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Experimental study of the bubble size distribution in a pseudo-2D bubble column Y.M. Lau, K. Thiruvalluvan Sujatha, M. Gaeini, N.G. Deen, J.A.M. Kuipers

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S0009-2509(13)00355-2 http://dx.doi.org/10.1016/j.ces.2013.05.024 CES11068

Chemical Engineering Science

Received date: 20 December 2012 Revised date: 8 May 2013 Accepted date: 14 May 2013 Cite this article as: Y.M. Lau, K. Thiruvalluvan Sujatha, M. Gaeini, N.G. Deen, J. A.M. Kuipers, Experimental study of the bubble size distribution in a pseudo2D bubble column, Chemical Engineering Science, http://dx.doi.org/10.1016/j. ces.2013.05.024 This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting galley proof before it is published in its final citable form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

Experimental study of the bubble size distribution in a pseudo-2D bubble column

Y.M. Lau, K. Thiruvalluvan Sujatha, M. Gaeini, N.G. Deen , J.A.M. Kuipers
Multiphase Reactors Group, Department of Chemical Engineering and Chemistry, Eindhoven University of Technology, The Netherlands P.O.Box 513, 5600MB Eindhoven

Abstract This work presents an experimental study of the bubble size distribution of a bubbly ow using digital image analysis (DIA). In order to facilitate the image measurement technique a pseudo-2D bubble column is chosen for the experiments. To obtain well-dened inlet conditions a gas sparger, consisting of 20 needles, is used. By employing DIA, the bubble size distribution (BSD) has been measured for a range of supercial gas velocities. The resulting BSDs are expressed in terms of a probability density function (PDF). For low supercial gas velocities of 5 and 10 mm/s the PDF has a unimodal shape, while for higher supercial gas velocities of 15 and 20 mm/s the PDF has a bimodal shape. The eects of coalescence and break-up of bubbles are visible by evaluating the changes of the resulting BSDs for increasing supercial gas velocity. A comparison of gas hold-ups is made between the calculated BSD and the liquid expansion height. This comparison shows how well the BSD obtained with DIA describes the actual gas hold-up in the

Corresponding author: N.G.Deen@tue.nl

Preprint submitted to Chemical Engineering Science

May 17, 2013

column. Keywords: Digital Image Analysis, Gas-liquid ow, Bubble columns, Bubble size distribution, Gas hold-up 1. Introduction Gas-liquid bubble column reactors are widely used in many industrial applications, e.g. Fischer-Tropsch process for hydrocarbon synthesis, hydrogenation of unsaturated oil, coal liquefaction, fermentation and waste water treatment. One of the important factors in the design of mass transfer in such reactors is the gas-liquid interfacial area, which depends on the bubble size distribution (BSD). In general, the gas-liquid interfacial area is a function of geometrical conguration, operating parameters, physical and chemical properties of both phases. To optimize bubble column processes, it is essential to know the BSD in the particular system at dierent operating conditions. However it is very dicult to measure the BSD in an industrial bubble column. Therefore, dierent types of laboratory-scale bubble columns have been employed to study the bubble size. Br oder and Sommerfeld (2007) measured bubble sizes in a lab-scale 3D column with an average gas volume fraction between 0.5 5.0 % and a mean bubble diameter ranging between 2 4 mm. Mena et al. (2005) measured the bubble size distribution in a mass transfer system in a lab-scale 3D column at a low supercial gas velocity of 2.8 mm/s. Majumder et al. (2006) reported the bubble size in a modied bubble column reactor at supercial liquid velocities of 70.7-141.4 mm/s and supercial gas velocities of 1.7-13.58 mm/s. Sch afer et al. (2002) discussed the inuence of operating conditions and physical properties of the gas and

liquid phases on the initial and stable bubble sizes in a bubble column reactor operating in the homogeneous regime. Other than these mentioned studies, there are many more (Polli et al. (2002), Mandal et al. (2005), Wongsuchoto et al. (2003), Montante et al. (2008), Diaz et al. (2008), Bordel et al. (2006), Lage and Esposito (1999), etc.). Most of these experimental studies on the bubble size distribution are performed using Digital Image Analysis (DIA) for low void fraction bubbly ow or only near-wall measurements for high void fraction bubbly ow. DIA is a non-intrusive technique, which can measure irregular-shaped bubbles accurately with a wide range of bubble sizes (Honkanen et al. (2005)). Non-intrusive techniques are preferred above intrusive ones, as these do not disturb the ow. Recognizing individual bubbles from digital images is tedious. This is because even at low void fraction ( 1 %) a large number of bubbles is overlapping (40 %) (Lecuona et al. (2000); Rodriguez-Rodriguez et al. (2003)). The objective of this work is to investigate the BSD in a pseudo-2D bubble column with the use of DIA. The image analysis incorporates the watershed transformation by Meyer (1994) to separate overlapping bubbles. Measurements are performed for bubbly ows up to the limit where bubble detection is no longer possible due to the high void fraction. The main subject of this work is to investigate the eect of the supercial gas velocity and the evolution of the BSD along the height of the column.

2. Experimental set-up and technique 2.1. Pseudo-2D bubble column Bubble size distributions are measured in a pseudo-2D bubble column. Air and distilled water are used as the gas and the liquid phase respectively. A schematic representation of the column and its measurement zones are illustrated in Figure 1. The measurement zones are maintained for dierent initial liquid heights (H0 ). The column is made of glass with dimensions of 0.20 0.03 1.0 m (W D H ). It is equipped with a needle sparger, which is used to obtain well-dened inlet conditions at the gas distributor. The sparger consists of a row of 20 needles and is aligned in the centre of the bottom-plate of the column. The needles have an inner diameter of 1 mm and an outer diameter of 1.3 mm. The needles extend 10 mm above the bottom plate and are spaced with a centre-to-centre distance of 10 mm. The gas ow rate is controlled with mass ow controllers. For the BSD measurements, series of 5000 images with a frequency of 50 Hz are obtained using a highspeed CMOS camera (Lavision, HighSpeedStar 3G). The focal length of the lens is 50 mm. The camera is positioned at a distance of 1.50 m in front of the pseudo-2D column and the column is illuminated from the back. The acquired images are gray scale images with a resolution of 1024 1024 pixels, yielding a spatial resolution of 0.18 mm. The eld of depth is 0.14 m, which is larger than the column depth. 2.2. Digital Image Analysis The bubble properties that can be obtained from an image are the projected area and shape. Subsequently, from these quantities the centroids and 4

top 0.183m

0.583m

measurement windows

middle

0.400m 0.383m needle sparger

column height 0.6m 0.2m column width 0.200m 0.188m

column depth 0.03m

bottom

water 0.005m needle sparger air

Figure 1: Schematic overview of the pseudo-2D bubble column set-up with the measurement windows (top, bottom and middle).

equivalent diameter can be calculated. To acquire these values, a number of operations are performed upon the images (see overview in Figure 2). Starting with the obtained image, the background is removed using local area thresholding, where the image is divided in blocks, each of which is independently thresholded by employing the Otsu (1979) lter. Subsequently, a global threshold is applied to create a binary image, separating the bubbles from the background. To this end, an appropriate global threshold value is chosen from the histogram of the image gray scales. After these lters have been applied, the detected objects are divided into solitary bubbles and overlapping/clustering bubbles on the basis of the roundness. The roundness is determined as: S Ro = 4A 5 (1)

with S the surface perimeter and A the area. The applied criteria to distinguish isolated single bubbles is Ro < 1 1.5, which is determined by trial and error on an initial set of images. The resulting two images are segmented independently and subsequently combined to yield an overall image with solitary and separated overlapping/clustering bubbles. The image with the solitary bubbles is segmented by labelling the solitary areas, and the image with the overlapping/clustering bubbles is segmented using a watershed transform by Meyer (1994). Finally, the area of pixels of each bubble object of both images is counted and converted from pixel to metric values using the magnication of the image. From the measured area, the equivalent diameter is calculated as follows: de = 4A

(2)

This image measurement technique is described in detail in the paper of Lau et al. (2013). Examples of the detected bubbles in the pseudo-2D bubble column are shown in Figure 3. Note that the smallest bubble diameter that can be detected in the images is equal to 0.9 mm, which corresponds with 5 pixels. The measured BSDs are expressed in the form of a number-based Probability Density Function (PDF). 3. Results and discussion 3.1. Visual description Measurements are performed for dierent initial liquid heights (0.5, 0.6 and 0.7 m) with supercial gas velocities ranging from 5 to 30 mm/s for an air-water system. The measurement zones (top, middle and bottom) are shown in Figure 1. Samples of the obtained camera images with an initial 6

original

ltered

solitary

overlap/cluster

lter

separate

watershed result

segment & combine

Figure 2: Image processing sequences to determine the bubble size distribution.

(a) vsup = 5 mm/s

(b) vsup = 15 mm/s

(c) vsup = 25 mm/s

Figure 3: Example images of detected bubbles at various supercial gas velocities ranging from 5 mm/s to 25 mm/s.

liquid height of 0.6 m are shown in Figures 4 and 5. These are merely snapshots of the measured time series and cannot visually illustrate the bubbly ow dynamics. By visual analysis of the time series, the following is observed. At low supercial gas velocity of 5 mm/s (see Figures 4a, 4d and 4g), the bubbles appear to be similar in size at the dierent regions of the column. The bubbles rise very slowly upward in a homogeneous fashion. For a super-

cial gas velocity of 10 mm/s (see Figures 4b, 4e and 4h), coalescence and break-up of bubbles start to play a role. This results in a wider BSD than the BSD observed with a supercial gas velocity of 5 mm/s. Occasionally, there are some regions where the bubbles rise faster. For a supercial gas velocity of 15 mm/s (see Figures 4c, 4f and 4i), a bubble plume becomes more evident and bubbles rise faster in the column. A plume is a dynamic region within the bubble column, where the bubbles rise with a higher velocity. Bubbles in this dynamic region are larger due to coalescence of bubbles. The smaller bubbles accumulate close to the side walls and are dragged down by the down-ow of the liquid. A wide bubble size distribution in the column is obtained and small vortical structures are formed close to the side wall regions. At 20 mm/s (see Figures 5a, 5d and 5g), two bubble regions (plumes) with high bubble rise velocity are observed and down-ow of smaller bubbles at the side walls is clearly visible. Some small vortices also occur at the region between the plumes. At even higher supercial gas velocities of 25 mm/s (see Figures 5b, 5e and 5h) and 30 mm/s (see Figures 5c, 5f and 5i), a large number of small bubbles is formed due to intense bubble break-up. The bubbly ow is very chaotic, which makes visual observation very dicult.

(a) top, vsup = 5 mm/s (b) top, vsup = 10 mm/s (c) top, vsup = 15 mm/s

(d) vsup = 5 mm/s

middle, (e) vsup = 10 mm/s

middle, (f)

middle,

vsup

15 mm/s

(g) vsup = 5 mm/s

bottom, (h)

bottom,

vsup

= (i) vsup = 15 mm/s

bottom,

10 mm/s

Figure 4: High-speed camera images of the bubbly ow for the dierent measurement zones (top, middle and bottom) in the pseudo-2D bubble column for supercial gas velocities ranging from 5 to 15 mm/s and an initial liquid height of H0 = 0.6 m.

(a) top, vsup = 20 mm/s (b) top, vsup = 25 mm/s (c) top, vsup = 30 mm/s

(d) vsup = 20 mm/s

middle, (e) vsup = 25 mm/s

middle, (f)

middle,

vsup

30 mm/s

(g)

bottom,

vsup

= (h)

bottom,

vsup

= (i) vsup = 30 mm/s

bottom,

20 mm/s

25 mm/s

Figure 5: High-speed camera images of the bubbly ow for the dierent measurement zones (top, middle and bottom) in the pseudo-2D bubble column for supercial gas velocities ranging from 20 to 30 mm/s and an initial liquid height of H0 = 0.6 m.

10

3.2. Bubble velocities Bubble velocity measurements have been performed via bubble image velocimetry (Deen (2001)) for the supercial gas velocity range from 5 to 30 mm/s with an initial liquid height H0 = 0.6 m. Series of 5000 image pairs of the entire column with a frequency of 50 Hz are obtained for bubble velocity calculations. The average vertical bubble velocities across the width of the pseudo-2D bubble column at heights of 0.15, 0.30 and 0.45 m are given in Figure 6. This gure shows for a low supercial gas velocity of 5 mm/s an uniform up-ow of the rising bubbles. By increasing the supercial gas velocity, bubble down-ow regions near the side walls and a bubble up-ow region in the centre across the width of the bubble column are developed.

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0.35

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bubble velocity [m/s]

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sup

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0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

0.05

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0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

0.1 0

0.1 0

x/D

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(a) H = 0.15 m
0.35

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0.2

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sup

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0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

0.1 0

x/D

(c) H = 0.45 m Figure 6: Average vertical bubble velocities across the width of the pseudo-2D bubble column at 0.15, 0.30 and 0.45 m column heights for an initial liquid height of H0 = 0.6 m and dierent supercial gas velocities.

12

3.3. Integral gas hold-up To illustrate how well the BSD obtained with DIA describes the actual gas hold-up in the column, the integral gas hold-up is calculated on basis of the measured bubble sizes and is compared with the integral gas hold-up calculated using the liquid expansion height. Using the measured bubble
BSD sizes, the gas hold-up (g ) is calculated as follows from the DIA data: N BSD g =

i=1

d3 ) ( 6 i (3)

Vwindow

Here, Vwindow is dened as the volume of the measurement zone minus the border volumes, where bubbles crossing/touching the borders are not taken into account in the detection algorithm (borderkill). With a length of the mean bubble diameter db from each side of the height H and width W of the measurement zone and the depth D, Vwindow (see Figure 7) is calculated as follows: Vwindow = (W 2db ) (H 2db ) D (4)

H For the actual gas hold-up (g ) in the bubble column, the expansion of the

liquid height in the column is used:

H g =

Hf H0 Hf

(5)

where Hf is the height of aerated liquid. Figure 8 shows the comparison of the gas hold-up determined by DIA/BSD and liquid height expansion. On increasing the supercial gas velocity, the gas hold-up in the column increases. Increase of the initial liquid height in the column has no signicant eect on the gas hold-up. At low superH BSD . This is seems to be larger than g cial gas velocity of 5 mm/s, g

13

width

db measurement window

measurement window minus border volumes height

Vwindow
db column wall column wall

db

db

Figure 7: Schematic representation of Vwindow for the calculation of the gas hold-up.

because of the Vwindow for which too much border volumes are subtracted. In comparison with higher supercial gas velocities, for 5 mm/s there are only a small number of bubbles crossing/touching the borders. This results in an underestimation of the actual liquid volume, which in turn results in an overpredicted integral gas hold-up. In spite of the imaging errors (noise and oversegmentation) introduced by the images, DIA/BSD is reasonably accurate at lower supercial gas velocities up till 20 mm/s, but at higher velocities the error becomes very large. At high supercial gas velocities, the presence of undetected small bubbles as shown in Figure 5 will contribute largely to the gas hold-up error. Therefore the BSDs obtained at supercial gas velocities exceeding 20 mm/s are omitted in this work.

14

12

12

12

BSD height expansion

10 10

BSD height expansion

10

BSD height expansion

[%]

[%]

[%]
g
0 0.5 1 1.5 2 2.5 3 3.5

g
4

0.5

vsup [c m/s]

1.5

2.5

3.5

vsup [c m/s]

0.5

vsup [c m/s]

1.5

2.5

3.5

(a) H0 = 0.5 m

(b) H0 = 0.6 m

(c) H0 = 0.7 m

Figure 8: Eect of the supercial gas velocity on the gas hold-up with dierent initial liquid heights.

3.4. Bubble size distribution The PDFs of the bubble size distribution for dierent initial liquid heights are illustrated in Figures 9 and 10. It can be seen that for all three initial liquid heights the trends are the same and the initial size distribution at the bottom region of the column prevails at the upper regions. It appears that there exists an equilibrium between bubble coalescence and break-up along the height of the column, and that this equilibrium is solely determined by the gas supercial gas velocity and independent of the initial liquid height. To illustrate the eect of the supercial gas velocity on the BSD, the PDF of the middle region of the column is plotted in Figure 11 for an initial liquid height of H0 = 0.6 m. Other initial heights show similar trends and are not shown here. At a low supercial gas velocity of 5 mm/s, the bubbles enter the bottom section of the column with a mean diameter of approximately 4 mm, which is retained throughout the higher sections (see Figure 9a). For higher initial liquid heights (see Figures 9b and 9c), the height of the peak in the PDF becomes sharper with the height of the measurement zones. The 15

dierences can be explained by the location of the top measurement zone, as for an initial liquid height of 0.5 m, the gas-liquid mixture only lls half of the measurement section, causing exit eects on the PDF, while for the other liquid heights the free surface area of the water is well above in the top section. This deviation is observed for all measured supercial gas velocities. Similar trends are observed for a supercial gas velocity of 10 mm/s for all three initial liquid heights (see Figures 9d, 9e and 9f), but with a wider bubble size distribution and a single peak at 5 mm. Coalescence and breakup of bubbles are starting to play a role and it seems that its equilibrium is almost reached in the bottom section, since the shape does not change much throughout the middle and top sections. At a supercial gas velocity of 15 mm/s (see Figures 10a, 10b and 10c) a bimodal bubble size distribution is observed with a small peak at 2.5 mm and a large peak at 5 mm. In the bottom section, the PDF is a non-bimodal wide distribution, developing into a bimodal distribution in the middle and top sections due to coalescence. Increasing the supercial gas velocity to 20 mm/s leads to similar eects, but also to more break-up (small peak at approximately 5 mm and a large peak at 2.5 mm).At 15 and 20 mm/s, the equilibrium between coalescence and breakup is not obtained in the bottom section, but still develops throughout the column. From these reported BSDs, it seems that the initial liquid heights of 0.5, 0.6 and 0.7 m has almost no eect on the resulting BSDs. The calculated number mean bubble diameter , the standard deviation and the Sauter mean diameter d32 are listed in Table 1. It shows that with the increase of supercial gas velocity, increases up till a supercial gas velocity of 20 mm/s, while and d32 both keep increasing.

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0.35

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diameter [mm]

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(a)

H0

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&(b)

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&(c)

H0

0.7

&

vsup = 5 mm/s
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vsup = 5 mm/s
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diameter [mm]

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diameter [mm]

(d) H0 = 0.5 m & vsup =(e) H0 = 0.6 m & vsup =(f) H0 = 0.7 m & vsup = 10 mm/s 10 mm/s 10 mm/s

Figure 9: Bubble size distribution for the supercial gas velocities of 5 and 10 mm/s with initial liquid heights (H0 ) of 0.5, 0.6 and 0.7 m.

17

0.15

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0.15

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diameter [mm]

(d) H0 = 0.5 m & vsup =(e) H0 = 0.6 m & vsup =(f) H0 = 0.7 m & vsup = 20 mm/s 20 mm/s 20 mm/s

Figure 10: Bubble size distribution for the supercial gas velocities of 10 and 20 mm/s with initial liquid heights (H0 ) of 0.5, 0.6 and 0.7 m.

18

vsup = 5 mm/s
0.3

v v v

sup sup sup

= 10 mm/s = 15 mm/s = 20 mm/s

0.25

PDF []

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diameter [mm]
Figure 11: Evolution of the bubble size distribution for increasing supercial gas velocity with an initial liquid height (H0 ) of 0.6 m.

4. Conclusions In this work a novel digital image analysis (DIA) technique is used to measure bubble size distributions (BSDs) in a pseudo-2D bubble column. From the resulting BSDs, it can be seen that the initial bubble size distribution created at the bottom of the column prevails throughout the height of the column. It appears that quickly an equilibrium is reached between the coalescence and break-up. The eect of break-up increases, as the supercial gas velocity is increased. The supercial gas velocity has a major eect on 19

H0 = 0.5 m vsup [mm/s] 5 10 15 20 [mm] 3.88 0.79 4.46 1.37 4.57 1.99 4.45 2.35 d32 [mm] 4.22 5.36 6.50 7.37

H0 = 0.6 m [mm] 3.88 0.80 4.45 1.38 4.55 1.97 4.41 2.32 d32 [mm] 4.23 5.37 6.46 7.28

H0 = 0.7 m [mm] 3.90 0.80 4.46 1.34 4.56 1.94 4.43 2.28 d32 [mm] 4.25 5.33 6.41 7.20

Table 1: The mean, standard deviation and d32 of the detected bubbles for dierent initial liquid heights and supercial gas velocities.

the hydrodynamics and henceforth on the bubble size distribution within the bubble column. The initial liquid height in the bubble column during the experiments has little inuence on the bubble size distribution. Increasing the hold-up in the column makes it dicult to determine the bubble size due to increased bubble overlap in the images. The hold-up in the column measured by the DIA is lower than determined by liquid expansion. This is because 2D images are used to extract 3D bubble shape information, whereas the actual bubble shape could be dierent. For velocities more than 20 mm/s, small bubbles contribute largely to the gas hold-up, whereas the gas hold-up from DIA is determined only using the large bubbles. Nomenclature A g area, [m2 ] integral gas hold-up via the liquid expansion height, [-] 20

BSD D DIA d d32 de db H H0 Hf i N PDF Ro S Vwindow vsup W

bubble size distribution depth of the column, [m] digital image analysis diameter, [m] Sauter mean diameter, [m] equivalent diameter, [m] mean bubble diameter, [m] height of the column, [m] initial liquid height, [m] nal liquid height, [m] index number of bubbles, [-] probability density function roundness, [-] surface perimeter, [m] volume of the measurement window, [m3 ] supercial gas velocity, [m/s] width of the column, [m]

21

Acknowledgements This project is part of the Industrial Partnership Program Fundamentals of Heterogeneous Bubbly Flow, which is funded by FOM, AkzoNobel, DSM, Shell and TataSteel. References Bordel, S., Mato, R., Villaverde, S, Modeling of the evolution with length of bubble size distributions in bubble columns, Chemical Engineering Science 61 (2006), 3663-3673. Br oder, D. and Sommerfeld, M., Planar shadow image velocimetry for the analysis of the hydrodynamics in bubbly ow, Meas. Sci. Technol. 18 (2007) 2513-2528. Diaz, M.E., Iranzo, A., Cuadra, D., Barbero, R., Montes, F.J., Galan, M.A., Numerical simulation of the gas-liquid ow in a laboratory scale bubble column. Inuence of bubble size distribution and non-drag forces, Chemical Engineering Journal 139 (2008), 363-379. Deen, N.G., An experimental and computational study of uid dynamics in gas-liquid chemical reactors, PhD thesis, Aalborg University Esbjerg, 2001. Honkanen, M., Saarenrinne, P., Stoor, T., Niinim aki, J., Recognition of highly overlapping ellipse-like bubble images, Meas. Sci. Technol. 16, 2005, 1760-1770.

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