum Dawson, HA Nit Experiences with large Outokumpu flotation 6s 4 minimum Tarvainon, M machines (8) for large cells itu, Discussion period 45 Degner, V.A, Authors’ replies, 63 Dominici, P XiVIM PC. 1012 Minimum Lawrence, GA. Toronto, Canada (1982) (9) 48 CCIM Bulletin, November 1988 ”Gm rubntLe mBLE he I” == FIGURE 5. Schematic of conductivity probe arrangement used for RTD determiaation. {65% 10 95% passing 374m, agreement between liquid and solid phase RTDs should be very good. Discrete measurement techniques have included atomic ab- sorption for specific metal ions, and ultraviolet spectrophoto- ‘metry for dye tracers. When doing discrete measurements the use of dye is favoured because of the lower cost and more rapid analysis. ‘The continuous method used involves the measurement of pulp conductivity at the vessel discharge following the int ‘duction of a strongly ionic salt tothe feed stream. This method has met with success at Brunswick Mining because of the low cost and ease of performing the RTD tests. It is applicable wherever the background conductivity remains fairly stable, a condition which should be checked for beforehand. “There are a few circuits where this condition is not met due to the introduction of conductance altering chemicals (e.g. copper sulphate). Figure $ shows a schematic of the Foxboro lectrodeless Conductivity Probe (model 1210) as hooked-up to a strip-chart recorder. A null control has been added (@ 9.volt battery) to provide good range flexibility for the unit. ‘The probe itself is a doughnut at the end of a 6 m flexible ‘able. Figure 6 shows an example of a typical conductivty- probe RTD output for a single tank conditioning unit. Tracers A suitable tracer should have most of the following characteris- * Cost — relatively low cost for both the tracer as well as the analytical method. * Detectability — have relatively constant background levels in the steam being monitored. * Convenience — the preparation of both the tracer and the subsequent samples for analysis should be as straightforward as, possible. This cannot be overstressed ‘+ Non-Interference — the racer should not interfere or react 10 any significant extent with the process being measured, “Table 3 ists the various type of due and salt tracers which are TABLE 3. Characteristics of FIGURE 6. RTD output respome for ‘measured with conductivity probe. in use for RTD measurement of flotation and mixing at Bruns- ‘wick Mining and tei advantagesdsadvantages, Where poss ‘ie, conductivity measurement fs performed because of is tow ‘cost eae of use and the non interfering efor of the sal used Of the sats sted in Table 3 CaCl is the preferred salt due to is igher ionic character and low cost. For very large flows, oF very large, vessel the quantity of sal equted has sometimes precluded ts we. Rhodamine WT, although avery powerful dye Suitable for mater tracing, suffers fom very high coat and high Tess (over SOM) possibly dc to adsorption on ois, when sed svi res, The Faressn dye, Uranne, s prefered for ota tion work, however, samples mist be covered prior to analysis de to depradation ofthe dye when expore to tltravole ight. In flotation cies where activated carbon is added the use of dyes is not posible because of dye adsorption by the carbon. Both the Rhodamine WT and the Uranine hve slight frothing Characteristics when used inthe foaton cieuts a Brunswick Mining. An exclent review aie onthe use of various dye tracers and their specifications is given by Smart and Laidlaw®. “The use of lithium chloride has not presented any problems aside from the cost of he chemial andthe sbsequent analysis by atomic adsorption. It tends tobe the choice when ether the conductivity or Uranine de ae not suitable. ‘The choice of sampling interval is left to the common sense of | the tier Obviouly, the frequency should be higher a the ‘beginning of the test up to and including the expected mean resi- dence time. Zerosime sampling i also necessary. The impor. tance of extending the empbing prio once as mc of the RTD tail as posible i sresed so that an accurate determination othe area under the curve posible. Analysis and Improvement of Existing Operations The following examples ilustrate two applications of RTD Incthods for analyzing and improving the existing operation at Brunswick Mining. Fotation cell"“affing” was the inti wid phase tracers in use at Brunswick Mining ‘Sampling ‘Continuous! ‘Tracer Discrete Advantages __ Disadvantages Analysis uch cD usually low costly background noise absorption Salts background readings or Cacly inexpensive ‘may vary ‘conductivity Naci cD CaCl, preferred large quantites Kel sometimes required Rhodamine WT D low detectability very costly : limits uly ease of analysis ‘may adsorb on solids spectro. byes photometer Uranine > reasonable cost destroyed by tluorometer ease of analysis uly light cover time 8 Volume 81, No. 919{URE 7, Effect onthe RTD of decreasing the open are be- tween cell fora bank of four 8.5 m cls, ‘experience with these techniques while the conditioner study is Baffling of Flotation Cells AAs part of a mine and mill modernization and expansion pro- ‘gram undertaken between 1978 and 1981, a total of 128 new and replacement flotation cells, ranging in size from 1.4m t0 8.5 m? ‘were installed. These were of the open tank or “*hog-trough” type arranged in banks of from 3 to 8 cells between intermediate boxes, Typical are the 8.5 m? lead and zinc rougher! scavenger ‘banks arranged in single cows ina 444-4 cell combination. They replaced banks of 19 Sala BFP 240 double-cells in series. ‘Concern over the metallurgical performance ofthese new cells was expressed soon aftr installation and was quantified when 2 test-bank of a competitor's internally-baffied machines (of equivalent volume) clearly outperformed the hog-trough units, Preliminary RTD tests using dye tracer (Rhodamine WT) in cated a significant difference in the plug flow (PF) component and profil of the curves. Subsequently, a series of metallurgical {esis and RTD curves were generated for a bank of four 8.5 m? units having various degrees of internal baffling. The baffles were simple stee partitions, bolted vertically into the tanks between ‘mechanisms, each partion having a central opening of adjustable “area. The percentage open area was defined as being relative o the cross-sectional area of pulp in the flow direction. A small sand relief slot was provided atthe botiom of each partion plate. The normalized RTD curves for the tests are shown in Figure 7 while the corresponding data are provided in Table 4. The results show that as increased baffling reduced the open area between mechanisms from 100% to 12%, the metallurgical performance of the zine rougher bank improved from 33% to almost $1M% recovery without affecting grade. As evident from Figure 7 the plug flow characteristics of the RTD curves in- creased from 0.14 100.30 with inereased cel baffling. No signifi- cant inerease in power consumption was noted during the tests. CCellby-cell samples also showed an increasing zinc gradient down the bank with increased baffling. It was concluded that the unbatfled hog-trough cells were contributing to internal FIGURE 8, Effect on cleaner al control of baffling » bank of five 85 m? cell. recirculation currents and, hence, significant short circuiting of {eed to the cel talboxes. "These tests were some of the first using Rhodamine WT, a dye ‘which tends to suffer from high losses (over 90%) when used in pulps. As a result, some uncertainty existed with respect to the {otal area under the distribution curves. ©, as plotted in Figure 7, is, therefore, relative to the calculated ‘mean residence time, 'V/Q, instead of the mean of the distribution. This accounts for the shift in 8 toward values less than 1. The conclusions regard- ing short cizcuiting aze still felt to be valid as borne out by the significant metallurgical improvements achieved. "As areull ofthis study, Brunswick baffled all of ts hog-trough cells and now insists that any new cells be partitioned with the minimum opening size possible, The calculation procedure used to determine the minimum opening size is based on the expected flowrates and maximum allowable hydraulic head-loss While still maintaining acceptable level control. In addition to improved recovery asa result of bale installa- tion, several other benefits also accrued in reagent consumption and improved circuit control: ‘ Xanthate consumption decreased 25% to 30% on a bank of seven 3 m? cells used for reverse cleaning (Le. pyrite flotation from sphalerite) of zinc concentrate. ‘Both the standard deviation and the mean value of the tail for a bank of five 8.5 m zinc cleaners decreased with the installa- tion of baffles, as evident from Figure 8. It should be noted that the process control loops required retuning as the response characteristics of the circuit had changed markedly. * On several other circuits cell baffling has permitted stage addi- tion of reagents because cells now operate individually rather than as one large tank Improved selectivity and flotation control are considered to be especially advantageous when dealing with fine-grained mas- sive sulphides™1®, On a final note, it should be mentioned that the baffling of flotation eels has resulted in various improve- ‘ments on several, but not all, circuits. Iti fair to assume that where short- ces for rougher banks and the mode! ling clearly showed thatthe use of sixteen 8 m? machines would Yield only marginally lower recoveries and sill provide for much less short circuiting than either the 16 nv of 32 my units. Similar ‘analyses were performed for the cleaner banks. Table 8 sum- marizes the design numbers for the new flotation equipment. It should be noted that in no case were fewer than 10 cellsin-series chosen due to the increase in short circuiting and detrimental effect on flotation recovery exhibited by fewer numbers of larger cell. Confirmation that lip length to cell volume was suf- 2 Flotation No. of cals Coll volume circuit ™ (CuP Rougher 16 8 @ tines) ‘st cleaner and 2» 3 ‘leaner scavenger 2nd 10 3 Zn Rougher 16 8 (lines) ‘st cleaner and 2 8 ‘leaner scavenger 2nd cleaner 6 5 41d cleaner 2 3 ficient in each case was also necessary to ensure that froth removal would not be the rate limiting factor in flotation. Concluding Remarks ‘To date, the work at Brunswick Mining has confirmed the im- portance of considering not only the mean residence time but also the residence time distribution for both flotation and related unit operations. Suffice it to say that when the inefficien- cies of non-ideal flow are ignored, gross errors in design and shortfalls in performance may result. ‘The techniques of RTD analysis have been well developed by the chemical engineering profession but have not been applied {o the same extent by operational mineral processors. This must bbe regarded as unfortunate because the methods and analyses have proven to be easy 1o apply and yield valuable quantitative information for both the improvement of ex and the design of new ones. Regarding the question of the appropriate number of cellin- series, an appreciation of Figure 4 reveals thatthe ultimate per- formance will be a function of the flotation kinetic (k), the number of cells-in-seies (and hence the D/UL of the RTD), and. the (otal installed volume. Of course, providing for extra volume will offset the shortcomings of a circuit with few cell-in- series. However, the more cellsin-seres the better the plug flow characterises of the installation and the less short-circuiting ‘whieh will oceur; a condition which must be considered favour- able for most flotation systems. In view ofthis, plant operators should be skeptical about the claims of some manufacturers regarding the use of few numbers of large cells, and cell designs fof the open-tank, multiplespindle type. The application of the ‘methods outlined in this paper permit the engineer to evaluate the various process and economic trade-offs when selecting the size and number of cells, or for that matter, the design of other unit operations as well Volume 81, No.918Acknowledgments “The author wishes to thank those many individuals who have contributed to this work, in parclar, 1.B. Philips, 3. Geldart and J. Clements, Thanks are also due Brunswick Mining for permission fo publish this paper REFERENCES 1. LEVENSPIEL, 0., Chemical Reaction Engineering: Wiley, 2nd Edition, 1972 2 COLEMAN, R.L., Mineral Processing Plant Design; Molar and Bhappa, eds, AIME, 1960, pp. 14-182. 3, Anonymous," Mining Equipmen! International (Aprils 1983, pp. 19-25, 4. SUTHERLAND, DN, International Journal of Mineral Process ing (7), 1961, p. 319-346, 5. CHURCHILL, M., and DEGNER, V.R., Mining Enginering (uly, 1982; pp. 787-792 6. ARBITER, N., and WEISS, N.L., SME Transactions, Vo. 247, 1970, pp. 340347 ‘WILSON, R-A., and DAWSON, H.A., Mineral Procesing Plant Design; Mular and Bhappu, ed., AIME, 1980, pp. 183-200 NIITT, T., and TARVAINEN, M., Procesdings XIV Inter ‘ational Mineral Processing Congress (Sesion Vi), CIM, 1982, pp. VITA-VI?-2 Discussion and Authors Replies; ibid, pp. 36:39. ‘YOUNG, P., Mining Megazin, Vol. 146, 1982, pp. 35:39. 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