Elsevier

Chemical Engineering Science

Volume 60, Issues 8–9, April–May 2005, Pages 2333-2339
Chemical Engineering Science

Intensifying micromixing in a semi-batch reactor using a Rushton turbine

https://doi.org/10.1016/j.ces.2004.10.041Get rights and content

Abstract

The ‘iodide–iodate’ reaction scheme has been used to ascertain the effectiveness of micromixing in a semi-batch reactor when feeding with pipes rotating and discharging continuously into the region of highest local specific energy dissipation rate, εT. The results are compared with those obtained using a fixed pipe at the equivalent position and at other positions including near the top surface, the most convenient position industrially. The results show significant intensification, i.e., a seven-fold reduction in ‘waste product’, between the most convenient fixed feed pipe position and the rotating pipes, even at the modest specific power input of 1.0W/kg. This mode of addition also ensures that feeding is always into a constant value of εT, whereas with a static pipe close to the impeller the reactants are being fed in a region where εT varies cyclically. This difference in the εT values experienced by the two modes of addition poses problems for previous models of micromixing in the literature linking selectivity to local specific energy dissipation rates.

Introduction

Mixing at the molecular scale (micromixing) is important in processes such as polymerization, precipitation and in determining the selectivity of competing fast chemical reactions. Therefore, a lot of work in the last few years has been done on micromixing, developing experimental methods (Baldyga and Bourne, 1999, David et al., 1985, Fournier et al., 1996) to characterize it. During this time, experimental techniques like laser Doppler velocimetry and particle image velocimetry (PIV) have significantly improved, giving more reliable values of εT, the local specific energy dissipation rate. Knowledge of the values of this parameter is important as high levels enhance micromixing.

Rushton turbines (RTs) have been extensively studied and the flow patterns and the turbulence properties, including the spatial distribution of εT, for this impeller are relatively well known. Nienow and Wisdom (1974) and Van’t Riet and Smith (1975) both reported the presence of a trailing vortex pair behind each blade where very high rotational shear rates were found and the latter tried to identify the position of their axis using flow followers combined with a photographic technique. Since then, many other authors (Lee and Yianneskis, 1998, Sharp and Adrian, 2001, Stoots and Calabrese, 1995, Yianneskis and Whitelaw, 1993, Yianneskis et al., 1987, for example) have studied the flow structure close to the RT with laser based methods giving a more precise indication of the position of the vortex axis (Fig. 1) and the value of other turbulence parameters. Takahashi and Nienow (1992) used the vortex cavity structure produced at very low gas flow rates to show the vortex axis position and found similar results. Lee and Yianneskis (1998) found that the maximum values of turbulent kinetic energy in the vessel are present in the vortex at a position 1530 behind the Rushton blades.

Estimation of the value of εT for RTs has been made by a number of authors. Cutter (1966) was the first to use a tracer/photographic technique and latterly laser-based techniques have been used, e.g., Zhou and Kresta (1996) and Schäfer (2001). All concluded that most of the energy was dissipated in the impeller discharge stream. For example, Wu and Patterson (1989) found that 60% of the energy transmitted to the tank from the impeller was dissipated in the impeller and the impeller discharge stream. Other authors have tried to measure the maximum local εT value; for example, Cutter (1966) based on his streak photography whilst Wu and Patterson (1989) and Schäfer (2001) and many of the others listed above used a laser-based technique. Overall, agreement between different workers has been poor and values of (εT)max/ε¯T=φmax from 20 to 140 have been reported by Zhou and Kresta (1996) as the impeller, D, to tank diameter, T, ratio was reduced from 12 to 14. This range of φmax encompasses the values found by all the workers. This variation in the values reported in the literature arises not only from the different D/T ratios utilised but also from the assumptions and numerical manipulations required to obtain εT from the raw, randomly fluctuating velocity data. It is also necessary to consider the complexity associated with the presence of a regular fluctuating component due to the blade passage and whether 360 ensemble data or angle resolved data should be used. In addition, close to the impeller, all parameters vary very significantly, even for very small changes in position.

Predictions of εT values have also been made by computational fluid dynamics. Typically kε models have been used. Again, these studies show the highest values in the impeller discharge stream. More recently, estimates of φmax have been made for the trailing vortex using the sliding mesh technique, e.g. Ng and Yianneskis (2000) giving φmax40 and Bujalski (2003) giving a φmax25. However, it should also be recognised that generally, when local εT values based on the kε model have been integrated over the volume of the tank to give ε¯T, very low values of ε¯T compared to the experimental ones have been found (Bujalski, 2003).

In our previous paper (Assirelli et al., 2002), we used the ideas summarized above to pick a precise fixed feed point for optimizing micromixing in a semi-batch reactor. Thus, the feed was introduced through a fixed pipe positioned at 1.04 times the radius of the RT and at the top of the blade, estimated from the literature to be the location of φmax. The consecutive feeding, iodide–iodate technique (Guichardon and Falk, 2000) was used to assess the effectiveness of this feed position for the optimization of micromixing. It was found that this position minimized the amount of unwanted material compared to that produced at three other fixed positions further away from the impeller. For example, for a particular set of conditions, it could be reduced from 20% when feeding near the top of the vessel to 5% (Assirelli et al., 2002). A similar result confirming the effectiveness of this feed position for a semi-batch reactor was found by Schäfer (2001). He also estimated φmax50 in good agreement with the value that he obtained by LDA.

Given this result, it was decided to see if even more efficient micromixing could be achieved by feeding into the region of highest εT continuously. In other words, in the previous work, though the feed was continuous, it was only intermittently into this region, depending at any instant on the position of the feed pipe relative to the precise position of a single impeller blade. Thus, only six times per revolution of the impeller would the feed be into the region of maximum εT and then only briefly. However, if the feed point rotated with the impeller, feed could be maintained 100% of the time into the point of maximum εT. This paper reports the results from developing such a feed method.

Section snippets

Experimental rig

The experimental work followed very closely to that previously reported in Assirelli et al. (2002). Therefore, only a brief description will be given here. Fig. 2 shows the 0.29 m diameter (T), fully baffled cylindrical Perspex tank and the position of all the static injection points investigated by Assirelli et al. (2002). The precise position of the tip of the feed pipe is shown in Table 1 with the direction of injection pointing towards the shaft of the impeller. Tests undertaken with a

Experimental technique and data treatment

Reactions were undertaken in the semi-batch mode using the successive iodide–iodate method (Fournier et al., 1996)H2BO3-+H+H3BO3,5I-+IO3-+6H+3I2+3H2O,I2+I-I3-.

Reaction (1) involves an instantaneous acid–base neutralisation to give the desired product and reaction (2) is the Dushman reaction giving the undesired product, here iodine. Reaction (3) is the further reaction between iodine formed from reaction (2) with iodide to form triiodide. The reactants’ concentration used were chosen

The power number

The power number, Po, was measured by an air-bearing technique and found to be 4.3 for both the RT and the MRT. The mean specific energy dissipation rates, ε¯T, where ε¯T=P/ρV for each rotational speed investigated, are given in Table 4.

Comparison of results for one static feed pipe with one rotating feed pipe

Fig. 5 compares the segregation index, XS, for the four static feed positions investigated previously (Assirelli et al., 2002) and for the injection with the MRT for four rotational speeds, N. For all these conditions with the static pipe, the previous work (

Conclusion

A MRT has been conceived to intensify micromixing and the iodide–iodate technique (Fournier et al., 1996) has been employed in this work to verify the effectiveness of the novel system. Injection of acid in various positions inside the tank using a static pipe led to a decrease of the segregation index, XS, in going from a position far away from the impeller (position 1 and 2) to very close to it where the trailing vortex of the RT is generated (position 4). Thus, positioning the static

Notations

Bbaffles width, m
Cimpeller clearance off the bottom, m
dppipe inner diameter, m
Dimpeller diameter, m
Hliquid height, m
Nstirring speed, s-1
Popower number, dimensionless
rradial coordinate of feed point, m
Rradial distance, m
Ttank diameter, m
Vliquid volume, m3
Wblade width, m
xidisk and blades thickness, m
XSsegregation index, dimensionless
Yactual yield of undesired product, dimensionless
YSTmaximum yield of undesired product, dimensionless
zaxial position of feed point, m
Zaxial coordinate, m

Greek letters

α

Acknowledgements

One of us (MA) acknowledges financial support for this project by Huntsman Polyurethanes Europe BVBA (Belgium) and the School of Chemical Engineering in Birmingham (UK). The authors also thank Bob Sharpe and other workshop staff for their technical assistance, especially with the fabrication of the MRT impeller.

References (24)

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