Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 1 of 13 S Removal From Acid Gas Streams

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1 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 1 of 13 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Selective H 2 S Removal From Acid Gas Streams Karimi A., Jafari Nasr M. R. *, Bakhtiary H. R., Tavassoli A. Gas Research Division, Research Institute of Petroleum Industry (RIPI), National Iranian Oil Company (NIOC) jafarimr@ripi.ir Abstract The concept of airlift reactor was used for hydrogen sulfide removal from acid gases using chelated iron solution. Rate equations for kinetic absorption and regeneration reaction and hydrodynamic parameters considering reactor behavior and internal geometry were determined. In this study experimental setups for Investigation and calculation of above parameters were provided. Air and water were used as working fluids for calculation of hydrodynamic parameters in gas and liquid phases. Correlations that express variations of two critical parameters, gas hold up and liquid circulation velocity, with superficial gas velocity were presented. Finally, a software Autosweet was developed for design and simulation of the reactor. Variations of the concentration profile of the reactants and products at unsteady and steady state, the required time to achieve to the steady state conditions, volume of the reactor in absorption and regeneration sections, gas hold up and liquid circulation velocity can be calculated based on implemented model in this study. Keywords : Airlift reactor, Tracer response technique, Hydrodynamic model, Catalytic solution. Kinetics, Modeling, Chelated iron, Hydrogen sulfide References 1. Sada etal., 1987, Oxidation Kinetics of Fe II EDTA and Fe II NTA Chelates by Dissolved Oxygen, Ind. Eng. Res., 26: Wubs, H., Beenackers, A., 1993, Kinetics of the Oxidation of Ferrous Chelates of EDTA and HEDTA in Aqueous Solution, Ind. Eng. Chem. Res., 32: Bello, R.A., Robinson, C.W. and Moo-Young, M., 1984, Liquid circulation and mixing characteristic of airlift contactors, Can J. Chem. Eng., 62: Jones, A.G., 1985, Liquid circulation in a draft tube bubble column, Chem. Eng. Sci., 40: Verlaan, P., Tramper, J., Van t Riet, K. and Luyben, K.ch.A.M., 1986, A hydrodynamic model for an airlift-loop

2 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 2 of 13 bioreactor with external loop, Chem. Eng. J., 33: B43-B53 6. Siegel, M.H., Merchuk, J.C. and Schugerl, K., 1986, Airlift reactor analysis: interrelationships between riser and down comer and gas-liquid separator behavior, including gas recirculation effects, AIChE, 32: Chisti, Y., 1989, Airlift bioreactors, Elsevier Science Publishing Co., 1st Edition, New York. 8. El- Gabbani, D. H., 1977,Hydrodynamic and mass transfer characteristics of an airlift contactor, MSc. Thesis, University of Waterloo, Ontario, Canada. 9. Onken, U. and Weiland, P., 1983, Airlift fermenters, construction behavior and uses, Advances in Biotechnological Processes, 1: Young, M.A., Carbonell, R.G., and Ollis, D.F., 1991, Airlift bioreactors: analysis of local two-phase hydrodynamics, AIChE, 37: Saez, A.E., Marquez, M.A., Roberts, G.W. and Carbonell, R.G., 1998, Hydrodynamic model for gas-lift reactors, AIChE, 44: Marquez, M.A., Saez, A.E., Carbonell, R.G., and Roberts, G.W., 1999, Coupling of hydrodynamics and chemical reaction in gas-lift reactors, AIChE, 45: Jafari, M.R., Bakhtiari, H.R., Karimi, A., Tavassoli, A., 2002, Single step H 2 S removal using chelated iron solution, Part A-Investigation of hydrodynamic parameters in an internall loop airlift reactor, Submitted to IchemE. Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Selective H 2 S Removal From Acid Gas Streams Karimi A., Jafari Nasr M. R. *, Bakhtiary H. R., Tavassoli A. Gas Research Division, Research Institute of Petroleum Industry (RIPI), National Iranian Oil Company (NIOC) jafarimr@ripi.ir Abstract The concept of airlift reactor was used for hydrogen sulfide removal from acid gases using chelated iron solution. Rate equations for kinetic absorption and regeneration reaction and hydrodynamic parameters considering reactor behavior and internal geometry were determined. In this study experimental setups for Investigation and calculation of above parameters were provided. Air and water were used as working fluids for calculation of hydrodynamic parameters in gas and liquid phases. Correlations that

3 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 3 of 13 express variations of two critical parameters, gas hold up and liquid circulation velocity, with superficial gas velocity were presented. Finally, a software Autosweet was developed for design and simulation of the reactor. Variations of the concentration profile of the reactants and products at unsteady and steady state, the required time to achieve to the steady state conditions, volume of the reactor in absorption and regeneration sections, gas hold up and liquid circulation velocity can be calculated based on implemented model in this study. Key words: Airlift reactor, Tracer response technique, Hydrodynamic model, Catalytic solution. Kinetics, Modeling, Chelated iron, Hydrogen sulfide Introduction Airlift reactors as a type of bubble columns are also used in biochemical fermentation and biological wastewater treatment. In this research liquid phase oxidation process using iron chelate catalytic solution (LOCAT) has been employed for treatment of acid gas streams. Advantages of these systems include the ability to treat both aerobic and non-aerobic gas streams, high H 2 S removal efficiencies, great flexibility; essentially 100% turndown on H 2 S concentration in feedstock, and quality and the production of innocuous products and by products. The process is named "autocirculation" which both absorption and regeneration reactions are carried out in a single vessel according to the following equations respectively: (1) The overall reaction is the reaction given in equation (3): (2) The autocircualtion scheme of the reactor is illustrated in Fig.1. In these reactors, hydrostatic pressure difference due to gas sparging in one segment causes a circulating motion in different parts of the reactor. Direction of motion is upward in the light section and downward in heavier section. These sections are named riser and downcomer respectively. In riser both absorption and regeneration reactions are carried out. In the initial section of the riser, in which equation (1) occurs, acid gas is sparged and absorbed into a catalytic solution. Then, the solution flows in regeneration section in which air is sparged where equation (2) occurs. The regenerated catalytic solution re-enters to the riser absorption zone due to the presence of the natural circulation. Due to applying different method for measuring kinetic parameters and model for interpreting the experimental results literature shows a great controversy regarding them. The investigations commonly confirm that the regeneration reaction can be considered first order with respect to the oxygen concentration [1,2]. Sada et.al. [1987], reported this order equal to [1], however, the other investigators reported it to be mostly equal one and two [2]. Reviewing some papers shows that the order varies between one and two when ph and concentration of chelated iron solution change. In this (3)

4 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 4 of 13 research, an experimental investigation is performed to determine rate equations for RIPI20*, iron chelate catalytic solution (i.e. Fe-EDTA complex), and a model are developed to predict variations of the unsteady and steady state concentration of the reactants and products. In this reactor gas holdup and liquid velocity are two important hydrodynamic parameters, which affect the mixing and gas-liquid mass transfer efficiency and play an important role in design and simulation. These parameters have been studied extensively by many investigators such as Bello [3], Jones [4], Verlaan [5] and Siegel [6]. It was found that these parameters increased as the aeration rate increased. Use of the correlations cited in literature is commonly limited to the experiment conditions and cause these correlations not to be used for a specific application. Most of the correlations expressed gas holdup as a power function of gas superficial velocity and a direct relation between liquid velocity and superficial gas velocity in the following expressions [3,7,8]: α and β are constants which depend on fluid properties and flow regime respectively. (4) In this equation, ω is a function of reactor geometry and the liquid physical properties and γ depends on flow regime [9]. In this study similar correlations developed in an internal loop airlift reactor in the form of equations (4) and (5). A large number of hydrodynamic models have been proposed. For instance, Young etal. [10] and Saez etal. [11] presented models for external loop airlift reactors which include governing, continuity and momentum equations, for riser, downcomer and separator [10-12]. Considering some modifications in their given relations, those can be used for internal loop airlift reactors. (5) Experimental setup Kinetic experiments were carried out in a glass reactor illustrated in Fig2. The reactor has 10cm diameter and 20 cm height. Both phases are well mixed via two impellers located at two positions in the bulk of gas and liquid on the agitator shaft. The agitator speed in all experiments is constant and equal to 300 rpm. Variations of iron concentration and dissolved oxygen in liquid phase is measured and saved using an oxidation-reduction probe (ORP) and a DO electrode. The experimental apparatus for study of the gas holdup and the liquid velocity in a concentric tube airlift reactor is shown in Fig.3. The reactor is constructed of glass material with internal diameter and height of down comer equal to 17.5 and 180 cm, respectively. The diameter and height of draught tube are 14.5 and 190 cm, respectively. This makes the ratio of the cross-sectional area of the riser to the down comer equals to Gas liquid separator at the top of reactor is 62 cm in height and 25 cm in diameter. The gas flows through an antenna sparger in the riser. The sparger consists 28 holes each with 1mm diameter. The draught tube was located 5 cm above the conical section. The gas flow rate was measured

5 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 5 of 13 by a mass flow controller with superficial velocity ranging from 0.2 to 2.5 cm/s. The gas phase holdup was obtained by U-tube monometer connected to pressure taps at four different axial positions in the riser. Liquid velocity obtained by two PH sensors located at two different points of the riser. The response time of PH sensors is about 0.5 second. The read out values of PH meters are stored in a PC through an interface and proper cable for online data acquisition. After gas flow adjustment and two-phase flow establishment, 2 ml of 10N NaOH solution is injected to the reactor as tracer. Injection port is located in the conical section at 5cm above the bottom of the reactor. It is noteworthy that this work must be performed rapidly. Results and discussion Gas holdup In these experiments, one of the monometer ends was connected to the reference point and the other one to a desired point along the riser. By degassing of rubber tubes the level of the monometer liquid will be equal in both sides so that static pressure difference can be eliminated. Then, a given gas flow rate is sparged in the reactor and dynamic pressure difference was read out. In the next step, for fixed conditions, the rate of gas flow rate was increased. This procedure was repeated for the other points along the riser. The local values of gas holdup along the riser for different superficial gas velocities are given in Fig.4. Fig.5 reveals variation of the average value of four points along the riser gas holdup with increasing of the superficial gas velocity. Equation (4) gives a correlation fitted to the predicted average value of gas holdup in the riser as follows: Fig.6 shows variations of overall gas holdup with the gas superficial velocity obtained from following equation: (6) (7) Liquid circulation velocity In this part of experiments, using tracer response technique, variations of liquid circulation velocity with gas superficial velocity were investigated. For each operating condition (i.e. fixed gas flow rates) response curves of PH meters were determined Fig. 7. Linear velocity of riser liquid is obtained by the following equation:

6 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 6 of 13 Where L r is the distance between the two PH sensors in the riser and t r is the difference in response time of second peaks of the response curves obtained by the two PH sensors in the riser. Fig.8 shows the experimental result. Fitting of data leads the following correlation in the form of equation (5): (8) V lr (9) Variations of riser liquid velocity as a function of riser average gas holdup are shown in the Fig.9. Fitting the measured values on the figure as a power law function results the following correlation: V lr = (10) Absorption reaction kinetics The reaction mechanism is as follows: (11) (13) (12) Writing the intrinsic rate equation in the power form yields: (14) The aim here is to determine values of n 1, m 1 and k 1. The experimental data are analyzed to determine rate constant and finally the rate equation for absorption of H 2 S in chelated iron solution at ph=8-10 and for T=22 o C can be derived as follow: Calculation steps of n 1, m 1 and k 1 are shown in Fig. 10, 11 and 12. (15)

7 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 7 of 13 Regeneration reaction kinetics Reaction mechanism is considered as follows: (16) for the intrinsic rate equation yields: (17) Considering power form The experimental data are analyzed to determine rate constant. The rate equation for regeneration reaction kinetics is: (18) Calculation steps of n 2, m 2 and k 2 are shown in Fig. 13, 14 and 15. (19) Autosweet Program Using determined rate equations for absorption and regeneration sections, Autosweet program was prepared to predict overall performance of the reactor and safe operating zone in both sections for a given condition. To solve above equations, some hydrodynamic parameters such as gas holdup, liquid velocity, equations, some hydrodynamic parameters such as gas holdup, liquid velocity, pressure distribution, bubble diameter are required. These parameters were investigated in simultaneous work of the authors [13]. Gas holdup and liquid velocity profiles, the required height for complete absorption of H 2 S (safe operating zone), concentration profile of two phases and percentage of conversion at both steady and unsteady sates are determined. Figure 15,16,17, 18,19 are outputs of this software. Conclusion 1-The absorption reaction of hydrogen sulfide by chelated iron III is first order with respect to the both reactants. 2-Regeneration reaction is first order with respect to the oxygen and is second order with respect to the

8 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 8 of 13 chelated iron II concentration 3-It was found that liquid velocity and gas holdup increase as a power law function as the superficial gas velocity increases. It was also found that liquid circulation velocity increases as a power law function as the gas holdup increases. Correlations for the specific geometry of the reactor and superficial gas velocity have been presented. 4-A mathematical model was developed to predict hydrodynamic parameters in two-phase, concentration profile of the reactants and products at unsteady and steady state, the required time to achieve to the steady state conditions, volume of the reactor in absorption and regeneration sections. 5-The results of this study were used to design a new reactor for H 2 S removal at RIPI with 850 liters capacity and also for optimization of similar reactors in operating units. 6-Application of such reactors for H 2 S removal is genuine and development of the model is necessary for simulation of larger scale units. 7-Comparison of the theoretical and experimental results shows a good agreement and confirms the capability of the model implemented and the Autosweet program. Nomenclatures U gr Riser gas superficial velocity ms -1 V Lr Liquid velocity in riser ms -1 A Cross sectional area m 2 Concentration of hydrogen sulfide at gas bulk mol/m 3 Concentration of iron in catalytic solution Reaction rate mol/sec mol/lit Concentration of oxygen mol/lit m, n Order of a reactant in reaction mol/m 2.sec Greek letters

9 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Select... Page 9 of 13 γ Constant - β Constant - α Constant s β m -β ω Constant - ε Average holdup in cross section - ε gr Average holdup along riser - ε ov Overall gas holdup - Average gas holdup at cross section - References 14. Sada etal., 1987, Oxidation Kinetics of Fe II EDTA and Fe II NTA Chelates by Dissolved Oxygen, Ind. Eng. Res., 26: Wubs, H., Beenackers, A., 1993, Kinetics of the Oxidation of Ferrous Chelates of EDTA and HEDTA in Aqueous Solution, Ind. Eng. Chem. Res., 32: Bello, R.A., Robinson, C.W. and Moo-Young, M., 1984, Liquid circulation and mixing characteristic of airlift contactors, Can J. Chem. Eng., 62: Jones, A.G., 1985, Liquid circulation in a draft tube bubble column, Chem. Eng. Sci., 40: Verlaan, P., Tramper, J., Van t Riet, K. and Luyben, K.ch.A.M., 1986, A hydrodynamic model for an airlift-loop bioreactor with external loop, Chem. Eng. J., 33: B43-B Siegel, M.H., Merchuk, J.C. and Schugerl, K., 1986, Airlift reactor analysis: interrelationships between riser and down comer and gas-liquid separator behavior, including gas recirculation effects, AIChE, 32: Chisti, Y., 1989, Airlift bioreactors, Elsevier Science Publishing Co., 1st Edition, New York. 21. El- Gabbani, D. H., 1977,Hydrodynamic and mass transfer characteristics of an airlift contactor, MSc. Thesis, University of Waterloo, Ontario, Canada. 22. Onken, U. and Weiland, P., 1983, Airlift fermenters, construction behavior and uses, Advances in Biotechnological Processes, 1: Young, M.A., Carbonell, R.G., and Ollis, D.F., 1991, Airlift bioreactors: analysis of local two-phase hydrodynamics, AIChE, 37: 403.

10 Experimental Investigation and Mathematical Modeling of An Air-Lift Reactor for Sel... Page 10 of Saez, A.E., Marquez, M.A., Roberts, G.W. and Carbonell, R.G., 1998, Hydrodynamic model for gas-lift reactors, AIChE, 44: Marquez, M.A., Saez, A.E., Carbonell, R.G., and Roberts, G.W., 1999, Coupling of hydrodynamics and chemical reaction in gas-lift reactors, AIChE, 45: Jafari, M.R., Bakhtiari, H.R., Karimi, A., Tavassoli, A., 2002, Single step H 2 S removal using chelated iron solution, Part A-Investigation of hydrodynamic parameters in an internall loop airlift reactor, Submitted to IchemE.

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