Chemical Engineering Journal 172 (2011) 609614

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Chemical Engineering Journal

journal homepage: www.elsevier.com/locate/cej

Study of the rate of diffusion controlled liquidsolid reactions accompanied with gas generation in batch xed bed reactor in relation to wastewater treatment
T.M. Zewail , A.A. Zatout, G.H. Sedahmed
Chemical Engineering Department, Faculty of Engineering, Alexandria University, Alexandria 21544, Egypt

a r t i c l e

i n f o

a b s t r a c t
Factors affecting the rate of liquidsolid diffusion controlled reactions at gas evolving xed bed reactor were studied by measuring the mass transfer coefcient of cathodic copper deposition from acidied CuSO4 above the limiting current where simultaneous H2 evolution takes place in a reactor packed with either cylinders or Rasching rings with no net electrolyte ow. Variables studied were particle size, bed height and H2 discharge velocity. The rate of mass transfer was found to be proportional to the square root of H2 discharge rate. Bed height and particle size were found to have a negligible effect on the rate of mass transfer. For a given set of conditions the mass transfer coefcient at a xed bed of cylinders is higher than that at a xed bed of Raschig rings. A mathematical model based on bombardment of the mass transfer surface by high kinetic energy bubbles is presented to explain the results. Mass transfer data at the cylinder bed reactor were correlated by the equation J = 1.58(Re Fr )
0.166

Article history: Received 2 January 2011 Keywords: Fixed bed Mass transfer Gas evolving electrodes Efuent treatment Copper deposition and electrochemical reactor

While the data at a xed bed of Raschig rings were correlated by the equation J = 1.4(Re Fr )
0.162

Practical applications of the results in the design and operation of xed bed electrochemical and catalytic reactors used in wastewater treatment were highlighted. 2011 Elsevier B.V. All rights reserved.

1. Introduction In view of their high specic area and high mass transfer coefcient xed beds are used widely in building catalytic reactors used to conduct diffusion controlled reactions. The use of packed beds of large particles in building electrochemical reactors used in heavy metal removal from wastewater is receiving a growing attention [17] in view of the fact that large particle xed beds do not suffer from problems such as the high pressure drop and bed clogging by the deposited metal which are displayed in the case of porous beds made of small particles. Although much work has been done on the mass transfer behavior of xed beds under different hydrodynamic conditions such as single phase ow [1,2], two phase ow [3,4], gas sparging [5,6] and natural convection [7,8], scant attention has been given to the mass transfer behavior of gas evolving xed beds despite the frequent occurrence of this case in practice. Simultaneous H2 generation along with the main reaction is encountered in xed bed electrochemical reactors used to remove heavy metal

Corresponding author. Tel.: +20 3 5914475. E-mail address: tagchem04@yahoo.com (T.M. Zewail). 1385-8947/$ see front matter 2011 Elsevier B.V. All rights reserved. doi:10.1016/j.cej.2011.05.058

ions such Cd2+ , Pb2+ , Cr6+ , etc. from waste solutions by cathodic reduction [9]. Also simultaneous gas generation takes place in the catalytic removal of pollutants such as hydrogen peroxide (H2 O2 ) and hydrazine (N2 H4 ) from waste solutions in xed beds where O2 and N2 evolve respectively on the catalyst surface [10,11]. Also simultaneous H2 evolution takes place with catalytic copper deposition where Cu2+ ions are reduced to Cu by formaldehyde [12]. Simultaneous H2 evolution takes place sometimes during removal of heavy metals from wastewater by cementation on a less noble metal especially from solution of low pH [13]. Other examples include the production of CaCl2 by reacting HCl with a xed bed of limestone and production of salts by reacting xed beds of metal scrap (solid waste) with acids. The effect of gas evolution on the rate of diffusion controlled dissolution of a single sphere of limestone, and metal in HCl was studied by Akselrud et al. [14]. The aim of the present work is to throw some light on the effect of simultaneous gas evolution on the rate of liquidsolid diffusion controlled reactions which take place in xed beds with no net solution ow. To this end the effect of H2 evolution on the cathodic deposition of copper from acidied CuSO4 solution on a xed bed of cylinders, and a xed bed of Raschig rings was studied. Previous studies on the effect of simultaneous gas evolution on the rate

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Nomenclature a, a1 , a2 , a3 and a4 constants A bed area (cm2 ) C concentration of CuSO4 (M) D diffusivity (cm2 /s) bubble diameter (cm) db dp particle diameter (cm) F Faradays constant (cal/mol) acceleration due to gravity (cm/s2 ) g IH2 current consumed in H2 evolution (A) I current passing through the cell (A) Icu current consumed in copper deposition (A) K mass transfer coefcient (cm/s) natural convection mass transfer coefcient (cm/s) Kn Kf forced convection mass transfer coefcient (cm/s) Ko overall mass transfer coefcient (cm/s) pressure (atm) P R gas constant (cal/mol K) temperature (K) T V gas (H2 ) discharge velocity (cm/s) Z number of electrons involved in the reaction J mass transfer J factor = StSc0.66 Schmidt number ( /D) Sc St Stanton number (K/V) Fr Froude number (V2 /gdp ) Re Reynolds number ( Vdp / ) Kinematic viscosity ( / ) (cm2 /s) viscosity of the solution (g/cm s) density of the solution (g/cm3 )

effect of gas bubbles in case of low porosity porous electrode made of metal felt or metal powders justies the use of xed bed made of large particles in building gas evolving electrochemical reactors as used in the present work. 2. Theory Heat and mass transfer at gas generating surfaces take place through a complex mechanism as a result of the various events and interacting variables involved in bubble generation and the accompanying uid motion. Gas evolution involves various simultaneous and consecutive processes which include nucleation, bubble growth, separation from the surface, bubble coalescence before and after separation and buoyancy driven motion. Three different models were presented to explain mass transfer enhancement at gas evolving surfaces, namely: (i) the microconvection model which is based on the fact that the growing bubble induces a laminar liquid ow past the mass transfer surface [22,25,26]. (ii) The penetration model [15] assumes that the detachment of a bubble from the electrode surface creates a void which is lled by a fresh solution, unsteady state diffusion takes place between the fresh solution and the mass transfer surface until a new bubble is formed. (iii) The hydrodynamic model assumes that the macroconvection induced by the rising bubble swarm enhances the rate of mass transfer by thinning the diffusion layer in a manner similar to single phase natural convection [16,20]. Both the microconvection model and the penetration model lead to a log K/log V slope of 0.5 while the hydrodynamic model leads to a value of 0.33. Bubble coalescence which may take place before or after separation from the mass transfer surface at high gas discharge velocities increases the log K/log V slope to higher values [16,20]. The above models were derived and validated using mass transfer surfaces of simple geometries such as vertical and horizontal plates where the gas bubbles grow, detach and move freely in the solution. In case of gas evolving xed beds bubble motion is restricted by the void fraction of the bed, accordingly for a given gas discharge velocity, the enclosed gasliquid dispersion gains higher momentum than a solution enclosed between two parallel plates. The high shear stress of the rising gasliquid dispersion inside the bed detaches bubbles from the bed particles prematurely [17,18,27]. Under such conditions the penetration model and the microconvection model may not be dominating because other more inuential effects such as the high kinetic energy of the enclosed bubbles comes into play. The present work presents a different mechanism for mass transfer enhancement based on the collision between the high kinetic energy bubbles and the xed bed particles. When a bubble collides with a xed particle across the diffusion layer, the bubble brings a fresh supply of solution in its turbulent wake to the collision site, unsteady state diffusion between the fresh solution and the collision site on the mass transfer surface takes place until a new collision takes place. This situation can be expressed by the equation [28]. dC d2 C =D 2 dt dy (2)

of diffusion controlled reactions were based on simple geometries such as vertical and horizontal plates [15,16]. Although some work has been done on the effect of simultaneous gas evolution on the pressure drops in continuous xed bed electrochemical reactors [17,18], only one study was conducted on the effect of H2 evolution on the cathodic reduction of ferricyanide ion from alkaline solution in a xed bed of spheres [19]. Mass transfer studies at gas generating simple geometries such as vertical and horizontal plates have shown that acidity and alkalinity of the medium have a profound effect on the ability of gas bubbles to enhance the rate of mass transfer [1621], the present work sheds more light on the role of acidity and alkalinity of the medium in case of gas generating xed beds. Knowledge of the mass transfer coefcient K at gas generating xed beds with no net solution ow is essential for the design and operation of continuous gas evolving xed bed reactors (with solution ow) which are usually used in practice for wastewater treatment. The overall mass transfer coefcient Ko due to gas evolution and solution ow is given by [22]. Ko = [Kf2 + K 2 ]
0.5

(1)

where Kf is the mass transfer coefcient due to solution ow. In view of the analogy between heat and mass transfer, the present study may be of value to the case of heat and mass transfer under nucleate boiling in xed bed reactors used to conduct exothermic diffusion controlled liquidsolid reactions. In a recent development Shah et al. [23] and Al-Fetlawi et al. [24] studied the effect of simultaneous H2 and O2 evolution on the rate of reduction and oxidation respectively of vanadium salts used in vanadium redox ow batteries; the authors who used porous carbon felt electrodes found that gas evolution is detrimental to the cell performance since it reduces the active surface area for the reaction and reduces both the mass transfer and the charge transfer coefcients. This adverse

This upon integration using the pertinent boundary conditions yields K =2 D t

0.5

(3)

where t is the contact time of the fresh solution with the collision site. The residence time t is proportional to the frequency of bubble collision with the mass transfer surface which in turn depends on the number of bubbles generated per second in the solution. The number of bubbles (n) evolved per second in the solution can be

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obtained by dividing the volume of gas evolved per second by the average volume of gas bubbles, i.e. n= VA
3 /6 db

(4)

where V is the supercial gas velocity (cm3 /cm2 s); A is the area of the mass transfer surface and db is the bubble diameter. The residence time t is proportional to the inverse of the above equation, i.e. t=
3 a dd

VA Substituting for t in Eq. (3) we get

0.5

(5)

K = a1

DVA
2 d3 d

(6)

Although Ibls penetration model [15] and the present model use Higbie mathematical treatment [28], the two models differ in how the surface is renewed, in Ibls penetration model mass transfer is enhanced by bubble detachment from the mass transfer surface across the diffusion layer while in the present model, free bubbles with turbulent wake from outside the diffusion layer strike the mass transfer surface. Like other models of mass transfer at gas evolving surfaces, Eq. (6) is useful in predicting the value of log K/log V slope but it cannot be used to estimate the value of K because the proportionality constant a1 and the bubble diameter are not known. Accordingly the present work seeks to correlate the data using a dimensionless equation similar to the used in correlating mass transfer in gas sparged systems. 3. Materials and methods The apparatus consisted of a cell and electrical circuit (Fig. 1). The cell consisted of a cylindrical plexiglass container of 19 cm

diameter and 25 cm height divided into two compartments by a tight porous diaphragm. The diaphragm was made of a synthetic fabric wrapped on a perforated plastic cylinder of 8.5 cm diameter and xed to the container bottom by a 0.5 cm thick layer of wax. The inner packed bed electrode (cathode) was made of randomly oriented copper cylinders or copper Raschig rings, four bed heights were used: one layer, two layers, three layers and four layers of cylinders or Raschig rings. Three different cylinder and three different ring diameters were used: 6, 8 and 10 mm, in all cases the aspect ratio (length/diameter) was one. The cell anode was a cylindrical copper sheet of 15 cm diameter placed in the outer compartment of the cell. The electrical circuit consisted of 12 V dc power supply with a voltage regulator and a multirange ammeter connected in series with the cell. Current was fed to the bed by an insulated copper wire brazed to a cylinder or a ring placed in the bottom of the bed cathode. Before each run the packing material was etched in 10% H2 SO4 , washed with distilled water and dried. The two compartments of the cell were lled with electrolyte up to a height of 15 cm. Care was taken that the level of the electrolyte was the same in both compartments. Electrolysis was conducted at a xed current above the limiting current of copper deposition (Fig. 2) to evolve H2 simultaneously with copper deposition. H2 discharge velocities (cm3 /cm2 s) were varied by changing the value of the current passing in the cell. Electrolyte was composed of 1.5 M H2 SO4 as a supporting electrolyte and 0.01 M CuSO4 . Electrolysis was conducted at 25 1 C for a time sufcient to produce 35% change in CuSO4 concentration of the inner compartment so that no correction for the diminishing copper sulphate concentration was necessary in calculating the mass transfer coefcient [15,20,29]. A fresh solution was used in each run. All solutions were prepared using AR chemicals and distilled water. The limiting current of copper deposition (Fig. 2) under different conditions was determined in a cell similar to the above cell but without the synthetic fabric wrapped around the perforated plastic cylinder which contained the xed bed. The limiting current was determined as mentioned elsewhere [7]. Natural convection limiting current data under different conditions were published early elsewhere [8]. After electrolysis above the limiting current the solution of the inner compartment was analyzed by iodometry [30], the current consumed in depositing copper (Icu ) was calculated using Faradays law and the analytically determined decrease in CuSO4

1.2 1 0.8 0.6 0.4 0.2 0 0.4

Fig. 1. Apparatus. (1) 12 V dc power supply, (2) multirange ammeter, (3) wax layer of 0.5 cm thickness, (4) xed bed of cylinders or Raschig rings, (5) plexiglass container, (6) electrolyte level, (7) porous diaphragm, and (8) cylindrical copper anode.

Current, A

0.6

0.8

1.2

Cathode potential, V
Fig. 2. Typical polarization curve obtained for a xed bed of Raschig rings under natural convection. Ring diameter = 1 cm; bed height: 4 height; CuSO4 conc. = 0.01 M.

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concentration. The mass transfer coefcient K was calculated from the equation [31] K= Icu AZFC (7)

The current consumed in H2 evolution IH2 was calculated by subtracting the current consumed in depositing copper from the total current passing through the cell (I). The H2 discharge velocity (V) was calculated from the equation V= RTIH2 PZFA (8)

Solution density and viscosity needed for data correlation were determined by a density bottle and Ostwald viscometer respectively [32]. The diffusivity value for Cu2+ was obtained from the literature [31]. 4. Results and discussion Fig. 3 shows the effect of H2 discharge rate on the mass transfer coefcient of copper deposition in a xed bed of cylinders at different cylinder diameters and bed heights, the data t the equation K = a2 V 0.5 (9)

Bed height and cylinder diameter have a negligible effect on the mass transfer coefcient. Fig. 4 shows the effect of H2 discharge velocity the mass transfer coefcient of copper deposition in a xed bed of Raschig rings at different bed heights and cylinder diameters; as in the case of cylinder bed, the data t the equation K = a3 V 0.51 (10)

Also bed height and ring diameter have a negligible effect on the rate of mass transfer. The exponents 0.5 and 0.51 agree with the prediction of the present model [Eq. (6)]. To appreciate the extent to which the rate of mass transfer is enhanced by gas evolution, the enhancement efciency dened by = K Kn 100 Kn (11)

was calculated, where Kn is the natural convection mass transfer coefcient. For the present range of conditions ranged from 188 to 384% for cylinder bed and from 40 to 418% for ring bed. An overall mass transfer correlation was envisaged by using the dimensionless groups J, Re and Fr usually used in correlating mass transfer data for gas sparged systems. Fig. 5 shows that for a xed bed of cylinders, the data t equation J = 1.58(Fr Re)0.166 (12)

Fig. 3. Effect of H2 discharge velocity on the mass transfer coefcient at a xed bed of cylinders. Number of layers per bed: () one; ( ) two; () three; ( ) four.

With an average deviation of 17.6% while Fig. 6 shows that data for xed bed of Raschig rings t the equation J = 1.48(Fr Re)0.162 (13)

With an average deviation of 19.6%. Where J is the mass transfer J factor = K/VSc0.66 , Re Reynolds number = Vdp / and Fr Froude number = V2 /gdp . In a previous study the rate of mass transfer at a H2 evolving xed bed of spheres was determined for the cathodic reduction of K3 Fe(CN)6 in alkaline solution, the data were found to t the equation [19]. K = a4 V 0.325 (14)

The discrepancy between the exponent 0.325 and the present exponents is consistent with the results of previous studies on mass transfer at H2 evolving vertical and horizontal plates in acid and alkaline solutions [15,16,20,21,29,33,34]. In acid solutions the tendency of H2 bubbles to coalesce before and after separation from

the electrode surface is high while in alkaline solution the reverse is true. Previous studies on mass transfer at gas evolving simple electrodes have shown that large bubbles produced in acid solution favour mass transfer enhancement by the penetration and microconvection mechanism which give a log K/log V slope of 0.5 [22]. On the other hand the small sized bubbles which are produced in alkaline solution enhances the rate of mass transfer through macroconvection which gives a log K/log Vg slope ranging from 0.15 to 0.33 [16,20]. It seems that the above argument applies also for gas evolving xed beds where in acid solutions a 0.52 value was obtained for log K/log V while 0.33 values was obtained for alkaline solutions [19]. It would be of interest to compare the mass transfer coefcient at gas evolving xed bed and a horizontal upward facing disc of diameter equal to the bed diameter, Fig. 7 shows that for a given H2 discharge velocity the mass transfer coefcient is much higher at the horizontal disc. This may be explained in part by the decrease in reactant concentration as the gasliquid dispersion

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Fig. 5. Overall mass transfer correlation for a xed bed of cylinders. Cylinder diameter, mm: () 6, () 8; ( ) 10.

Fig. 6. Overall mass transfer correlation for a xed bed of Raschig rings. Ring diameter, mm: () 6; ( ) 8; () 10.

two phase ow [3] where liquidsolid mass transfer at xed beds of cylinders was found to be higher than that at xed beds of Raschig rings. The relatively low mass transfer coefcient of gas evolving xed bed compared to horizontal gas evolving at surface does not

Fig. 4. Effect of H2 discharge velocity on the mass transfer coefcient at a xed bed of Raschig rings. Number of layers per bed: () one; ( ) two; ( ) three; () four.

goes up through the bed. Replenishment of the reacted solution by a fresh solution from the pool above the bed is hindered by the bed particles. This shortcoming may be partially remedied in practice by using a continuous xed bed reactor; solution ow would replenish the reacted solution in the bed. Fig. 6 also shows that for a given set of conditions xed bed of cylinders produces higher rates of mass transfer than xed bed of Raschig rings, this may be attributed to the maldistribution of current and ow of a gasliquid dispersion in case of Raschig rings. The inner surface of vertically oriented rings receives little or no current while horizontally oriented rings receives little momentum beside the blanketing effect of H2 bubbles formed inside the rings. On the other hand the whole surface of cylinder packing is available for current and gasliquid ow. The present nding that cylinder packing is more efcient than ring packing is consistent with the mass transfer results conducted under natural convection [6,7], single phase ow [1,5] and

Fig. 7. Comparison between the mass transfer behavior of a gas evolving horizontal disc and xed beds: horizontal disk; xed bed of cylinder xed bed of Raschig rings.

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detract from their technical importance in building reactors in view of their high volumetric mass transfer coefcient (KA) which determine the reactor productivity. 5. Conclusion (1) Mass transfer at gas evolving xed beds was found to t a modied surface renewal mechanism based on bubble bombardment of the packing particles. This mechanism leads to log K/log V slope of 0.5 which agrees with the experimental data for beds of cylinders and beds of Raschig rings. For the sake of reactor scale up, the data were correlated using the dimensionless group J, Re and Fr. The mass transfer coefcient calculated from the present equations can be used in the design and operation of continuous gas evolving xed bed electrochemical reactor used for heavy metal removal from waste solutions as shown by Eq. (1). (2) Despite the high specic area of xed bed reactors, their mass transfer behavior in case of conducting liquidsolid reactions accompanied with gas evolution is inferior compared to simple geometries such as the at plate. The performance of gas evolving xed beds may be improved by operating them continuously with superimposed forced convection to replenish the reacted solution in the limited bed void fraction. (3) In contradistinction to low porosity porous electrode made of metal powders and metal felts where simultaneous gas evolution reduces the rate of the main reaction [23,24], the present results show that simultaneous gas evolution enhances the rate of the diffusion controlled main reaction by a maximum four times in case of xed bed reactors built of relatively large particles. References
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