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International Journal of Mineral Processing 99 (2011) 78–83 Contents lists available at ScienceDirect International Journal of Mineral Processing j ourna l homepage: www.e lsev ie r.com/ locate / i jm inpro On the gas dispersion measurements in the collection zone of flotation columns E. Matiolo, F. Testa, J. Yianatos 1, J. Rubio ⁎ Laboratório de Tecnologia Mineral e Ambiental (LTM), Departamento de Engenharia de Minas-PPGEM, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves, 9500/75, 91501-970, Porto Alegre, RS, Brazil ⁎ Corresponding author at: Mining Engineering Dep do Rio Grande do Sul, Brazil. Tel.: +55 51 33089479; fa E-mail addresses: juan.yianatos@usm.cl (J. Yianatos) URL: http://www.ufrgs.br/ltm (J. Rubio). 1 Chemical Engineering Department, Santa María Uni Chile. 0301-7516/$ – see front matter © 2011 Elsevier B.V. A doi:10.1016/j.minpro.2011.03.002 a b s t r a c t a r t i c l e i n f o Article history: Received 29 September 2008 Received in revised form 21 February 2011 Accepted 11 March 2011 Available online 29 March 2011 Keywords: Gas hold-up Column flotation Bubble size Bubble superficial area flux This work shows the results of gas dispersion parameters in a fully controlled laboratory column flotation cell, namely gas hold-up (εg), superficial gas velocity (Jg) and bubble size distribution, measured directly by image analyses using the LTM-BSizer. Gas hold-up and bubble size (and their distribution) were found to be strongly dependent on Dowfroth 250 concentration and superficial gas velocity. A fairly linear relationship between experimental εg and bubble superficial area flux (Sb) was established, and results are compared to those calculated using drift flux analysis. Data obtained are discussed in terms of solution, hydrodynamics and interfacial phenomena. Possible implications on the role of the frother in the energy dissipation in bubble generation and on interfacial tensions are explored. artment, Universidade Federal x: +55 51 33089477. , jrubio@ufrgs.br (J. Rubio). versity, P.O. 110-V, Valparaíso, ll rights reserved. © 2011 Elsevier B.V. All rights reserved. 1. Introduction The properties of bubbles (gas) dispersion or hydrodynamic conditions clearly play an important role in froth flotation and applied flotation to effluent treatment. Recent developments (Schwarz and Alexander, 2006; Dahlke et al., 2005; Hernández et al. 2003; Grau and Heiskanen, 2003; Chen et al., 2001; Finch et al., 2000; Deglon et al., 2000; Gorain et al., 1997, 1998, 1999) have permitted reliable measurements of some gas dispersion parameters, namely gas hold-up (εg), bubble size (db), gas rate (Qg) or superficial rate (Jg) and bubble surface area flux (Sb): Jg = Q g A ð1Þ where A is the cell cross-sectional area, and the bubble surface area flux (Sb) defined by: Sb = 6⋅Jg db ð2Þ Many attempts to relate these parameters to flotation performance have beenmade by a number of authors (Hernández et al., 2003; Grau et al., 2005; Grau and Heiskanen, 2003; Kracht et al., 2005; Deglon et al., 1999; Gorain et al., 1998). Jameson et al. (1977) derived that the first-order flotation rate constant (k) is given by: k = 0:25⋅Ec⋅Jg db ð3Þ where Ec is the collection efficiency, the term ending up in terms of surface area flux, yielding: k = 0:25⋅Ec⋅Sb ð4Þ Some data reported suggests that bubble surface area flux (Sb) and gas hold-up are related by the following relation (Finch et al., 2000): Sb = 5:5⋅εg ð5Þ This relation would have advantages, because the gas hold-up is easier to measure and would solve the problem of poor bubble size measurements (Tavera et al., 2001). This appears to be the case for flotation columns andmechanical cells, both laboratory and plant scale, over the approximate range Sbb130 s−1 and εgb25%. Yet, Heiskanen (2000) claims that, in practice, the Sb better matches with the flotation rates of the fine fractions and suggests thatmore experimental work on the k–Sb relationship with different mineralogical species, is needed. With regard to the Sb values, Deglon et al. (2000); Power and Franzidis (2000) and Gorain et al. (1997) found that for normal (non- flooding) operating conditions, bubble surface area flux lied typically within the range of 30–70 s−1. Recently, some of these hydrodynamic plant data have been combined, whereby typical mean bubble diameter ranged between db=1–1.5 mm and Jg=1–2 cm/s. Herein, theoretical and practical http://dx.doi.org/10.1016/j.minpro.2011.03.002 mailto:juan.yianatos@usm.cl mailto:jrubio@ufrgs.br http://www.ufrgs.br/ltm http://dx.doi.org/10.1016/j.minpro.2011.03.002 http://www.sciencedirect.com/science/journal/03017516 79E. Matiolo et al. / International Journal of Mineral Processing 99 (2011) 78–83 considerations of their border limits have been reported (Yianatos and Henríquez, 2007). In summarizing, bubble surface area flux has been related to flotation performance and claimed to be a key “machine variable”. However, most of the available data have been taken, calculated or measured in conventional cell and only a few have been done in column flotation cells. The effect of frothers has been revised lately, in terms of air dispersion into fine bubbles, froth stabilization, interactions at the water/gas interface and with collector molecules adsorbed into solid particles, water carrying effect and their main effect on bubble size and uprising velocity (Finch et al., 2006, Melo and Laskowski, 2006, Grau et al., 2005, Nguyen et al., 2003). This article is a contribution to the general discussion on the possible implications of frothers in bubble generation (energy and size) -interfacial tensions and system hydrodynamics. 2. Experimental 2.1. Column flotation A laboratory flotation column, 2.54 cm diameter and 2.20 m total height, made of Plexiglas was used as the experimental apparatus (Fig. 1) for gas dispersion measurements in a two-phase system (air/ water). Bubble generator used was a porous stainless cylinder with a nominal porous size of 5 μm. Fig. 1 shows the set-up for the hydrodynamic measurements. 2.2. Gas hold-up measurement For the experiments in a two-phase system (water/air), the required amount of Dowfroth 250 was added to 30 L of tap water in Fig. 1. Experimental set-up of the natural pH (around 6–7). This solution was continuously agitated using a stirrer and introduced after 10 min in the column, with a peristaltic pump. The interface level was controlled by a peristaltic pump located at the column bottom discharge and the air rate (injected directly into the bubble generator) was measured by a mass flowmeter and regulated with a pinch valve (Fig. 1). Gas hold-up (εg) in the two-phase system (air–water) was measured by pressure difference over a section of length, L of 83 cm in the collection zone just below the froth. Pressure was sensed by water-filled manometers and the fractional gas hold-up was determined by: εg = ΔH L ð6Þ where ΔH is the difference in the manometer readings. 2.3. Bubble size measurement procedure Bubble size measurements were made using the LTM-BSizer (Rodrigues and Rubio, 2003) whereby the image analysis system included the bubble capture cell, a microscope and a CDD camera (Fig. 2). This technique (LTM-BSizer) employs a sampler to draw bubbles, rising in a column, into a special viewing chamber and exposes them to a digital camera, after they have decelerated and stopped. Thus common problems related to the movement of bubbles, namely focus, illumination, photographic speed and bubbles overlapping are all overcome. Results obtained are in good correlation with those values reported with the traditional image analysis method and show that using this technique, accurate size distributions can be produced, conveniently and efficiently (Rodrigues and Rubio, 2003, 2007). laboratory flotation column. Fig. 2. The LTM-BSizer for the determinations of the bubble size distribution (Rodrigues and Rubio, 2003). 80 E. Matiolo et al. / International Journal of Mineral Processing99 (2011) 78–83 3. Results and discussion Fig. 3 shows the size distribution of the generated bubbles and Fig. 4 summarizes the mean bubble diameter (Sauter) at different Dowfroth concentrations (10 to 40 mg L−1) for a superficial gas velocity fixed at 0.49 cm s−1. Herein, values obtained from drift-flux calculations (Yianatos et al., 1988), are enclosed for comparison reasons. Results show that when the frother concentration increases, the bubbles become smaller with the Sauter mean diameters decreasing from about 1000 μm to about 470 μm. This minimum (reaching a plateau) for the bubble size (and its size distribution) also depends on sparger and flow mixer (if venturi, needle valve, and static mixer) designs. Rodrigues and Rubio, 2003 found, for a similar system and frother (used in this work), bubbles can be as small as 200 μm with a venturi, for the same frother concentration range. The higher fluid velocity (and the higher energy to be dissipated ahead) inside the venturi, compared to a porous (perforated) cylinder, explains the difference in bubble size and in the hold-up values. Explanations for this behavior have been given by a number of authors and the bubbles size decrease appears to be associated to the energy required for bubbles generation. This may be related to a decrease of the liquid–air interfacial tension, when the frother concentration increases, but there is no agreement on this issue. A frother may produce a dramatic effect on bubbles size distribution (and narrowed) but may not substantially decrease the air/water interfacial tension. In the absence of frother, big (not- measurable) bubbles are formed while for concentrations higher than 5 mg/L, the average bubbles size decreased substantially. Cho and Laskowski (2002), studied the effect of frothers on the size of bubbles, in single and multi-hole spargers and a flotation cell. These authors found that the size of bubbles strongly depends on frother concentration only when multi-hole spargers are utilized or when energy (arising from the liquid turbulence) is transferred, producing cavity phenomenon, and small bubbles are formed. At low frother concentrations, lower than a “critical coalescence concentration” (CCC), the bubble size is much larger, indicating a sort of coalescence as the main mechanism determining the size. This coalescence phenomenonmight be prevented at frother concentrations exceeding this CCC value, which is empirically determined as the froth dosage at the break point of the slope (Melo and Laskowski, 2006, Laskowski, 2003, Sweet et al., 1997, Grau et al., 2005). Conversely, Finch et al. (2008) (to appear) believe that there is no agreed mechanism on how frothers act to reduce bubble size. These authors claim that there would be a breakup mechanism, phenomena associated with bubble shape, with its hydrodynamics in pulps (velocity and surface flows). The resulting force would be associated with surface tension gradients and it would impulse this breakup phenomenon. The fact is, when bubbles are formed in pure water, where little pressure transfer exists, large bubbles are produced. At operating pressures lower than 3 atm and in the absence of frothers, there is no sufficient energy to overcome attrition and nucleation to form small bubbles. However, a decrease in solution/air interfacial tension provides low energy nucleation sites and minute bubbles are generated. Results obtained in previous works (Takahashi et al., 1979, Féris and Rubio, 1999, Féris et al., 2000) show that the minimum “energy”, ΔF, to be transferred to the liquid phase to form bubbles by a cavity phenomenon (arising from the liquid turbulence) is given by the following equation (Takahashi et al., 1979): ΔF = 5:3⋅Π⋅γ3 Po−Pað Þ3 ð7Þ where: γ air–water surface tension (Nm−1) Pa flotation cell atmospheric pressure (atm or Pascal units); Po flow entrance pressure (atm or Pascal units) or pressure in the sparger Thus, the energy required to generate bubbles will be smaller with lower air–liquid interfacial tensionsandwithhigherpressuredifferences image of Fig.�2 Fig. 3. Bubble size distribution at different Dowfroth 250 concentrations and at constant Jg, 0.49 cm s−1. 81E. Matiolo et al. / International Journal of Mineral Processing 99 (2011) 78–83 across the sparger (inlet e outlet). Thus, when lowering the air–liquid interfacial tension (Fig. 5) in a few units (7–10mN/m−1 units), the liquid–solid attrition will be smaller at the sparger outlet (or inside if water is used as carrier for the air). This results in a faster fluid flow velocity and in a rapid bubble formation, after nucleation and cavitation. This would explain the initial very sharp inclination of the curve (Figs. 4 and 5) and the onward plateau appear to be independent on this decrease in surface tension. Furthermore, many authors find that there is a poor correlation between bubble size and surface tension but not many works deal with errors committed in their experimental work. Fig. 5 for instance, poses the problem of the data accuracy and reliability, which highlights this ignored fact. It seems to be clear that surface tension measurements depend on equipment (method) used, temperature and on water quality. This situation is clearly shown in Fig. 5, where curves are different even if the frother sample is the same. Thus, image of Fig.�3 400 500 600 700 800 900 1000 1100 0 5 10 15 20 25 30 35 40 45 [DF 250], mg.L-1 B ub bl e di am et er , µ m LTM-BSizer Drift flux Fig. 4. Bubble size (Mean Sauter Db) as a function of DF 250 concentration. Comparison between bubbles sizes measured using the LTM-BSizer (Jg, constant at 0.49 cm/s and Jw=0) and calculated by a drift flux method (Yianatos et al. 1988). 0 5 10 15 20 25 30 0.2 0.4 0.6 0.8 1.0 1.2 Superficial gas rate, cm·s-1 G as H ol du p, % [DF250], mg/L 5 10 20 30 40 Fig. 6. Gas hold-up values as a function of superficial gas rate (Jg), at different DF 250 frother concentration and JW=0.66 cm/s. 10 15 20 25 [DF250], mg/L 5 10 20 30 40 as H ol du p, % 82 E. Matiolo et al. / International Journal of Mineral Processing 99 (2011) 78–83 despite using Nima or Kruss tensiometers, which employ the same interaction of a platinum ring (DuNouy) with the surface being tested, using very pure and ions free water, the experimental values were fairly different (assuming that not many differences would be encountered between 24 and 27 °C). Unfortunately, Grau et al. data (2005) do not include temperature, neither informed about water quality (measurements appear to be done using a platinum ring). 0 5 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Superficial gas rate, cm·s-1 G Fig. 7. Gas hold-up values as a function of superficial gas rate (Jg), at different DF 250 frother concentration and JW=0 cm/s. 3.1. Gas dispersion parameters Figs. 6 and 7 show the experimental gas hold-up values as a function of superficial gas velocity (Jg) for Dowfroth 250 concentra- tions 5 to 40 mg L−1, and Jw of 0.66 and 0 cm/s, respectively. These figures show a typical increase in gas holdup with Jg. Also, for a constant Jg, the higher frother dosage the higher the gas hold-up. Yet, increasing the frother dosage, the hold-up values increase probably due to bubble size decreasing and again, after a certain concentration, this trend tends to level off (20–40 mg/L Dowfroth 250, in this case). According to Fig. 4, the bubbles decrease dramatically in size, but only at very low dosages. According to some authors, the CCC is reached at higher frother dosages, thus ceasing the increase of gas hold-up because the bubbles size reduction stops. Also, comparison of Figs. 6 and 7 shows that increasing the superficial liquid rate Jw from 0 to 0.66 cm/s, the gas hold-up increases for the same frother dosage and superficial gas rate Jg. Fig. 8 shows the relationship between the bubble surface area flux (Sb) and the gas hold-up (εg), with JW=0 cm/s, comparing experimental data (LTM-BSizer) and values calculatedby the drift- flux relationship (Yianatos et al., 1988). Experimental data shows a 56 60 64 68 72 76 0 10 20 30 40 50 60 Su rf ac e te ns io n, m N .m -1 Nima (this work, 24 ºC) Krüss (this work, 27 ºC) Rodrigues and Rubio, 2003, Krüss 25ºC Grau et al., 2005 [DF 250], mg.L-1 Fig. 5. Surface tension of aqueous solutions as a function of frother (DF 250) concentration. Values determined in different periods, conditions and authors. good correlation and results confirm that for the range of interest, the relationship between bubble surface area flux and gas hold-up is reasonably linear (as predicted by drift-flux), with a better fit at low Jg (closer to a countercurrent flow). This finding reinforces the fact that the gas hold-up can be considered as a good estimate of bubble surface area flux to characterize the flotation process (i.e. to correlate the kinetic rate constant in the collection zone). Fig. 9 shows the effect of the superficial liquid flowrate Jw on the Sb–εg relationship, calculated by drift-flux. According to this prediction an increase in Jw will increase the gas hold-up, keeping the gas rate and bubble size constant. Otherwise, for a constant gas hold-up the bubble surface area flux will decrease by increasing Jw, if the bubble size increases. 0 10 20 30 40 50 60 70 80 90 100 0 5 10 15 20 25 Gas Holdup, % B ub bl e su rf ac e ar ea f lu x (S b) , s -1 Jg, cm/s 0.33 0.49 0.66 0.82 0.49 LTM BSizer Fig. 8. Relationship between the bubble surface area flux (Sb) and the gas hold-up (εg), with JW=0 cm/s. image of Fig.�4 10 20 30 40 50 60 70 80 90 100 0 5 10 15 20 25 30 Gas Holdup, % B ub bl e su rf ac e ar ea f lu x (S b) , s -1 Jw = 0 cm/s Jw = 0.66 cm/s Fig. 9. Relationship between the bubble surface area flux (Sb) and the gas hold-up (εg), with JW=0 and Jw=0.66 cm/s. 83E. Matiolo et al. / International Journal of Mineral Processing 99 (2011) 78–83 4. Conclusions Gas dispersion parameters were measured in a well characterized laboratory column flotation cell. Gas hold-up and bubble size (and their distribution) were found to be strongly dependent on Dowfroth 250 concentration and on superficial gas velocity. A good relationship between experimental gas hold-up and bubble surface area flux (Sb) was found for experimental values and with those calculated using drift flux analysis for Jw=0. Data obtained are discussed in terms of solution, hydrodynamics and interfacial phenomena. The role of the frother in the energy dissipation in flow constrictors and in bubble generation and interfacial tensions was explored. Acknowledgments The authors gratefully acknowledge CAPES and CNPq for the scholarships awarded to E. Matiolo and F. Testa. Special thanks to Prof. R. T. Rodrigues, Camila Centeno and Alexandre Englert, from UFRGS, for thehelp in thebubble size and surface tensionmeasurements. J. Yianatos and J. Rubio wish to thank Conycit-Fondecyt, grant no. 7070233, for allowing the visit of J. Rubio to Chile and the research on flotation at U. 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Yianatos, J.B., Finch, J.A., Dobby, G.S., Xu, M., 1988. Bubble size estimation in a bubble swarm.Journal of Colloid and Interface Science 126 (1), 37–44. Yianatos, J.B., Henríquez, F., 2007. Boundary conditions for gas rate and bubble size at the pulp–froth interface in flotation equipment. Technical note. Minerals Engineering 20, 625–628. On the gas dispersion measurements in the collection zone of flotation columns Introduction Experimental Column flotation Gas hold-up measurement Bubble size measurement procedure Results and discussion Gas dispersion parameters Conclusions Acknowledgments References
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