Comparison of solids suspension criteria based on electrical impedance tomography and visual measurements

Similar documents
ASSESSMENT OF THE MINIMUM POWER REQUIREMENTS FOR COMPLETE SUSPENSION IN TOP-COVERED UNBAFFLED STIRRED TANKS

Dense Solid-Liquid Suspensions in Top-Covered Unbaffled Stirred Vessels

Application of the CFD method for modelling of floating particles suspension

Comparison of Agitators Performance for Particle Suspension in Top-Covered Unbaffled Vessels

EffectofBaffleDesignontheOff-bottomSuspensionCharacteristics ofaxial-flowimpellersinapilot-scalemixingvessel

CFD Analysis and Experimental Evaluation of the Effective Parameters on Paint Homogeneity in Mixing Tanks

An Overview of Impellers, Velocity Profile and Reactor Design

Calculation of Power, Shear and Gas-liquid mass transfer in reactors for fermentation.

Michael Kinzel Leonard Peltier Andri Rizhakov. Jonathan Berkoe Brigette Rosendall Mallory Elbert

AN OVERVIEW OF IMPELLERS, VELOCITY PROFILES AND REACTOR DESIGN

CFD SIMULATIONS OF SINGLE AND TWO-PHASE MIXING PROESSES IN STIRRED TANK REACTORS

Rouzbeh Jafari, Philippe A. Tanguy, and Jamal Chaouki. 1. Introduction

Comparison of Different Techniques for Modelling of Flow Field and Homogenization in Stirred Vessels*

ENGG 199 Reacting Flows Spring Lecture 4 Gas-Liquid Mixing Reactor Selection Agitator Design

MIXING 97 Multiphase Systems

CFD SIMULATION OF SOLID-LIQUID STIRRED TANKS

PARTICLE SUSPENSION WITH A TX445 IMPELLER

UNIVERSITA DEGLI STUDI DI PISA. Facoltà di Ingegneria Corso di Laurea in Ingegneria Chimica. Tesi di Laurea

Chaos in mixing vessels

Effect of Geometry on the Mechanisms for Off-Bottom Solids Suspension in a Stirred Tank

Effect of Suspension Properties on the Electrochemical Method. Ing. Kamila Píchová

Free Surface Instabilities in a Model Unbaffled Bioreactor

Evaluation of Large Eddy Simulation and Euler-Euler CFD Models for Solids Flow Dynamics in a Stirred Tank Reactor

AGITATION AND AERATION

Experimental Investigation and Optimization of Solid Suspension in Non-Newtonian Liquids at High Solid Concentration

CFD ANALYSIS OF TURBULENCE EFFECT ON REACTION IN STIRRED TANK REACTORS

PIV Measurements to Study the Effect of the Reynolds Number on the Hydrodynamic Structure in a Baffled. Vessel Stirred by a Rushton Turbine

AGITATION/GAS-LIQUID DISPERSION. CHEM-E Fluid Flow in Process Units

Effect of Baffles Geometry on Hydrodynamics in a Mechanically Agitated System

Power requirements for yield stress fluids in a vessel with forward-reverse rotating impeller

THE VELOCITY FIELD IN THE DISCHARGE STREAM FROM A RUSHTON TURBINE IMPELLER

Effect of the Tank Design on the Flow Pattern Generated with a Pitched Blade Turbine

MASS TRANSFER EFFICIENCY IN SX MIXERS

EFFECT OF IMPELLER TYPE AND NUMBER AND LIQUID LEVEL ON TURBULENT BLEND TIME

APPLICATION OF MODELS WITH DIFFERENT COMPLEXITY FOR A STIRRED TANK REACTOR

Oxygen transfer, mixing time and gas holdup characterization in a hybrid bioreactor

Copyright Warning & Restrictions

Effect of a Continuous Feed on the Fluid-Dynamics of a Mechanically Stirred Tank

PIV STUDY OF MIXING CHARACTERISTICS IN A STIRRED VESSEL WITH A NON-NEWTONIAN FLUID

Three-phase reactors with mechanical agitation are commonly used

Simulation of Multiphase Flow in Stirred Tank of Nonstandard Design

THINK FLUID DYNAMIX Mixing, Homogenization & Blend Time. THINK Fluid Dynamix

1. Starting of a project and entering of basic initial data.

Chemical Engineering Science

RELATION BETWEEN PARTICLE RISING BEHAVIOR AND LIQUID FLOW AROUND THE BOTTOM OF A STIRRED VESSEL

Solid-Liquid Mixing In Agitated Tanks : Experimental And CFD Analysis

Dynamic Effect of Discharge Flow of a Rushton Turbine Impeller on a Radial Baffle J. Kratěna, I. Fořt, O. Brůha

Assessing Mixing Sensitivities for Scale-up. Matthew Jörgensen Atlanta, 10/20/2014

- A Comic by Hugh Macleod.

PHEN 612 SPRING 2008 WEEK 12 LAURENT SIMON

STUDY ON THE HOMOGENIZATION SPEED IN A TANK EQUIPPED WITH MAXBLEND IMPELLER

M Manuela R da Fonseca, DEQB. Mixing

Blade Angle Effects on the Flow in a Tank Agitated by the Pitched-Blade Turbine

Computer Life (CPL) ISSN: The Numerical Simulation on Internal Gas-liquid Two Phase Flow Field of. Three Layers of Air Stirred Reactor

Direct Production of Crystalline Boric Acid through Heterogeneous Reaction of Solid Borax with Propionic Acid: Operation and Simulation

CFD Analysis of a Stirred Vessel Bioreactor with Double Pitch Blade and Rushton Type Impellers

PLO MIXING AND RTD IN TANKS: RADIOTRACER EXPERIMENTS AND CFD SIMULATIONS

Flow Generated by Fractal Impeller in Stirred Tank: CFD Simulations

PIV measurement and study on turbulence generator flow field of medium consistency pump

NUMERICAL STUDY OF THE EFFECT OF BLADE SZE ON PUMPING EFFECTIVENESS OF A PADDLE IMPELLER IN AN UNBAFFLED MIXING VESSEL

Liquid Mixing in Agitated Vessels

The Role of Rheology in the Flow and Mixing of. Complex Fluids

Experimental determination of the agitation requirements for solids suspension in dissolution systems using a mini paddle apparatus

Large-eddy simulations (LES) have been used to study solids dispersion in an

ENGG 199 Reacting Flows Spring Lecture 2b Blending of Viscous, Non-Newtonian Fluids

A study of mixing by PIV and PLIF in bioreactor of animal cell culture

We are IntechOpen, the world s leading publisher of Open Access books Built by scientists, for scientists. International authors and editors

PIV MEASUREMENTS AND CFD SIMULATION OF VISCOUS FLUID FLOW IN A STIRRED TANK AGITATED BY A RUSHTON TURBINE

EXPERIMENTAL INVESTIGATION AND CFD MODELING OF MICROMIXING OF A SINGLE-FEED SEMI-BATCH PRECIPITATION PROCESS IN A LIQUID-LIQUID STIRRED REACTOR

Three-dimensional measurements in the baffle region of a turbulently stirred tank

Estimation of Agitator Flow Shear Rate

Study on residence time distribution of CSTR using CFD

THE COMPUTATIONAL-FLUID-DYNAMICS STUDY OF AN UNBAFFLED STIRRED VESSEL WITH ECCENTRICALLY POSITIONED IMPELLER

MASS TRANSFER COEFFICIENTS DURING AERATION BY A SELF-ASPIRATING IMPELLER

Experimental measurement and computational fluid dynamics simulation of mixing in a stirred tank: a review

Chapter Four. Experimental

mixing of fluids MIXING AND AGITATION OF FLUIDS

Experimental and Numerical Investigation of Two- Phase Flow through Enlarging Singularity

Research Article Performance of Single and Double Shaft Disk Separators

Characterization of slurry systems by ultrasonic techniques

Numerical Simulation of Flow Field in a Elliptic Bottom Stirred Tank with Bottom Baffles

Particle size analysis -Chapter 3

Turbulence Characteristics in a Rushton Stirring Vessel: A Numerical Investigation

EVALUATION OF THE EFFECT OF PITCHED BLADE TURBINE ON MIXING IN AN ELECTROCHEMICAL REACTOR WITH ROTATING RING ELECTRODES.

ISEC The 21st International Solvent Extraction Conference. Standardized Settling Cell to Characterize Liquid-Liquid Dispersion

Modeling of dispersed phase by Lagrangian approach in Fluent

INVESTIGATION OF TURBULENCE MODULATION IN SOLID- LIQUID SUSPENSIONS USING PARALLEL COMPETING REACTIONS AS PROBES FOR MICRO-MIXING EFFICIENCY

Flow structures in solid-liquid suspensions in mixing and confined jets

The experimental study of the coherent structures generated in the agitated vessels and effected by fluid viscosity

Effect of column diameter on dynamics of gas-solid fluidized bed: A statistical approach

ARTICLE IN PRESS. chemical engineering research and design x x x ( ) xxx xxx. Contents lists available at ScienceDirect

Rheology of strongly sedimenting magnetite suspensions

Separationsteknik / Separation technology

International Journal of Scientific & Engineering Research, Volume 6, Issue 5, May ISSN

Investigation of Blend Time for Turbulent Newtonian Fluids in Stirred Tanks

CHAPTER 7 NUMERICAL MODELLING OF A SPIRAL HEAT EXCHANGER USING CFD TECHNIQUE

Large eddy simulations of flow instabilities in a stirred tank generated by a Rushton turbine *

EFFECT OF DISTRIBUTION OF VOLUMETRIC HEAT GENERATION ON MODERATOR TEMPERATURE DISTRIBUTION

LIQUID FILM THICKNESS OF OSCILLATING FLOW IN A MICRO TUBE

Mixing Performance of Counter-Axial Flow Impeller using Computational Fluid Dynamics

Transcription:

1 2 3 4 Comparison of solids suspension criteria based on electrical impedance tomography and visual measurements Petri Tervasmäki*, Jari Tiihonen, Heikki Ojamo *Corresponding author, petri.tervasmaki@oulu.fi, +358 40 5474973 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 Abstract Different approaches have been adopted to quantify the performance of stirred vessels in suspending sinking solids into liquid phase. In this study we used electrical impedance tomography (EIT) to estimate the solids distribution in a lab-scale stirred vessel with a diameter of 362 mm. Also visual measurements were made to determine the cloud height and just suspended impeller speed. Quartz sand with a density of 2650 kg/m 3 was employed as the solid phase with different particle size fractions from 50 to 180 µm and solids volume fractions of 7.5 and 15 %. The effect of impeller type was studied by using two axial flow impellers, a pitched blade turbine and a hydrofoil impeller. Two different states partial and homogeneous suspension were defined from the EIT data in addition to visual measurement of complete off-bottom suspension and cloud height. Partial suspension was determined from the EIT data, and it was reached at relatively low agitation rates. Visual measurements and data from the literature also support this observation, and EIT was proved to be a suitable method to quantify a repeatable partial suspension criterion. Complete off-bottom suspension was measured visually by determining the agitation rate at which there were no stationary solid particles at the vessel bottom for longer than 2 seconds. However, the applicability of this widely used criterion was questioned in the case of dense suspensions of small particles. Homogeneous suspension was estimated from the EIT data, and it was reached by approximately doubling the impeller revolution rate from the partial suspension criterion. The hydrofoil impeller reached all states of suspension with lower power consumption compared to the pitched blade turbine. 1

26 27 28 Keywords Solid-liquid mixing; electrical impedance tomography; homogeneity; suspension criteria; axial flow impeller 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 1 Introduction Solid-liquid suspensions are encountered frequently in different areas of process industries, and stirred vessels used in mixing the two phases have been under extensive research for decades. Factors that affect the suspension of solid particles to the liquid phase include physical properties of solid and liquid phases, the fraction of solids relative to liquid, geometric parameters of the system and agitation conditions. The state of suspension is often divided into three separate criteria, on-bottom motion (or partial suspension), off-bottom suspension and homogeneous suspension (Atiemo-Obeng et al., 2004). Partial suspension is defined as a state at which most of the solids are moving at the vessel bottom excluding a formation of fillets at some parts. Off-bottom suspension (or complete suspension or just suspended impeller speed, Njs) was first defined by Zwietering (1958) as an agitation rate at which no particles remain at the vessel bottom for more than 1 2 s. Homogeneous suspension refers to a state in which the particles are uniformly distributed throughout the vessel. The definition of partial suspension is rather broad and there are different approaches to experimentally measure this state of suspension (Bujalski et al., 1999;Chudacek, 1986;Micale et al., 2002). Njs and homogeneous suspension are clearly defined. However, the applicability of Njs is questionable for dense suspensions of small particles (Kraume and Zehner, 2001), and the determination of homogeneous suspension requires more detailed knowledge of the distribution of the solid phase. Several methods have been used to assess the state of suspension. Visual methods are simple and can be used to determine the just suspended impeller speed (Njs) and a level at which the solids rise at a certain agitation rate, usually referred to as cloud height (CH). Micale et al. (2002) used a pressure gauge at the vessel bottom to determine the fraction of suspended solids in relation to total solids. Kraume (1992) and Bujalski et al. (1999) compared different visual states of suspension (cloud height, Njs) to mixing time and concluded that the effect of solids on the mixing time compared to the mixing time of liquid alone can be divided into the following phases. First, when only a small fraction is suspended, the mixing time of the suspension is 2

56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 similar to the case of liquid only. At this point, the liquid circulates efficiently and the few suspended particles may be distributed almost throughout the vessel. With increasing agitation, a larger fraction of the particles are suspended resulting in a non-steady circulating flow and decreased cloud height. The longest mixing time is measured at this point and a further increase in the agitation rate increases the cloud height while the mixing time decreases. These methods describe the state of suspension to some extent but they fail to give detailed information on the distribution of solids inside the vessel. Local solids concentration can be measured either by direct sampling (Barresi and Baldi, 1987;MacTaggart et al., 1993) or indirectly by comparing differences in the solids concentration to optical (Angst and Kraume, 2006;Ayazi Shamlou and Koutsakos, 1989;Fajner et al., 1985;Magelli et al., 1990;Magelli et al., 1991;Montante et al., 2003) or electrical (Špidla et al., 2005) properties of the suspension. As pointed out by MacTaggart et al. (1993), it is difficult to gain a representative sample from a complex two-phase flow, and optical methods are usually restricted by the solids concentration. Electrical impedance tomography also makes use of conductivity differences between the phases and has only recently been used to quantify solid-liquid mixing (Harrison et al., 2012;Hosseini et al., 2010;Stevenson et al., 2010;Tahvildarian et al., 2011). Other recent measurement methods which have been used to measure the distribution of solids include magnetic resonance imaging (Stevenson et al., 2010) and particle tracking methods such as positron emission particle tracking (PEPT) (Guida et al., 2011). In this article, we apply electrical impedance tomography to measure the solids suspension and distribution in a stirred vessel with moderate to dense solids concentration (XV = 7.5 15 %) and small particle sizes (< 180 µm). The results from the EIT-measurements are also compared with traditional visual measurements of Njs and cloud height. In addition, criteria to determine the states of partial and homogeneous suspension from the EIT data are presented. 81 82 83 84 2 Materials and Methods 2.1 Experimental Setup The experiments were conducted in a flat-bottomed stirred vessel with an inner diameter T = 362 mm equipped with four baffles with a width of 0.12T. Impeller type, particle size of solids, 3

85 86 87 88 89 solids loading and agitation rates were varied during the experiments. Two types of impellers were used, a four-bladed pitched blade turbine (4PBT) with a blade angle of 45 and a diameter D = 155 mm and an Outotec OKTOP3200 which is a three-bladed hydrofoil impeller with D = 145 mm. The impellers are presented in Figure 1. Both impellers were positioned with an offbottom clearance C = 0.9D. 90 91 92 93 94 95 96 97 98 99 100 Figure 1. a) A 4-bladed pitched blade impeller with a blade angle of 45, D = 155 mm and b) OKTOP3200, a 3-bladed hydrofoil impeller, D = 145 mm Quartz sand with a density of 2650 kg/m 3 was sieved to known fractions of particle size, and the fractions that were used in the experiments were 50 75, 75 100 and 125 180 μm. Solids concentration varied from 200 to 400 g/l (volume fraction XV = 7.5 15 %). Tap water at room temperature (22 C) was used as the liquid phase. Each combination of impeller type and slurry properties (XV and dp) was measured at 13 agitation rates. Different ranges for impeller revolution rates were used depending on the impeller type and solids properties in order to reach all desired levels of suspension. Experimental conditions are presented in detail in Table 1. Table 1. Solids concentration, particle size and agitation rates that were used for the experiments XV dp N [] % μm OKTOP3200 4PBT 7.5 50-75 125-500 - 15 50-75 125-500 - 7.5 75-100 125-500 100-320 15 75-100 125-500 100-320 7.5 125-180 200-650 150-500 15 125-180 200-650 150-500 101 102 103 2.2 Electrical Impedance Tomography (EIT) The stirred vessel was equipped with an electrical impedance tomography measurement system (Numcore Ltd, Finland). The Numcore EIT system consists of three operational blocks: the 4

104 105 106 107 108 109 110 111 112 113 114 115 116 117 118 119 120 121 122 123 124 125 126 127 128 129 130 electrodes that form the interface between the process and the measurement system, an EIT- device that performs the current injection, voltage measurements and signal processing and, finally, a PC with software that generates the tomographic image. The details of the measurement system and image reconstruction are presented by Heikkinen et al. (2006). Circular electrodes were attached to the inner surface of the vessel in nine planes with four electrodes per plane. A slightly modified opposite current injection strategy was used with a total of 28 independent current injections. An adjacent strategy, where voltages are measured from adjacent electrodes, was used for the voltage measurements. The solution domain based on the reactor geometry was discretized into a mesh consisting of tetrahedral elements with a total of 16032 elements and 76145 nodes. Reference data for the EIT-measurement were recorded from a vessel that was filled with water only. Baffles and other interiors were present during the reference data capture, and separate reference data sets were recorded for different impellers. Solids concentration at a certain conductivity value was calculated by the Equation (2.1)., / = X (2.1) Where Xi,ms/Vtot is the solids concentration at height i [gsolids / l] σmax is the maximum conductivity of the vertical profile [ms/cm] σavg is the average conductivity of the vertical profile [ms/cm] σi is the conductivity at height i [ms/cm] X is the average solids concentration [gsolids / l] 2.3 Other measurements In addition to EIT, the suspension was also examined visually during the measurements. Cloud height was determined for each measurement as the height at which the solids remained stationary for some time. There were local bursts towards higher and lower cloud height, but a height at which the cloud height remained constant for some time could be distinguished. Also Njs was determined visually for each reactor and slurry configuration by observing the transparent bottom of the vessel in well-lit conditions so that movement of the particles could be distinguished. A criterion where no particles remained stationary for more than 2 seconds was used for Njs. 5

131 132 133 134 In order to measure power consumption, the vessel was placed on a table that rotates freely, and the force exerted by this rotation was measured with a force transducer. When, in addition to the measured force, the distance from the centre of the tank to the force transducer and impeller rotational speed are known, impeller power draw can be calculated by the Equation (2.2). 135 136 137 138 where = 2 (2.2) P is the power draw of the impeller [W] F is the measured force [N] r is the length of lever arm [m] N is the impeller rotational speed [s -1 ] 139 140 141 142 143 144 145 146 147 148 149 150 151 152 153 154 155 156 3 Results and Discussion 3.1 Suspension criterion from the EIT data A typical EIT data set from one measurement is presented in Figure 2 where the average conductivity at three separate planes is plotted against time. Impeller revolution rate was increased stepwise from 125 to 500 during the measurement. At the agitation rates from 125 to 190, some stationary solids were gradually lifted to the suspension and also sudden, occasional bursts of solids could be distinguished. These can be seen as a fluctuation of the conductivities during a constant agitation rate. At 210, however, the conductivity at the lowest plane reaches a minimum and a steady state of conductivity is reached throughout the vessel. Further increase in the agitation rate results in an almost instantaneous step change of the conductivities towards a more homogeneous suspension. It can be concluded from the visual inspections that this condition of minimum conductivity at the bottom was not equal to the just suspended criterion Njs as suggested by Ayazi Shamlou and Koutsakos (1989) and Nienow (1997), but there were always stationary solid particles remaining at the vessel bottom. A similar trend was found for all measurements, and this state of suspension will be referred to as partial suspension criterion (Nps) and can be interpreted as the maximum concentration of solids at the bottom part of the vessel. A further increase in the agitation rate still withdraws some stationary solids from the bottom but it also lifts more of the 6

157 158 suspended solids to the upper parts of the vessel resulting in a decrease in the local solids concentration at the lower parts. 0,215 0,21 Conductivity [ms/cm] 0,205 0,2 0,195 0,19 125 150 170 190 210 230 250 275 300 350 400 450 500 0,185 0:00:00 0:10:00 0:20:00 0:30:00 0:40:00 0:50:00 1:00:00 1:10:00 1:20:00 159 160 161 162 163 164 165 166 167 168 169 170 171 172 173 time [h:mm:ss] 5.5 cm 17.7 cm 34.4 cm Figure 2. Conductivity at levels 5.5 cm (0.15 H), 17.7 cm (0.49 H) and 34.4 cm (0.95 H). OKTOP3200 impeller, 4 baffles, dp = 75 100 μm, XV = 7.5 % A repetitive pattern was also found in cloud height measurements at Nps. Below this agitation rate, cloud height either could not be determined, remained constant or even decreased with increasing agitation. Only above this agitation rate cloud height increased monotonically with agitation. This finding is similar to the one reported by Bujalski et al. (1999), Kraume (1992) and Michelett et al. (2003). For relevant particle sizes, the maximum mixing time occurs at agitation rates below Njs together with a discontinuity in cloud height. After reaching the maximum value, mixing time quickly decreases and cloud height increases with increased agitation. Micale et al. (2002) used a pressure gauge at the vessel bottom to assess the amount of unsuspended solids and fitted the data with a two-parameter model to calculate an impeller revolution rate at which 98 % of the particles were suspended. On average, an increase of 30 % in agitation rate was required to suspend the last 2 % of the particles resulting in a twofold increase in power consumption. Thus, 98 % suspension was referred as sufficient suspension, 7

174 175 176 177 178 179 180 181 182 183 184 185 186 187 Nss. The relationship between Nps and Njs in our experiments was somewhat similar, Njs being on average 40 % larger than Nps. However, no clear correlation between the two suspension criteria could be established and the variation of Njs with respect to Nps was quite high as will be pointed out in the next sections. As a conclusion, it can be stated that the fluctuation in the EIT data at the low agitation rates can be explained by the non-steady circulating flow suggested by Kraume (1992) and the lowest applicable impeller revolution rate should always be above the partial suspension criterion. It is easy to determine from the EIT data and it gives more consistent results compared to the visual measurement of Njs which is problematic to determine especially for high solids concentrations and small particle sizes. The effect of geometric parameters and suspension properties on the partial suspension (Nps) and Njs is assessed in later sections. 3.2 Homogeneous suspension Beyond the partial suspension criterion, the homogeneity of the suspension can be assessed by calculating the relative standard deviation (RSD) of the axial concentration profile = 1 1 1 ( ) (3.1) 188 189 190 where X is the mean solids fraction X is the average solids fraction at measurement height i n is the number of vertical data points 191 192 193 194 195 196 197 198 199 200 RSD of the axial concentration profile has been used by several authors (Hosseini et al., 2010;Jafari et al., 2012;Magelli et al., 1991;Tahvildarian et al., 2011;West et al., 1999) to quantify the effect of reactor geometry, suspension properties and impeller revolution rate on the homogeneity of solid-liquid suspension. RSD is plotted against power consumption for one reactor geometry with different slurry properties in Figure 3. It can be seen that the power required to reach a certain value of RSD is increased with increase in solids concentration and particle size. Also a point of minimum RSD, beyond which the value of RSD increases with increase in agitation power, can be distinguished. Similar findings have been reported in the literature (Harrison et al., 2012;Hosseini et al., 2010). However, the minimum value of RSD that was reached approached zero, independent of impeller type and slurry properties. This is in 8

201 202 203 contrast with the results of Hosseini et al. (2010) who reported that a more homogeneous suspension can be attained depending on the impeller or the particle size and volume fraction of solids. 0,4 0,35 RSD [-] 0,3 0,25 0,2 0,15 200 g/l, 75-100um 400 g/l, 75-100um 200 g/l, 125-180um 400 g/l, 125-180um 0,1 0,05 204 0 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1 P/m [W/kg] 205 206 207 208 209 Figure 3 RSD vs. power consumption per unit mass for different slurries agitated with OKTOP3200 impeller. Exponential fit is provided for eye-guidance and is calculated only until the minimum value of RSD. Distribution of the solid phase can also be assessed by one-dimensional sedimentationdispersion model for a batch system in steady-state using Peclet-number (Pe) as an adjustable parameter (Montante et al., 2003): X z H Pe X = 1 exp ( Pe) exp Pe z H (3.2) Pe =, (3.3) 9

210 211 212 213 214 215 216 217 where z is the axial position [m] X is the mean solids volume fraction X is the solids volume fraction H is the height of the liquid batch [m] Us is the settling velocity of solid particles in stirred medium [m/s] De,p is the dispersion coefficient for the solid phase [m 2 /s] Pe is the Peclet number (dimensionless adjustable parameter) 218 219 220 221 222 223 224 225 226 227 228 229 230 231 232 233 Steady-state can be assumed for N Nps as verified by the EIT data and Pe was calculated from the experimental data for these agitation rates. Pe and RSD can be related analytically, and experimental values have been shown to correlate almost linearly by (Magelli et al., 1991). A linear relationship between Pe and RSD was established from our data as shown in Figure 4. The value of Pe decreases as homogeneity of the suspension increases but, unlike RSD, it does not have a minimum value at homogeneous suspension. Instead, it approaches zero as homogeneity increases and may yield negative values if solids concentration is higher at the top part of the vessel. Measured and fitted profiles for three impeller revolution rates are presented in Figure 5 where it can be seen that fitted Pe-number yields a negative value at 500 and homogeneous suspension was reached with lower N. Thus, the most homogeneous suspension can be estimated to be between the agitation rates at which the value of Pe changes from positive to negative. Values for agitation rate (Nh), power consumption (Ph) and cloud height (CHh) at Pe = 0 as presented later in the text were calculated by linear interpolation. The assumption of linearity is justified as the agitation rate was increased with intervals of 50 or less. It should be noted that sedimentation-dispersion model gives, by definition, monotonical vertical profiles and cannot accommodate local inhomogeneties as shown in Figure 5. 10

0,7 0,6 0,5 RSD [-] 0,4 0,3 0,2 0,1 0-0,5 0 0,5 1 1,5 2 2,5 234 235 Pe [-] Figure 4 RSD vs. Pe for all measurements, RSD = 0.245Pe for Pe > 0 z/h 1 0,9 0,8 0,7 0,6 0,5 0,4 0,3 0,2 0,1 250 Pe = 0.99 350 Pe = 0.56 500 Pe = -0.12 0 0,5 0,6 0,7 0,8 0,9 1 1,1 1,2 1,3 1,4 1,5 236 Measured X / X average Fitted 237 238 239 240 241 242 Figure 5 Dimensionless axial solid concentration profile and profile fitted with the equation (3.2). OKTOP3200 impeller, 4 baffles, dp = 75 100 μm, XV = 7.5 % 3.3 Comparison of Suspension Criteria Three different suspension criteria visually determined Njs as well as partial and homogeneous suspension from EIT data were used in this study. For comparison, the values of N for each 11

243 244 245 246 247 248 249 250 251 252 253 254 255 256 257 258 259 260 261 262 263 264 265 266 267 268 269 270 271 272 criterion are plotted against particle size for both impeller types and solids concentrations in Figure 6. Regression curves for power law equation = are provided for eyeguidance. Three particle size fractions were used in the measurements with OKTOP3200 hydrofoil impeller (Figure 6a). Nps increases with particle size and for the range used in this work, Nps can be related to dp with an exponent of 0.41 (Nps dp 0.41 ) The same is not true for Njs, which increases significantly from 50 75 to 75 100 µm but only slightly from 75 100 to 125 180 µm size fractions. Also the difference between Nps and Njs decreases with increasing particle size. The values of Nh are significantly higher than Njs or Nps for all particle sizes but the effect of particle size is similar as for partial suspension (Nh dp 0.41 ). Similar power law dependencies of N vs. particle size have been reported in the literature (Chudacek, 1986). However, the results presented here considering the power law dependence should be read with caution as only three fractions in a relatively narrow size range were tested and particle size distribution within the fractions is not known. The measurements with the 4PBT were made with two particle size fractions (Figure 6b). The results follow similar trends as for OKTOP3200 but the Njs is closer to Nh rather than Nps. Actually, for solids volume fraction of 47 % and particle size of 75 100 µm, Njs is higher than Nh. This further questions the applicability of just suspended criterion as the suspension of the last few particles depend highly on the specific flow pattern at the vessel bottom. The effect of solids concentration is similar for all suspension criteria and both impellers and it increases the required agitation rate. Impeller revolution rates at Nh and Njs are plotted against Nps for each measurement in Figure 7. It is interesting to note that there is a good linear correlation between agitation rates required for partial and homogeneous suspensions, the relationship being Nh = 2Nps, independent of the stirrer type. Njs is always higher than the stirrer speed for partial suspension but no clear correlation is found between Njs and Nps. The twofold increase in the agitation rate when moving from partial to homogeneous suspension results in a theoretical increase of power consumption by a factor of 8. The largest values of power consumption are encountered for the largest particle size fraction for which the volumetric power consumption is around 1000 W/m 3 at the homogeneous suspension for both impellers. It should be noted that typically the 12

273 274 275 276 277 278 279 280 281 282 volumetric power consumption decreases in scale-up from laboratory to industrial scale depending on the suspension criterion and system geometry (Chudacek, 1986;Montante et al., 2003). Thus the volumetric power consumption of 1000 W/m 3 for homogeneous suspension in the laboratory scale does not unambiguously mean similar power consumption in the large scale industrial processes. However, the discussion of scale-up is out of the scope of this paper and is not continued here. Significant increase in the power consumption when moving from Nps to Njs and Nh still suggests that the sufficient state of suspension should be optimized between partial and homogeneous suspension. The sufficient state is process specific and may be related to reaction kinetics in leaching or crystallization reactors or simply a task of providing a homogeneous material outflow from a continuous mixing tank. 13

650 600 550 500 450 N [] 400 350 300 250 200 283 150 50 75 100 125 150 175 d p [μm] Homogeneous, Xv=15% Homogeneous, Xv=7.5% Just suspended, Xv=15% Just suspended, Xv=7.5% Partially suspended, Xv=15% Partially suspended, Xv=7.5% 450 400 350 N [] 300 250 200 284 150 50 75 100 125 150 175 d p [μm] 14

285 286 Figure 6 Agitation rate vs. particle size for different suspension criteria and impellers. The arithmetic mean of the limiting particle sizes of each fraction is used as dp. a) OKTOP3200 b) 4BPT 700 600 N h = 2.0N ps R² = 0.9 500 N h or N js [] 400 300 200 Nh Njs Nps 287 288 289 290 291 292 293 294 295 296 297 298 299 300 100 100 150 200 250 300 350 N ps [] Figure 7 Nh and Njs vs. Nps for all measurements Two impeller types are compared in terms of power consumption in Figure 8 where the power per unit mass required for partial and homogeneous suspensions is plotted for both the impeller types and different slurry properties. This figure further illustrates the substantial increase in power consumption when moving from partial to homogeneous suspension. The power consumption of the hydrofoil impeller is less than the power consumption of the pitched blade impeller for all suspension states and slurry properties. Similar results have been reported by other authors (Hosseini et al., 2010;Tahvildarian et al., 2011). For the partial suspension criterion, the difference between the impellers is rather large as the hydrofoil impeller consumes only 56 72 % of the power required by the pitched blade impeller, depending on the particle size and solids fraction. Similar figures for homogeneous suspension fall between 73 94 %. Increase in the concentration of solids (XV) from 7.5 to 15 % makes the two impellers more even and the smallest difference between the impellers is at the higher solids concentration. 15

0,8 0,7 0,6 P/m tot [W/kg] 0,5 0,4 0,3 OKTOP3200 4PBT 7.5%, 75-100um 7.5%, 75-100um 15%, 75-100um 15%, 75-100um 7.5%, 125-180um 7.5%, 125-180um 15%, 125-180um 15%, 125-180um 0,2 0,1 301 0 Partial suspension Homogeneous suspension 302 303 304 305 306 307 308 309 310 311 Figure 8 Power consumption per total mass of slurry at Nps and Nh. As noted previously, behaviour of cloud height was different for agitation rates below and above Nps. This is illustrated in Figure 9 where dimensionless cloud height is plotted against N for two measurements and, clearly, the cloud height starts to increase monotonically only after Nps. Homogeneous suspension was reached at cloud heights > 0.9. A histogram of cloud height that was reached at partial and homogeneous suspension is plotted in Figure 10. Cloud height at Nps is more scattered between 0.63 and 0.77 with an average of 0.69 whereas cloud height at Nh is more sharply concentrated between 0.92 and 0.98 with an average of 0.96. This is quite close to the value of 0.95, which has been used by (Chudacek, 1986) to determine a homogeneous suspension. The scattering of cloud height at Nps can be expected as the partial suspension 16

312 313 314 315 316 317 criterion is based only on the changes of solid concentration at the lower parts of the vessel. Total solids concentration has an effect on cloud height at Nps as can be seen from Figure 10. With less solids to be suspended (XV = 7.5 %), Nps is reached with lower agitation rates, and cloud height remains lower when compared to higher solids concentration (XV = 15 %). In order to reach homogeneous suspension, however, solids have to be distributed throughout the vessel, and the cloud height has to be sufficient for this suspension criterion. 1 0,9 0,8 (dashed lines), dp = 75-100 µm (solid lines), dp = 125-180 µm Cloud Height [z / H] 0,7 0,6 0,5 0,4 0,3 318 0,2 0,1 0 N ps N h 0 100 200 300 400 500 600 700 N [] 319 320 Figure 9 Dimensionless cloud height vs. impeller revolution rate for two different particle size fractions agitated with OKTOP3200 impeller, XV = 7,5 %. 17

No. of measurements 9 8 7 6 5 4 3 2 1 0 Nh Nps, 7.5% Nps, 15% 0.63 0.65 0.67 0.69 0.71 0.73 0.75 0.77 0.79 0.81 0.83 0.85 0.87 0.89 0.91 0.93 0.95 0.97 0.99 More 321 322 Cloud Height [z / H] Figure 10 Histogram of cloud height at Nps and Njs for all measurements 323 324 325 326 327 328 329 330 331 332 333 334 335 336 337 338 339 340 341 4 Conclusions Suspension of solid particles in liquid was measured by electrical impedance tomography (EIT) and visual inspection. EIT data were used to determine two different suspension criteria, partial and homogeneous suspension. Partial suspension was defined to be the agitation rate at which the solids concentration at the lowest plane of electrodes reaches a maximum. It was also shown that this is the lowest agitation rate at which the average axial solids distribution, measured by EIT, reaches a steady state. It was also found from the visual measurements that cloud height began to increase monotonically with agitation only at agitation rates above Nps. Similar suspension criterion has previously been described by several authors. A significant increase in the agitation rate and power was still required in order to suspend the rest of the particles and reach the complete suspension criterion (Njs). There was no clear correlation between Nps and Njs which further questions the applicability of the complete suspension criterion to suspension of small particles and high solids concentrations. Even further increase in the impeller revolution rate was required to reach homogeneous suspension, which was determined from the EIT data, and a good correlation between Nps and Nh was established. Dimensionless cloud height at Nh was found to be almost equal to 0.95 which has previously been used to describe a homogeneous suspension. Outotec OKTOP3200 hydrofoil impeller reached all of the used suspension criteria with less power consumption compared to the 4-bladed pitched blade turbine. Electrical impedance tomography was proved 18

342 343 344 to be applicable to determine the level of suspension in a wide range of suspension criteria. Therefore, EIT can be used to optimize not only the geometry of the vessel and impeller but also the state of suspension for a specific process. 19

345 346 347 Nomenclature C is impeller off-bottom clearance [m] CH is cloud height [m] or [-] 348 349 350 351 352 D De,p dp H m is impeller diameter [m] is the dispersion coefficient for the solid phase [m 2 /s] is particle diameter [m] is liquid height [m] is mass [kg] 353 N is impeller revolution rate [s -1 ] 354 355 356 P T Us is power [W] is tank diameter [m] is the settling velocity of solid particles in stirred medium [m/s] 357 V is suspension volume [m 3 ] 358 359 X z is the solids concentration (see subscripts for details) is axial position [m] 360 361 362 363 Greek letters σ is conductivity [ms/cm] Subscripts js complete suspension 364 365 ps h partial suspension homogeneous suspension 366 ms/vtot mass of solids per total volume [g / l] 367 368 ms/ml V mass of solids per mass of liquid [kgsolids / kgliquid] solids volume fraction [m 3 solids / m 3 tot] 369 References 20

370 371 372 373 374 375 376 377 378 379 380 381 382 383 384 385 386 387 388 389 390 391 392 393 394 395 396 397 398 399 400 401 402 Angst, R., Kraume, M., 2006. Experimental investigations of stirred solid/liquid systems in three different scales: Particle distribution and power consumption, Chemical Engineering Science 61(9), 2864-2870. Atiemo-Obeng, V. A., Penney, W. R., Armenante, P., 2004. Solid-Liquid Mixing, in: Handbook of Industrial Mixing, John Wiley & Sons, Inc., pp. 543-584. Ayazi Shamlou, P., Koutsakos, E., 1989. Solids suspension and distribution in liquids under turbulent agitation, Chemical Engineering Science 44(3), 529-542. Barresi, A., Baldi, G., 1987. Solid dispersion in an agitated vessel, Chemical Engineering Science 42(12), 2949-2956. Bujalski, W., Takenaka, K., Paolini, S., Jahoda, M., Paglianti, A., Takahashi, K., Nienow, A. W., Etchells, A. W., 1999. Suspension and liquid homogenization in high solids concentration stirred chemical reactors, Chemical Engineering Research and Design 77(3), 241-247. Chudacek, M. W., 1986. Relationships between solids suspension criteria, mechanism of suspension, tank geometry, and scale-up parameters in stirred tanks, Industrial and Engineering Chemistry Fundamentals 25(3), 391-401. Fajner, D., Magelli, F., Nocentini, M., Pasquali, G., 1985. SOLIDS CONCENTRATION PROFILES IN A MECHANICALLY STIRRED AND STAGED COLUMN SLURRY REACTOR. Chemical Engineering Research and Design 63(4), 235-240. Guida, A., Nienow, A. W., Barigou, M., 2011. Mixing of dense binary suspensions: Multicomponent hydrodynamics and spatial phase distribution by PEPT, AIChE Journal 57(9), 2302-2315. Harrison, S. T. L., Stevenson, R., Cilliers, J. J., 2012. Assessing solids concentration homogeneity in Rushton-agitated slurry reactors using electrical resistance tomography (ERT), Chemical Engineering Science 71, 392-399. Heikkinen, L. M., Kourunen, J., Savolainen, T., Vauhkonen, P. J., Kaipio, J. P., Vauhkonen, M., 2006. Real time three-dimensional electrical impedance tomography applied in multiphase flow imaging, Measurement Science and Technology 17(8), 2083-2087. Hosseini, S., Patel, D., Ein-Mozaffari, F., Mehrvar, M., 2010. Study of solid liquid mixing in agitated tanks through electrical resistance tomography, Chemical Engineering Science 65(4), 1374-1384. Jafari, R., Tanguy, P. A., Chaouki, J., 2012. Experimental investigation on solid dispersion, power consumption and scale-up in moderate to dense solid liquid suspensions, Chemical Engineering Research and Design 90(2), 201-212. 403 404 405 Kraume, M., Zehner, P., 2001. Experience with experimental standards for measurements of various parameters in stirred tanks: A comparative test, Chemical Engineering Research and Design 79(8), 811-818. 21

406 407 408 409 410 411 412 413 414 415 416 417 418 419 420 421 422 423 424 425 426 427 428 429 430 431 432 433 434 435 436 437 438 439 440 Kraume, M., 1992. Mixing times in stirred suspensions, Chemical Engineering and Technology 15(5), 313-318. MacTaggart, R. S., Nasr-El-Din, H. A., Masliyah, J. H., 1993. Sample withdrawal from a slurry mixing tank, Chemical Engineering Science 48(5), 921-931. Magelli, F., Fajner, D., Nocentini, M., Pasquali, G., 1990. Solid distribution in vessels stirred with multiple impellers, Chemical Engineering Science 45(3), 615-625. Magelli, F., Fajner, D., Nocentini, M., Pasquali, G., Marisko, V., Ditl, P., 1991. Solids concentration distribution in slurry reactors stirred with multiple axial impellers, Chemical Engineering and Processing 29(1), 27-32. Micale, G., Grisafi, F., Brucato, A., 2002. Assessment of Particle Suspension Conditions in Stirred Vessels by Means of Pressure Gauge Technique, Chemical Engineering Research and Design 80(8), 893-902. Michelett, M., Nikiforaki, L., Lee, K. C., Yianneskis, M., 2003. Particle Concentration and Mixing Characteristics of Moderate-to-Dense Solid-Liquid Suspensions, Industrial and Engineering Chemistry Research 42(24), 6236-6249. Montante, G., Pinelli, D., Magelli, F., 2003. Scale-up criteria for the solids distribution in slurry reactors stirred with multiple impellers, Chemical Engineering Science 58(23 24), 5363-5372. Nienow, A. W., 1997. Chapter 16 - The suspension of solid particles, in: N Harnby A2M.F. Edwards and A.W. NienowA2 N Harnby,M.F.Edwards, A.W. Nienow (Eds), Mixing in the Process Industries. Oxford, Butterworth-Heinemann, pp. 364-393. Špidla, M., Sinevič, V., Jahoda, M., MacHoň, V., 2005. Solid particle distribution of moderately concentrated suspensions in a pilot plant stirred vessel, Chemical Engineering Journal 113(1), 73-82. Stevenson, R., Harrison, S. T. L., Mantle, M. D., Sederman, A. J., Moraczewski, T. L., Johns, M. L., 2010. Analysis of partial suspension in stirred mixing cells using both MRI and ERT, Chemical Engineering Science 65(4), 1385-1393. Tahvildarian, P., Ng, H., D'Amato, M., Drappel, S., Ein-Mozaffari, F., Upreti, S. R., 2011. Using electrical resistance tomography images to characterize the mixing of micron-sized polymeric particles in a slurry reactor, Chemical Engineering Journal 172(1), 517-525. West, R. M., Jia, X., Williams, R. A., 1999. Quantification of solid-liquid mixing using electrical resistance and positron emission tomography, Chemical Engineering Communications 175, 71-97. Zwietering, T. N., 1958. Suspending of solid particles in liquid by agitators, Chemical Engineering Science 8(3-4), 244-253. 22