Residence Time Distributions In A Stirred Tank

Submitted to Industrial & Engineering Chemistry Research 10/28/03

Residence Time Distributions in a Stirred Tank – Comparison of CFD predictions with Experiment

by

Byung-S. Choi, Bin Wan, Susan Philyaw, Kumar Dhanasekharan and Terry A. Ring

Department of Chemical Engineering

University of Utah

50 S. Central Campus Drive

Salt Lake City, UT 84112

And

Fluent, Inc.

10 Cavendish Court

Centerra Resource Park

Lebanon, NH 03766-1442

Abstract

Residence time distributions (RTD) are measured for a both a baffled and unbaffled ~1.4 L laboratory reactor with several intern pipes and a Rushton turbine operating at different flow rates and impeller rpm’s. The experimental results for the baffled tank are compared to computational fluid dynamics (cfd) predictions of the residence time distribution using k- turbulence model in Fluent. All the qualitative aspects of the predicted RTD’s are similar to those measured experimentally. The mean residence times as well as the variances of the residence time are accurately predicted by cfd when the errors of both the experiments and the predictions are considered.

Introduction

The continuous stirred tank is used ubiquitously in the chemical process industry for mixing, reactions and crystallizations. The mixing in a continuous stirred tank is often not ideal. The residence time distribution (RTD) is one of the ways to characterize the non-ideal mixing in the tank. Comparison of the measured RTD with that of an ideal reactor allows the process engineer to diagnose the ills of the tank and mixer design. The engineer can then use an appropriate mixing model for the tank in combination with the kinetics of the reaction to be performed in the tank to develop an appropriate model for the reactor .

This paper measures the RTD of a laboratory reactor both with and without baffles and makes comparisons of these measurements with predictions for the RTD using computational fluid dynamics (cfd) with a k- turbulence model coupled with a dynamic two-species, fluid and tracer, mass balance operating with a step change of the concentration of tracer in the feed.

Experimental

The geometry of the ~1.4 L laboratory stirred tank reactor is shown in Figure 1. It has four baffles of the conventional thickness in contact with the wall of the tank, a Rushton turbine and three internal pipes, two feed ports and a thermal well protruding into the reactor from its top. One of the feed tubes dead ends at the approximate height of the impeller and the other is bent to feed directly below the impeller. Also protruding ever so slightly into the top of the liquid are a pH probe, conductivity probe, thermocouple, potassium specific ion electrode and level indicator. The flow of reactor output flows directly into a flow cell of a uV-Vis spectrometer operated at a fixed wavelength. All of these instruments as well as the feed pump, product pump, the jacket feed temperature, thermal well temperature and the rpm and torque on the stirrer are connected to an OPTO-22 data acquisition and control system collecting data at time intervals of 1 s. The reactor control system has the capability of controlling the feed source and reactor temperature to ±0.25 oC, the feed and product flow rate to ±0.5 ml/min, liquid level to ±3.9 mm and mixing speed to ±3 rpm.

The ratio of liquid level to the tank diameter (L/D) of the vessel in Figure 1 is 1.27 that is within the general range of 1.0 to 1.5 for most industrial stirred tank precipitators , . To reduce the energy input to the system while maintaining mixing uniformity, a standard baffle design was used consisting of four flat vertical plates, radially-directed (i.e., normal to the vessel wall), spaced at 90o around the vessel periphery running the length of the vessel’s straight side. Standard baffle widths are between 1/10 and 1/12 of the vessel diameter (T/10 or T/12), see Table 1 for details. The gaps with the vessel wall and base are left to allow the flow to clear the baffles. Recommended gaps are equal to 1/72 of the vessel diameter (T/72) between the baffles and the vessel wall, and 1/4 to one full baffle width between the bottom of the baffles and the vessel base. More of the detailed baffling information could be found in Kevin, et al. . Stirring was achieved by a six-bladed Rushton turbine. The dimensions of the turbine are also given in Table 1.

Peristaltic pumps whose rpm is controlled by an Opto 22TM control system establish the feeding and removal of product solution from the tank. Flow rate was obtained by the careful and repeated calibration of the speed of pump and tube size to ensure the desired feed and withdrawal rates as well as a constant residence time. Also the Opto 22 computer measures the on-line sensor quantities; temperature, pH, absorbance and conductivity as well as potassium ion concentration. All of these measurements were used to monitor the concentration of the tracer inside and exiting the reactor. The calibration for all of these systems is done before each run to assure measurement accuracy.

Measurement of the RTD

The RTD is determined experimentally by injecting a 10 ml volume of inert multi-component chemical tracer, a hot solution of 0.1 gm/L methyl blue dye, 50 gm/L NaCl, 20 gm/L KCl and 3.6 gm/L HCl with water, into the tank at time zero. In all experiments, the feed tube is the bent one that feeds just below the impeller. On-line analyzers detect each of the species in the tracer; blue dye with the aid of video camera and uv-vis spectrometer, temperature with a thermocouple, salt with conductivity, and concentration with pH meter were measured simultaneously with various conditions such as different flow rates and mixer rpm. Great care was used in synchronizing the pulse input with the initiation of data accumulation for RTD analysis and to calibrate the pumps to assure that the reactor space-time [=Vtank/Q] was accurately measured. A listing of all the experimental conditions used to measure RTD’s is given in Table 2a, for the without baffle experiments and Table 2b for the with baffles experiments. For all of these experiments data was taken at 1 s intervals. Figure 2 and 3 illustrate good mixing at 300 rpm and bad mixing at 0 rpm for the tank without baffles as measured by conductivity, pH and temperature. The uv-vis spectrometer data and K+ ion data is not shown in these figures, however, it is similar to that for the other curves presented in these figures. All of these curves show a fast increase at an early time followed by an exponential decrease as expected for a continuous stirred tank. The delay of the increase from time zero and the roughness of the increases clearly indicate parasitic mixing behavior as compared to the ideal mixing curve since it should increase abruptly in an instantaneous rise at time zero and decay exponentially with time thereafter. The RTD is obtained from these data by normalization in the typical manner .

(3.1)

where C(t) represents the concentration (or temperature) trace, e.g. Figures 2 and 3. An example of the RTD is plotted in Figure 4. Even for this good mixing case there are deviations from ideal mixing at short residence times where the initial rise is not immediate and is not a smooth curve. This figure also contains a plot of the ideal RTD for the stirred tank for comparison purposes. The mean residence time ( ) was calculated by integrating the RTD as follows

. (3.2)

The variance, or square of the standard deviation of the RTD is calculated using:

(3.3)

The magnitude of this 2nd moment is an indication of the spread of the RTD. In Figure 5 the mean resident time obtained from the experimental data is plotted as a function of mixer rpm for various feed flow rates for the tank without baffles. Here we see that the mean residence time decreases with increasing rpm until a constant value is reached. This constant value is approximately Vtank/Q, the space-time for the reactor, where Vtank is the reactor volume and Q is the volumetric flow rate. The error in the calculation of the mean residence time, tm, is ~8% of Vtank/Q for all experiments and was determined by experiments done in duplicate and some in triplicate. In Figure 6 the variance of the RTD divided by the space-time is plotted as a function of mixer rpm for various feed flow rates for the tank without baffles. The error in the variance of the residence time divided by the mean residence time is ~12% at all rpm’s and is larger than that of the mean residence time because two integrals with their inherent errors are involved in the variance divided by mean residence time calculation. For an ideal reactor the value of should be 1.0, which is observed, within the experimental error, at higher impeller rpm’s. With the Figure 5 and 6 one can see that mixer speed of 100 rpm was enough to approach perfect mixing for the unbaffled tank. With baffles, the results are shown in Figure 7 and 8. With baffles, the results are similar to those without baffles, however, the approach to ideal reactor behavior takes place at ~60 rpm as measured by , which is lower than the tank without baffles.

Cfd Predictions

A model of the stirred tank shown in Figure 1 was constructed in Fluent’s grid generation algorithm GAMBIT using a rotating mesh in the region

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