12th European Conference on Mixing Bologna, 27-30 June 2006

PARTICLE DISTRIBUTION IN STIRRED TANKS: EXPERIMENTAL AND NUMERICAL INVESTIGATIONS IN DIFFERENT SCALES
R. Angst, M. Kraume* Technische Universitt Berlin, Department of Chemical Engineering, Sekr. MA 5-7 Strae des 17. Juni 136, 10632 Berlin, Germany Tel.: +49 30 314-23701, Fax: +49 30 314-21134 e-mail: Matthias.Kraume@TU-Berlin.de
Abstract. In this contribution, investigations of the local dispersed phase volume fraction in up to 69 discrete positions of vessels of 0.2, 0.4 and 0.9 m diameter are presented. The particle distributions show a large degree of homogeneity when a cloud height of 90 % is reached. A quantitative comparison of the different scales is used to validate the homogeneity achieved with the H90 criterion. Changes of the local concentration with stirrer speed higher and lower than nH90 are investigated as well. The results for nH90 are compared to other common scale-up rules. Furthermore CFD simulations of the 0.4 m diameter vessel have been carried out. In regions of high homogeneity the numerical predictions show a good agreement with the experimental results but fail to predict the complex phenomena adjacent the clear liquid layer. Key words: Particle distribution, Suspension, Mixing, Solid-liquid, Stirred tank, CFD

1. INTRODUCTION One of the most common apparatuses for solid-liquid processes is the stirred vessel. Because of the tendency of most two-phase systems towards segregation, for a successful application solids distribution must show a certain degree of homogeneity. Achievement, measurement and scale-up of particle suspension have been investigated extensively in the past due to its importance for many industrial applications [e.g. 1-13]. Still there remains a large discrepancy between the accuracy and reliability of the available knowledge and the industrial demand. While there are many scale-up rules, few have been validated regarding the particle distribution in different scales. In this contribution local measurements of the dispersed phase volume fraction are carried out by means of an endoscope based technique. The 90 % cloud height or H90 criterion is investigated regarding the provided homogeneity of the local particle concentration in different scales. To consider possible deviations due to a different interpretation of the criterion [14] the dependency of the local concentrations on the stirrer speed was also examined. The results are compared to several common scale-up rules. With the increasing availability of processor speed, CFD can deliver more precise predictions of these problems [e.g. 5, 12-15]. Still, the simulation of the fluid dynamics in stirred vessels requires special care due to the transient behaviour of the flow. In this paper special attention is drawn to the macro instabilities caused by the dispersed phase. For a valid comparison between time averaged experimental and simulation data it was found to be mandatory to consider the strong fluctuations of the transient flow.

2. METHODS 2.1 Experimental Investigations The investigations have been carried out in vessels with diameters of 0.2, 0.4 and 0.9 m. The vessels (H = D) were geometrically similar and featured four baffles, six bladed pitched blade turbines and a dished bottom (d/D = h/H = 0.3125). As dispersed phase glass beads with a mean diameter of 200 m were applied. The investigated mean volume fractions were 5 and 10 %. The measurement of the local dispersed phase volume fraction was carried out by means of a proprietary endoscope technique (Fig. 1). The dispersed phase is illuminated by a flashlight. The endoscope directs the light that is scattered back by the particles to a CCDCamera. By means of a computational grey scale analysis, the local volume fraction is calculated as a mean value of 50 to 150 images taken at a frequency of 1 Hz. The system was calibrated in a fluidized bed with volume fractions between zero and 15 %. Due to a probe diameter of 7 mm the comparative studies in the different scales showed no significant influence of the probe on the flow field and thereby on the distribution of the dispersed phase. A detailed description is already published [1]. In the vessels DN200 and DN400 the endoscope was inserted vertically, while in vessel DN900 it was inserted horizontally through the side-wall of the vessel. In the latter case the endoscope can be pulled out wide enough that the front lens of the endoscope is flush with the inner surface of the vessel. In consequence, measurements of the local dispersed phase volume fraction in the direct proximity of the wall can be carried out, without any disturbance of the flow field. The scale-up of stirred suspensions has been investigated extensively in the past. Most researchers concentrated on the scale-up based on the just-suspended criterion. The corresponding state of complete suspension is certainly an important benchmark, but, given a complete suspension, the homogeneity of the suspension is of higher significance for many applications. Few quantitative studies on the homogeneity have been published. Besides the work of Buurman [6], extensive studies of industrially sized vessels have been published by Mak [10]. He states a decreasing homogeneity of the suspension in larger scales, when the complete suspension is used as a scale-up criterion. To provide a constant homogeneity of the local dispersed phase volume fraction in different scales Mak, like other authors (e.g. Molerus, Latzel, Judat in [17]) suggests P/V = const..
Fig. 1: Experimental set-up

2.2 Numerical Investigations The numerical investigations were carried out with the commercial code CFD 5.7.1 for the vessel DN400. A block structured grid of 180 was used with 104384 cells in the rotor and 282123 cells in the stator domain. The grid resolved the thickness of the stirrer-blades but considered the baffles as thin-surfaces. To obtain a good convergence, the residuals for each cell were observed and local refinements of the grid were accomplished to selectively reduce the local residuals where necessary. Nevertheless, the average, global RMS residuals are affected by high, local residuals in small regions at the blades and the bottom of the vessel. In consequence, for the vast majority of the cells, the residuals are significantly lower than indicated by the plotted averaged global RMS residuals. The mean dispersed phase volume fraction was kept constant during the calculations. The simulations were carried out with the Eulerian-Eulerian multi-fluid model. The SST turbulence model was applied. The numerical simulations presented in this contribution were calculated using the transient rotor-stator (sliding-mesh), as well as the frozen-rotor approach [18] that offers a significant reduction of the calculation time. The timesteps for the latter were set to be chosen automatically. For the transient rotor-stator simulation timesteps corresponding to a 5 rotation of the stirrer between two timesteps was chosen. For each timestep six iterations were calculated. The quasi-stationary frozen-rotor method does not resolve the various positions of the stirrer, but applies a rotating coordinate system for the rotor-part of the grid and thereby considers the transient interactions between rotor and stator. Despite the fact that it is considered stationary, the approach requires a discretisation of the time. Since the flow field in a stirred vessel is transient, a constant, stationary numerical solution is only obtainable with a high amount of numerical stabilisation. This can be accomplished e.g. by means of a coarser grid or more robust discretisation schemes. However, it is not likely, that the solution of a transient phenomenon that is forced to be stationary is valid. If it is at all, then only for a certain point of time and not for an average solution that one may associate with a stationary solution. In the frozen-rotor simulation the calculated variables vary, despite the fact that the residuals remain almost constant, thus the values depend on the number of iterations. These fluctuations of the variables can be observed in single phase as well as two-phase systems. A similar behaviour is typical for the transient rotor-stator approach. Here for each discrete timestep several iterations are calculated, resulting in a different value of each variable for each timestep, corresponding to the transient flow in a stirred vessel. In consequence for both approaches, frozen-rotor and transient rotor-stator, a comparison with time averaged experimental data can only be accomplished by averaging the calculated values as well. This can be done by averaging either over a number of timesteps in the case of transient rotor-stator calculations, or over a number of iterations when the frozen-rotor approach is applied. In any case the number of timesteps or iterations has to be large enough to capture a sufficient number of the occurring fluctuations. This leads, especially in the case of a transient rotor-stator approach, to very long calculation times. This is especially true for solid-liquid systems since the maximum timescale of the macro instabilities of the suspended, dispersed phase is significantly larger than in a single phase system. The maximum timescale of the fluctuations is limited by the size of the grid and the periodic boundaries involved (here: 180). 3. RESULTS 3.1 Experimental Investigations The local dispersed volume fraction for the investigated vessels is depicted in Fig. 2 a. The stirrer speed in each case was adjusted to provide a cloud height of 0.9 H, except for the ves-

sel DN900 where the cloud height was slightly higher. The abscissas of the three diagrams indicate the radial and vertical position of the measuring points relative to the geometry of the vessel at three different bottom distances of 0.25, 0.55 and 0.75 H. The ordinates show the local volume fraction of the dispersed phase. The concentration profiles show a rather high degree of homogeneity below a bottom clearance of 0.75 H. Significant differences from the mean concentration can only be observed at the shaft, where the local dispersed phase volume fraction is reduced, and at the wall. In the latter region the local concentration is decreased at a bottom distance of 0.75 H. At lower bottom distances local concentrations higher than the mean concentration were found at the wall. Fig. 2 b shows the local concentrations in the vessel DN900 for a stirrer speed higher (275 min-1) and lower (239 min-1) than nH90. Here the abscissas indicate the mean concentration of 5 %vol.. Due to the reduced could height at a bottom distance of 0.85 H the local concentrations for n = 239 min-1 are lower then for n = 275 min-1, where the local concentrations are close to the mean concentration of 5 %vol.. At bottom distances 0.75 and 0.65 H the local concentrations are almost identical. For lower bottom distances the local concentrations for n = 239 min-1 are higher than for n = 275 min-1.

[%vol.] ]

275 1/min
[%vol.]
12 8 r/R [-] 4 0 0,15 12 8 4 0 0,15 0,35 0,55 0,75 0,95 0,35 0,55 0,75 0,95

10

239 1/min

h/H [-] 0,85

0,75

0,75 H

0,65

0,55

0,55 H

0,45
12 8 4 0 0,15 0,35 0,55 0,75 0,95

0,35

0,25

0,25 H

0,15

0,15

0,35

0,55

0,75 r/R [-]

0,95

a)

b)

Fig. 2: Experimental results of the (a) local dispersed volume fraction for DN200, DN400, DN900 (b) local dispersed volume fraction for DN900 5%vol.; 200m particles, cloud height 0.9 H (except DN900); 678 min-1 (0.2 m vessel, 5 %vol.), 877 min-1 (0.2 m vessel, 10 %vol.), 419 min-1 (0.4 m vessel, 5 %vol.), 538 min-1 (0.4 m vessel, 10 %vol.), 275 min-1 (0.9 m vessel, 5 %vol., n > nH90), 239 min-1 (0.9 m vessel, 5 %vol., n < nH90)

Despite the fact that in Fig. 2 a in all investigated cases (except DN900) the cloud height matched 0.9 H, the local concentrations below a bottom distance of 0.75 H are close to the mean concentration. With the reduced local concentration at a bottom distance at 0.75 H and

the virtually particle-free zone above 0.9 H one would assume a higher local concentration below 0.75 H. Fig 2 b shows that this is true for a cloud height < 0.9 H while Fig 2 a indicates no significant reduction of the local concentrations below 0.75 H for a cloud height > 0.9 H (for DN900, 5 %vol.) compared to a could height of 0.9 H (DN200 and DN400, 5 %vol.). Other experimental investigations showed that with an increasing cloud height > 0.9 H the local concentration near the surface increases up to the mean concentration, while there is little or no reduction of the local concentrations in the measuring points located below 0.55 H. In Fig. 3 the specific 10,0 power input * (with = P/V) 5 %vol. 10 %vol. is shown for a particle diameP/V = const. ter of 200 m and mean dis- 0.33 P/V ~ D-0,33 (Nienow) persed phase volume fracwtip Tip = const. tions of 5 and 10 %. The abscissa shows the scale up facn > nH90 tor D/D0 with D0 representing the smallest investigated ves1,0 n < nH90 sel DN200. The stirrer speed matched a could height of 0.9 D except for the vessel DN900 with a mean dispersed phase volume fraction of 5 %vol., where the cloud height was either below or above 0.9 0,1 D. As Fig. 3 indicates, the 1 10 experimental results of the Scale-up factor D/D0 related power input can be approximated best with constant power by volume. Fig. 3: Measured relatedc power input * for DN200 ( , D ), DN400
Related power input * *= = //0 0
0 0

and DN900, particle diameter 200 m, 5 and 10 %vol., stirrer speed according to a cloud height of 0.9 H except for DN900, 5 %vol.

3.2 Numerical Investigations In Fig. 4 results of two different calculations are shown. For iteration 0-4600 the frozen-rotor approach was applied and the abscissa indicates the number of iterations. For 4600-8200 the abscissa no longer indicates the number of iterations but the number of timesteps for the transient rotor-stator simulation that was started using the results from the earlier frozen-rotor calculation as initial guess. Here for each timestep six iterations were calculated. The residuals are spread vertically since they show the development of the residuals after each iteration. Due to the change of the abscissa from iterations to timesteps, the entire abscissa is no longer equivalent to the calculation time. Since there are six iterations calculated per timestep, a certain measure on the abscissa for the frozen-rotor calculation equals one sixth of the calculation time for an equivalent measure of the transient rotor-stator calculation. The residuals of the frozen-rotor simulation in Fig. 4 a exhibit a plateau phase starting at 2500 iterations. The high absolute value of the RMS residuals is, as mentioned above, due to high local residuals in few regions of the grid that affect the RMS residuals. Despite the fact that the residuals are not becoming smaller anymore, the corresponding local concentrations show fluctuations. The result of this frozen-rotor simulation therefore is strongly dependent on the number of iterations. Variations of the local dispersed phase volume fraction of up to 4 % occur at pos. 3 located adjacent the clear liquid layer.

It is questionable that there is a correct number of iteration after which the local dispersed phase volume fraction is equivalent to the time averaged condition that is usually associated with a quasi stationary frozen-rotor simulation. To calculate the distribution of the dispersed phase without a dependency on the number of iterations, the local concentrations in the measuring points were averaged. Here the average local concentrations were calculated as mean values between 2500 and 4500 iterations. Similar fluctuations of the local dispersed phase concentration can be observed for the transient rotor-stator simulation from timestep 4600 to 8200. The duration of 3600 timesteps is equivalent to 50 revolutions of the stirrer or 7.2 s of real time at a stirrer speed of 419 min-1. The maximum range of the local variations is with more than 4 %vol. (or 80 % of the mean dispersed phase volume fraction) comparable to the frozen-rotor simulation. The transient, wave like behaviour of the calculated particle cloud adjacent the clear liquid layer (near pos. 3) is in agreement with the experimental observations. For the transient simulation the residuals are significantly decreased. In Fig. 5 the agreement of numerical and experimental a) 1,E-02 U Momentum Volume fraction results is remarkably good for V Momentum bottom distances below 0.75 H W Momentum k 1,E-03 with the frozen-rotor results slightly over-predicting the loTransient cal concentration at a bottom Rotor-Stator 1,E-04 distance of 0.25 H. At a bottom distance of 0.75 H the experiFrozen-Rotor mental results of the local vol1,E-05 ume fraction are over predicted by both numerical approaches. While for related radiuses be1,E-06 low r/R = 0.45 the agreement 8 with the experimental results is b) pos. 3 pos. 8 pos. 11 still good, the deviations in7 crease in the proximity of the wall to 50 %. Despite the fact 6 that there is no underestimation 5 of the predicted concentrations at smaller bottom distances this 4 behaviour is not related to pos3 sible problems with the mass balance, since this was checked 2 after each timestep. The effect is in agreement with the ex1 0 1000 2000 3000 4000 5000 6000 7000 8000 perimental results in Fig. 2 a. Number of Iterations / Timesteps Here likewise (for DN900, 5 %vol.) a cloud height larger Fig 4: a) Residuals and b) selected corresponding local dispersed than 0.9 H does not lead to a phase volume fractions, 200m particles,5 %vol., 0-4600 iterations: frozen-rotor, timestep 4600-8200: transient rotor-stator, symbols indireduction of the local concencate the variables not the number of data points (pos. 3: h/H = 0.75, trations below the mean disr/R = 0.6; pos. 8, h/H = 0.55, r/R = 0.6 D; pos. 11, h/H = 0.45, r/R = persed phase volume fraction 0.3) for bottom distances smaller than 0.75 H. The effect obLocal dispersed phase volume fraction [%vol.] Residuals (RMS)

served here is more likely to be an overestimation of the cloud height due to an improper modelling of the macro-instabilities introduced by the dispersed phase. 4. CONCLUSIONS The experimental results of the local dispersed phase volume fractions show no significant inhomogeneities below the cloud height of 0.9 H and match well for the differently sized vessels. No evidence for the existence of a pronounced local minimum in the centre of the circulation loop, as it is predicted by 8 some CFD-simulations [e.g. 15] was found. 4 r/R [-] A stirrer speed slightly larger than nH90 was found to have little impact on the local con0 0,2 0,4 0,6 0,8 centrations measured below 0.75 H. 8 For the investigated systems the scale-up 4 according to P/V = const. was found to match a cloud height of 0.9 H well. 0 Due to the high fluctuation of the simu0,2 0,4 0,6 0,8 lated local concentrations, averaging was found to be mandatory to be able to com8 pare them to time averaged experimental 4 values. To avoid the time consuming procedure 0 of averaging, a model for the large scale 0,6 0,8 macro instabilities acting like a high-pass, transient simulation similar to the low-pass function of turbufrozen-rotor simulation lence models, has to be implemented. experimental data It can be assumed that the fluctuations of the local dispersed phase volume fraction observed for the frozen-rotor simulation are Fig 5: Local concentrations, 200 m particles, 5 %vol., due to turbulence induced macro instabiliDN400, 419 min-1, frozen-rotor and transient rotorties that that are not related to the transient stator simulation, experimental data rotor-stator interaction. It can be concluded that the agreement of experiment and numerical simulation is good in regions of high homogeneity. At the 0.9 H, the cloud height, where high concentration gradients with fast and erratic wave like structures of a large timescales occur, the quality of the prediction is not satisfying. This may be due to the large time scale of these fluctuations or the comparably few oscillations included in the averaging of the final result.
[%vol.]

NOMENCLATURE D d H h n R r Indices H90 [m] [m] [m] [m] [min-1] [m] [m] diameter of the vessel diameter of the stirrer height of the vessel height stirrer speed radius of the vessel radius

0.25 D

0.55 D

0.75 D

90% cloud height

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