ETHICS: ae. | ( Seat) [ = eT) cil Taal eee) Sette! Measurement WER eri eli’ ene peti Dyed OEE adit ce tl ac nea ee ty Codes & Fabrication De Senin eect Ue matty Mat lal ei resIncrease Productivity Through Better Gas-Liquid Mixing The trend towards larger reactors has increased the demand on agitator systems. Developments in gas-liquid mixing technology can help meet these demands Werner Himmelsbach, Wolfgang Keller, Mark Lovallo, Thorsten Grebe and David Houlton Ekato ixing is one of the oldest unit loperations in the chemi eal process industries (CPI) and can also be one of the most demanding. The complex chal lenges presented by the wide variety of mixing tasks and sealeup needs encountered in the CPI have been compounded by a rapid rise in reactor size over the last three decades (Table 1), This trend towards larger-scale manufacturing processes has occurred across a wide range of applications including bulk cher specialty chemicals, formulated products (such as adhesives and coatings), foodstuffs, cosmetics and more. This article fo- cuses on techniques for gas-liquid mixing that can improve performance, which is particularly important when dering sealeup. (For more on mixing, not specific to gas-liquid, see CE, April 2006, pp. 46-53) Economy of scale The increase in reactor size has helped reduce costs and raise competitiveness in the global economy, but this trend has also increased demands on the performance of many reactor agita- tors. A holistic approach to increasing productivity issues, such as L.Produet quality and plant produc- tivity should be optimized. Produe ist address all relevant 50 tivity can be expressed as output per time and space as follows: pelt ve or as a specific production cost; | w ig a ae 2 Rae Inan ideal worl imized, and P. x P; should be nimized 2.Raw material and energy usage should be minimized 3.Discharges to. the environment and waste should be eliminated or minimized 4.Mechanical reliability should be maximized (this reduces not only maintenance costs and waste, but also extends operational availability and, therefore, productivity) The plant and processes should be designed with an eye to achieving faster times to market” (plant flex ibility). Consideration of flexibility issues at the design stage can sig nificantly shorten process develop- ment eycles, thereby representing a huge benefit to producers who need to maintain their competitiveness | by regularly bringing new products | to market ‘The competing demands tasks combined with huge inereases in seale (Figure 1) mean that traditional agitator and impeller designs are un- | CHEMICAL ENGINEERING WWW.CHE.COM OCTOBER 2007 FIGURE 4. This drive-shatt coupling land mechanical seal are for an 800-m? likely to provide the most economical performance. New, recently developed designs ean offer significant improve ments in process performance and cost reductions. The mechanical design, seal selection, surface finishes and new materials of construction also play a part in maximizing productivity: Significant developments in agita tion and reaction technology over the last 20 years have led to a much bet- ter understanding of design criteria, and of the best technical solutions to gas-liquid mixing challenges. Gas-lig uid reactor design is one of the areas that clearly shows the benefits of using modern technology to maximize P; and minimize Po, Designing for productivity The complexities of gas-liquid mixing stem from the variety of the physical demands encountered. A low-density compressible gas has to be dispersed into a much denser liquid with a rea sonably long eontact time. Usually, sig nificant turbulence must be induced into the liquid phase to aid mass trans- fer and reaction. In addition, rapid ‘movement of the liquid phase is often‘TABLE 1, PROCESS INDUSTRIES — EXAMPLES OF INCREASED SCALE AND OUTPUT IN RECENT DECADES Product | Number | Process Total | Production] Increase in of reac- | description feed | rate per | production tors X rate, | line, 1.000 | rate per re- reactor mesh |matsyr | actor 1975 _| size. m= = 2005 Polyethyk |2or3 | Polymerization / pre- | 150 | 400 3-6 ‘ene (HDPE)| X 300 | cipitation in cascade of continuous reactors Suspension] 200 | Bead polymerization, | not for | 65 3-6 (pve) semi-batch reactors _| batch Tere- 1X 1,000] Oxidation using air [7.500 |7,000 | 10-20 hinatic in single, continuous acid (PTA) reactor = ‘Amino |600 | Fed:batch. aerobic | not for | not 2-6 acids bioreaction batch | published ‘Aluminium |15X | Cascade of contin. | 1,500 | 800, 3 hydroxide | 4,500 _| uous precipitators Nickel | 1X 800 | Horizontal autoclave |700- | 30 New (hydro with 6 compartments | 1,000 technology metallurgy), __|(Gontinuous reactor) an ‘TABLE 2. EXAMPLES OF TECHNICAL REACTIONS WITH PURE GASES AND COMPLETE CONVERSION ‘Application Pressure] Volume] P/V, | Remark mms | kW/m? Fathardening (V>0) [2-8 [5-30 |1-2 | Balch hydrogenation Fatty acids hydrogena- |upto25| up to50 1-2 | Batch hydrogenation tion (WV = 0) Sorbitol 50-100| 20-100 2-4 | Batch hydrogenation Toluenediamine 72-20 }10-30/5-10 | Continuous hydroge- TDA / Aniline nation, strongly exo- thermic Ethylation.Ethinylation |5-20 |5-20 |2-4 | Batch Ethoxylation 3-10 |10-40|2-4 | Batch extreme volume increase Specialties (API's, addi | fypically| upto 141-5 | Magnetic drive or tives, ZieglerNattc-cata | up to mechanical seal Iysts ete.) 100 required at heat transfer surfaces that are far away from the impellers. For good measure, the liquid phase may sometimes contain 40-60 wt." solids, which must be maintained in suspen- sion. Not surprisingly, the final state of the art has not yet been reached. Reactors for gas-liquid reactions commonly consistoflarge pressure ves- sels with quite sophisticated internal components for gas feed and exhaust, liquid feed and outlet, heat transfer and baffling, as well as for agitation. Due to the hazardous nature of many processes, the mechanical seal with its peripherals is vital for plant safety As a result, the ga represent v operating costs for the user: ‘The performance of gas-liquid reac- tors has been significantly improved in recent years due to advances in agi- tation technology for two- and three phase systems. Simply changing to @ modern agitator design can some times have a large positive impact on the productivity of @ manufacturing plant. Even so, of de- sign improvements are not commonly performed when building new plants. Designs are often. simply copied or scaled up, without implementing even straightforward improvements. ‘The potential for increased pro- ductivity not only helps improve the efficiency of new plant reactors, but can also justify upgrading existing gas-liquid reactors, especially in high- cost regions such as Europe and North America. Firms that specialize in mix- ing can often help in assessing designs for improved agitation, since they have the benefit of an in-depth un derstanding of mixing fundamentals and reliable performance dat based (on years of development work. When process-specifie data are. nevessary to optimize a design or for scaleup, specialty mixing vendors ean offer to carry out process simulation and test work in dedicated mixing test equip- ment (Figures 2a and 2b). = FIGURE 2a. A test reactor should be ‘operated under carefully detined mixing conditions FIGURE 2b. Results from carefully run tests can be used as a basis for the pro- ‘duetion-seale design Reactions with pure gases From a reactor-engineering point of view, there are two major types of gas liquid reactions: those that. operate with a “pure” feed gas, and those in which the gas (air, for example) con tains a substantial fraction of inert gases, Typical pure gas reactants are hydrogen, oxygen, carbon dioxide, carbon. monoxide, chlorine, ethylene and ethylene oxide, Pure gas applica tions (Table 2) are generally those in which the gaseous reactant must be completely consumed, because it can not be released to the atmosphere (for cost, safety or ecological reasons) For a gas-liquid reaction to take place, a molecule of gas must dissolve in the liquid phase and then meet a molecule of the reagent. Often a cata lyst is also required, in which case both of the reactants must meet at-an active site on the eatalyst. Figure 8 a schematic representation of the lat ter process, The diffusion and reaction at the CHEMICAL ENGINEERING WWWW.CHE.COM OCTOBER 2007 54catalyst is usually very fast due to the very high, specific surface area of the catalyst, Therefore, the reaction is Lim- ited by transport of the gas through the boundary layer around the gas bubbles and into the liquid phase. The speeifie rate of mass transfer through the boundary layer is governed by the standard mass transfer equation. t @) k,ale®-e) The film mass transfer coefficient, ‘i, is mainly a function of the physical properties of the reactants; it is less sensitive to mixing conditions. The specific surface area, a, also depends on material properties, but can be sig- nificantly inereased by changes to the plant and process design. These fae- tors are usually expressed together as a specific mass-transfer capacity, kya, since it is difficult to measure ith ‘one directly. The term, za is usually correlated using an equation of the form: (4) where cand y are functions of the re- actor design and the chemical system, ‘Theterm (c*-c)in Equation(3) must also be carefully considered to achieve efficient production. It is sensitive to changes of process design, chiefly due to influences that can be brought to bear on the value c* (the theoretical equilibrium concentration of dissolved gas). The actual concentration of dis- solved gas in the liquid phase, e, is more a secondary funetion — it is de- termined by the relative rates of mass transfer and conversion of the gas, ‘The value of e* is, according to Henry's law, proportional to the par tial pressure of the reactive gas Hence, the use of gas in a pure form facilitates the process efficieney, but the presence of volatile solvents can reduce process efficiency. Increasing the reaction pressure ean be a simple means to boost produetivity (P;), but operation and investment costs go up with pressure, inereasing the specific production cost (Ps). The target for the design engineer is, therefore, to opti- mize kza and operating pressure, to achieve the required productivity at minimum cost, We now turn to two typieal examples assne= 5 §=12x10°M —pittusion § =(1.2t012)x 10° mS Sm (ovtmout captiary) Dittusion of gas-liquid reactions Convection using pure gases: the continuous —hydroge- nation of nitrobenzene to aniline; and the atch hydrogenation dea: = 5 t0 50 um °\ sranapor ite by liquid boundary layer of a complex organic molecule. Modern technology offers sub- stantial productivity improvements over ‘old designs for both of these cases, ecules must absor film into the bulk li tion. The molecule ary laye where the reaction Hydrogenation examples Hydrogenation processes are ployed widely throughout the CPI ‘These reactions are generally carried out on a multiphase basis (gas-liquid solid) with finely dispersed solid-metal catalysts (usually nickel in various po- ‘ous forms; or precious metals such as platinum or palladium that are finely dispersed on a porous carbon carrier) and at elevated pressures (up to 100 bar) and temperatures (up to 350°C). ‘The reactions are often strongly exo- thermic, This heat generation, to- gether with the hazards presented by handling hydrogen and the pyro- phoric metal catalysts, exacerbate the demands on the reactor system as a whole, Typical reactions include: * reduction of nitro compounds to amines * saturation of multiple bonds + reduction of carbonyls and nitriles Continuous hydrogenation. & good example of a hydrogenation reaction is the reduction of nitrobenzene to aniline (Figure 4), ‘This reaction is fast and very exo- thermic. The productivity of the reac- tor is usually limited either by mass transfer ofhydrogen gas into the liquid phase or by the need to remove large amounts of reaction heat (a typical conversion rate of 16 m.t/h of nitro- benzene requires about 18 MW of cool- ing). Maximizing the mass transfer not only increases the reaction rate, but is also desirable because high hy- drogen concentrations reduce the risk of producing undesired byproducts at the catalyst, To achieve the desired objectives, the reactor has to deliver high performance in terms of hydro igen mass transfer and heat removal Traditional hydrogenation reac- 52 CHEMICALENGINEERING WWW/CHE.COM OCTOBER 2007 FIGURE 3. Transport mechanisms for catalytic gas-liquid reactions with pure gases are depicted here. Gas mol- b out of the bub left) into the bound ary layer around it. The molecules then diffuse through the iquid, where they are mixed by convec- 35 must then diffuse through the bound- around the catalyst onto the catalyst surface, ke place NO» NH J +H, +2H,0 FIGURE 4. Catalytic hydrogenation of nitrobenzene to aniline is a typical hydrogenation reaction, tors (Figure 5, left) are fitted with a gas sparge ring near the base with an impeller arranged immediately above it to disperse the gas into the liquid. Gas that is not dissolved and reacted reaches the liquid surface and enters the headspace, inereasing the pres- sure, When the headspace pressure reaches the maximum allowable pres- , the feed must stop until hydro- gen has been absorbed from the head- space back into the liquid and reacted. ‘An impeller is often arranged at or near the liquid surface in order to gen- erate turbulence, thereby enhancing: mass transfer of hydrogen back into the liquid phase. However, “surface splashing” is very inefficient at gener- ating mass transfer and can severely limit the reaction rate. ‘To improve mass transfer with gas in the headspace, some reactor de- signs recirculate liquid from the bot- tom of the vessel via an injector (Fig- ure 5, second from left). This entrains the hydrogen and ean produce signifi- cantly higher rates of mass transfer However, it can also suffer several drawbacks 1. The delay between reaction and re- moval of heat in the external heat, exchanger may result in local over heating (reduced selectivity) 2. Effective mass transfer in the nozzle is followed bya relatively long period of hydrogen impoverishment during recireulation (leading to byproducts,He Traditional hhydrogenator: compact, surface gassing —_expensiv FIGURE 5. Various designs of hydrogena and deactivation of the catalyst) 3.The loop requires additional space and provision for thermal expan- sion between reactor and heat exchanger 4.The catalyst may not be homoge- neously suspended throughout. the reactor system (reduced effective volume) 5. The pump seal is submerged in the product (abrasive solids, increased maintenance) Another alternative is to recireulate hydrogen from the headspace back to the bottom of the reactor using an external compressor (Figure 6, second from right). This increases the mass transfer by inereasing the superficial velocity as ean be seen from Equation (4), and has the advantage of requiring, little modification of the reactor. How- ever, compressors are expensive, can incur high maintenanee costs and con- sume significant amounts of power. ‘A modern solution (Figure 5, right) uses a self-inducing turbine that acts like an internal compressor. This is illustrated in more detail in Figure 6. The feed gas enters the reactor through a simple feed pipe under- neath a primary gas-dispersion_ im peller that is designed with a built-in rotating sparger. This eliminates the need for a gas sparge ring that may block or corrode. Modern primary dis- persing impellers belong to the family ‘of modified and enhanced eoncave tur- bines that retain their performance characteristics well in the presence of a gas phase, Undissolved gas that. reaches the headspace is drawn down the hollow shaft and recirculated into the liquid phase by a specially de- with external recirculation: complex, inducing turbine: ‘compact, robust, Fequires space high performance n reactors are shown signed gas-induction impeller (vane turbine), This perpetually reeireulates gas from the headspace into the reac tion mixture with no need for any ex- ternal pump or compressor. The indue- tion effect eomes from the design of the hollow vanes. Gas is drawn through these into the low-pressure side of the impeller. When the speed is increased above a critical value, the pressure drop at the vanes exceeds the hydro- statie head and recirculation starts. ‘The gas recirculation rate can be calculated from a set of dimension less numbers. It is a function of the turbine type, diameter, speed and sub- mergenee, The vane type of turbine gives higher suetion efficiencies than traditional “channel turbines”, which consist of a series of radial channels between two horizontal disks, and the low pressure is generated by 2 two- phase flow through the channels. ‘The higher efficiency of the vane peller results in a higher gas-suetion rate and thus in higher kya values ac- cording to Equation (4) (Figure 7). The overall mass-transfer performance of these impellers is generally much bet- ter than surface splashing or a vortex. Comparing self-inducing turbines, alone (vane and channel types) shows the higher efficieney of the vane type. A combined gassing system can achieve even higher kya values, similar to, or even better than, those achieved by the more complex external recireula~ tion systems, In order to achieve a high eoncen- tration of both reactants in the zone of high turbulence, the feed of fresh liquid reactant is directed via a dip- pipe into the liquid intake of the main CHEMICAL ENGINEERING WWW.CHE.COM OCTOBER 2007 Mechanical magnetic coupling Interna gas reseulation Hotlow shat ‘Tube or plate heat exchanger Seif inducing ‘vane turbine Primary dlspenser concave ‘erine) FIGURE 6. A detailed view of a modern, ‘combined-gassing hydrogenation reac- tor is depicted 10,000; — tonsinee Sang = Woe ioe FIGURE 7. This figure compares ma transfer (log scale) with different selt- inducing impellers (oxygen in water at constant ionic strength of dissolved salt) gas recirculation impeller. The mix- ture with a high concentration of gas and liquid reactants then flows to the cooling surfaces to remove the heat of reaction and reduce the risk of local overheating. Several other performance charac teristies of the combined gassing sys- tem are also generally advantageous; 1.Formation of byproducts ean be re- duced, and catalyst life extended, because homogeneity is good and the risk of hydrogen starvation is low 2,The heat transfer capacity can be enhanced by installing heat trans- fer surfaces with specifie areas up to 20 m2m* in the reactor cham- ber. Reaction heat ean be dissipated where itis ereated, rather than in a remote heat exchanger Maintenance problems due to the mechanical seal are reduced because 53TABLE 3. PROCESSES THAT USE GASES WITH SIGNIFICANT INERTS Process, ‘Description Polyester precursors ‘Oxidation of para-xylene fo terephthalic acid. using air ‘Oxidation of sulfite ores to oxides (such as nickel and copper).using air joreactions using living cells to produce active pharmo- ‘eutical ingredients, vitamins, enzymes, foodstuffs and various specialty chemicals, using air Flue-gas desulfuriza- ‘Oxidation of calcium sulfite fo calcium sulfate, using air tion’ Precipitated calcium) Reaction of flue gases from a rotary kiln with calcium hy- carbonate roxide solution, and precipitation of the reaction prod- uct. using carbon dioxide ‘Strippers and de- sorbers scree | FIGURE 8. Reaction rate curves from a batch hydrogenation are given (1) surface gassing at 2 kW 2) and (3) combined gassing at 2 and 3 kWim? it is located in the gas space, away from the process liquids and solids Batch hydrogenation. Another ex- mple comes from the saturation of double bonds in a complex organic molecule. Figure 8 illustrates that im- proved performance can be achieved using a modern combined -gassing sys- tem instead of an old surface-gassing system. Curve (1) illustrates the rate ‘of completion of the reaction using surface gassing, the curves (2) and (3) show the relative rate of completion using combined gassing at different specific powers (2 and 3 kW/m’) Use of the latest technology can halve the reaction time in many ca ‘What is more, a well defined relation- ship between installed power and pro- ductivity can facilitate optimization of the plant economies. Gases with inert components Asdiscussed in the introduetion, many industrial processes use gases that are diluted with significant amounts of inert gas. Most commonly found are processes that use air (21% oxygen in nitrogen) or flue gases (carbon dioxide or sulfur dioxide in nitrogen, oxygen and mixed oxides), which are typically used on a once-through basis and then ischarged to the atmosphere. Table ts examples of applications in this category. Processes that use gases with inerts have some unique properties com- pared to those that use pure gases. Different mixing and gas-feed devices ‘may be required, and it is particularly nportant to pay attention to the stoi- chiometry of the reaction, Taking air ‘as an example, the following list of fac- tors must be considered: # The mass transfer rate is very sen. sitive to the concentration driving force Ac = ¢* - ¢ (Equation [3)). The equilibrium concentration, ¢%, is, proportional to the oxygen partial pressure, poy, which is reduced by the dilution in nitrogen to about one fifth + Full consumption of the oxygen from air is not possible as the driving foree, Ae, would tend to zero. There- fore, reactors using gases with inerts must operate with a stoichiometric excess, Industrial-oxidizer exhaust sases generally have around 4~ residual Op +The partial pressure of oxygen in the dispersed phase is changingras it is consumed, and this must be taken into aecount during reactor design calculations, Generally, a mean value of poy between feed and ex- haust can be calculated by integra- tion. In low-pressure applications, the enhancing effect of the hydro: statie pressure at the feed point on ‘Do must be considered * It is no longer possible to increase the mass transfer by recirculat- ing gas from the headspace, since the headspace gas concentration is depleted * The large quantity of inert nitrogen together with the requirement for a stoichiometric excess of reactant, and the saturation of the air bubbles by vapor from the liquid phase can sometimes lead to extraordinarily high gas rates in the reactor. This causes flooding of the impellers * The loss in mass-transfer capacity can partly be compensated by higher kya (power input, air rate and im- peller typelgassing system). Practi- cally, however, it generally leads to the requirement of larger reactors * Due to economies of scale, many reactors used for oxidations with air are now extremely large. Bulk chemical reactors are usually be- ‘54 CHEMICAL ENGINEERING WWW.CHE.COM OCTOBER 2007 Various processes use an inert gas fo remove a volatile ‘component from a liquid mixture. Although the mass transfer is into the gas stream itis physically equivalent to the other exam tween 200 and 1,000 m’, and min eral processing reactors can be up to 20,000 m’. At these scales, the problem of homogeneity in the actor can become significant. This, could be in terms of temperature, concentration of dissolved oxygen, reactants or nutrients, and. pH. With insufficient mixing, zones may exist where conditions are far from ideal. Whatever the inhomogeneity, the likely consequences are reduced output, lower quality or higher raw- material consumption Impellers for high gas rates ‘Traditionally, for reactors that. have very high gas rates, combinations of im. pellers such as flat-blade dise turbines (FBDT), piteh-blade turbines (PBI), or -wide-foil impellers (WEI) are used, The state of the art for many applications is now to use impellers of the coneave turbines family (Figure 9), adapted to fulfill specifi tasks in the reactor. ‘The full flow of feed gas ean be dis- persed into the Kiquid phase using a radially pumping primary disperser (PD), One or more secondary dispers ers (SD) may then be installed on the same shaft, but higher in the liquid, to provide a combination of axial blending of the liquid and redisper- sion of the gas, Redispersion is essen- tial for processes where the bubbles tend to coalesce rapidly. The PD can be equipped with a built-in rotating sparger so that the feed gas can be fed via a simple pipe arrangement, rather than needing a sparge ring. This can save investment costs and is opera tionally attractive, since a simple feed pipe is much less likely to become a source of contamination than a sparge ring with several hundred holes. Simi- larly, the risk of blockages or corrosion can be reduced, Another significant advantage of modern PD and SD impellers is thatPar opr or wide foils radial ‘xia, ‘Secondary disperser ania fecapersr Primary ai ‘all dispersion ‘of teed ge FIGURE 10. The effect of gas flow on ower retention of various impellers is shown, as discussed in the text their performance charaeteristies are ‘more stable than traditional designs. In the presence of significant quanti- ties of dispersed gas, traditional im- pellers rapidly loose power (Figure 10), whereas the concave-blade impel- s of the PD and SD types are much fected, This can simplify opera- tions that require varying gas rates, since the agitation power is relatively stable, thereby eliminating the need to adjust the agitator speed to ensure adequate mass-transfer performance {see kza correlation Equation [4]), Due to the instability of the performanee of traditional impellers, a speed control- ler is often required, which increases investment and operational costs, Figure 10 illustrates, using dimen- sionless terms, the correlation. be- peller power and gas feed- rate, These curves differ with varying Froude (Fr) numbers, which are the ratios of centrifugal to gravitational forces influencing the gas-liquid flow patterns. The three fields, as defined in Figure 10, are discussed below: Relatively low gas rates — Field 1. (Br = 0.05-0.3, Uy = 0.005-0.02 mis, FIGURE 12. This is a set of industrial- impellers, which generate P/V = 0.1-0.35 kW/m?) In this range, gasflow (@) numbers are typical of Teaching and bioreactors with low con- version rates. At these conditions, some wwide-foil (WE) impellers exhibit an in- crease of power number of up to 25% due to the change of the flow pattern around the blade, This ean be elimi nated or minimized by using a carefully designed concave impeller system. Moderate gas rates — Field 2. (Fr = OAL, Uog = 0.02-0.1 10/5, PIV = 1-5 kW/m®) Q numbers are typical of the majority of gas-liquid reactors. Tradi- tional impellers, such as PBT and FBDT, show very signifieant power number reductions caused by the formation of stable gas cavities on the trailing side of the blades (leading to a reduction in the blades’ drag coefficient). Very high gas rates — Field 3. Br 02-04, dg = 0.3-04 mis, PIV = 1-3 kW/m) These Q numbers are used in some high-efficiency continuous reac tors for bulk-chemicals manufacturing. (CHEMICAL ENGINEERING ‘Compartmentali FBDTs, and axially extended vortices with PD/SDs. The colors show the ratio of flow velocity to tip speed Blending in gas-liquid mixtures Homogeneity of the reaction mixture isa key factor for productivity, prod- uct quality and the avoidance of side reactions, but it is often overlooked because of the focus on achieving ad- equate mass transfer. Homogeneity of not just the liquid reactants is erucial, but also of dispersed and dissolved gas, mixture temperature, pH and the concentration of all reacting. compo- nents, This is true for bateh, fed-batch and continuous operations, ‘Typical flow patterns for bioreactor are depicted in Figure 11. The reactor on the left has multiple FBDTs; the reactor on the right a combination of the radially pumping PD and radially! axially pumping SD's.The radial flows from the FBDTs create two equal vo tices above and below each impeller These vortices “roll” on each other, generating poor material exchange in the axial direction, With the PD/SDs, the vortices have a strong axial defor. ‘mation and extension; they do not roll ‘on each other, but interact, This effect leads to @ reduetion of blend time by at least a factor of two (at the same WWW.CHECOM OCTOBER 2007 55TABLE 4. FLOODING PHENOMENA. Flooding phenomenon Design relevance power input and gas rate), hence sig- nificantly inereasing the homogeneity. Flooding ‘There is a limit to the gas flow that fan impeller of a given diameter and. speed can handle. Above this limit, gas flooding occurs. Flooding can, however, ecur in various ways and can look quite different from case to ease (Table 4), The various flooding phenomena appear at different gas feedrates, and ina different order, depending on the agitator design and operating condi- tions. This can lead to considerable confusion when comparing, flooding: correlations from literature. Flooding is generally less critical in small tanks, as the agitators are often. over designed. But for reactors in “world-seale” plants, especially those that are handling gas streams with large amounts of inerts, a detailed knowledge of the potential flooding phenomena ean be erucial, Independent of scale, each of these phenomenon happens when a certain ratio of gas power to impeller power is exceeded. The gas power is defined as the difference of potential enerey of the gas flow between entering and leaving the liquid. It is ereated by the hydrostatic head and is expressed as; n= AP 8-04 V a ‘The ratio of gas/impeller power ean be converted to the following di mensionless number and hence, to a seale-independent. correlation, which is strictly valid only with geometric similarity, D Qua ne FB mi IF the impellertanke diameter ratio is not constant, a corrective factor with D/T has to be added: oY Be (7) For a particular impeller, each of the flooding phenomenon deseribed in Table 4 will occur at a different value of the constants for flooding caieal aod ea GPA sncslea at ¢y, ¢g and x can only be determined ‘experimentally. Figure 18 shows an experiment, at pilot scale. As a general rule; the tank a Gas breaking through.gas _| Gas not fully dispersed, reduced interfacial eruptions on liquid surface __| area and mass transfer performance Increase of hydraulic loads on impellers, Shaft diameter, loads on agitator flange and vessel head ‘Change of flow patiern in the tank High mechanical loads on impellers (espe- cially large sizes). Important for feed and out- let locations Reduced pumping efficiency Reduced liquid flow velocities, scaling, sedi- mentation of solids o oa oz oo a a Ce) PoasPast FIGURE 13. This flooding with gas ‘eruption of about 0.4-m dia. tank diameter for flooding experiments should be at least: one meter, because at smaller scales the flow patterns with high gas content and eruptions breaking through to the liquid surface may not be fully evolved. Therefore, ¢ cy and x often appear to be scale dependent in small-scale trials. Data from small-scale trials are generally not suitable for scaling up to produe- tion scale “Loss of pumping capacity” is an important flooding phenomenon. Dif- ferent impellers have different sensi- tivities to the presence of a gas phase. Figure 14 shows the relative drop of flow velocity at the same point in a tank at the impeller level caused by ing gas feedrate (normalized as the gas feed power to agitator power ratio: Pygs/Payi) A similar Pyyg/Payiy ratio means that the impellers experi- ence the same gas feedrate at the same impeller power. These curves clearly show how the same phenomenon ap- pears at different gas rates for differ- ent impellers, Since flooding is defined asthe gas feedrate at which the pump- ing capacity is reduced to 50% of that in the absence of dispersed gas, Figure 14 shows that: * The PBY floods (loses pumping ca- pacity) at- minimal gas feedrates +The FBDT also rapidly approaches flooding. Its rapid loss in pumping capacity seems to correspond to its power drop under gassing + The PD retains its pumping capae- ity at high gas rates. It floods at gas feedrates about five times higher than the FBDT 56 CHEMICALENGINEERING WWIW.CHE.COM OCTOBER 2007 FIGURE 14. Loss of pumping capacity due to gassing (1) PD, (2) FEDT, (2) PBT Mass-transfer efficiency ‘As outlined above, mass-transfer capacity and thereby the produetiv- ity of the reaetor, ean be strongly af fected by the design of the impellers (or combinations of impellers) and the design of the gas-feed system, ‘The design engineer requires @ tool to compare the efficiency of these systems. One such measure is the “oxygen transfer efficiency” (OTE), which is usually defined as the quan. tity of gas dissolved per kWh of agi tator energy input. m, loins _ ye * =e) 8) However, OTE comparisons should be handled with care. There are many parameters that influence kya,¢* or 6, and that have nothing to do with the impeller performance at all. The most common sourees of error are: + kya depends on the gas flow via the superficial gas velocity, as deseribed in Equation (4). Higher gas rates are paid for by higher compre power, which does not appe Equation (8). Hence, a comparison at different 0, will lead to different, apparent OTES ‘The solubility, c®, is proportional to reactor pressure. Therefore, higher pressures lead to higher mass-trans- for rates. Again, this does not appear in Equation (8). Comparisons made at different pressures will show dif- ferent apparent OTEs — even with the same impellers * The mentioned effects will also oceurNOMENCLATURE a m?/m? specific g( interfacial area N st agitator speed ¢ kg/m? cehual concentation of dissolved gas Np = __ impeller power number, Np=P/(p N35) e kg/m? theoretical concentration of dissolved gas in |p N/m? pressure equilibrium wih bubbles By N/m? vapor pressure € = eonstan for ka correlation Piz — productivity defined in Equations (1) and (2) €3¢ = —__constanis for Hooding coneltion kW impeller power c $ ‘manufacturing cost Poos KW gas power dysle m diameter of gos bubble Pin, 0 bar partial pressure of reactive gas in bubbles dem diameter of catalyst parties gq? m/s gassing rate Dd” m_ _impller diameter oo sflow number, @ = q /ND? Fr = Froude-number, Fr = N?D /g s im Joble surface 9 m/s? acceleration due to gravity ' s time H m/s? Henry's soa T m Seana ; v mole/g_ lodine Volue ¥, m/s superficial gas velocity ky m/s filmmoss-transfer coefficient Vv? om? reactor or liquid volume ka 1/s specific mass-fransfer capacity x - ‘constant for ky, correlation tm ——kg/m's specifi mass tansfer rate of gas y constant fer ki, coreelaton M kg mass of product > kg/m? M —_kg/s overall mass flowrate 8p kg/m? in tall reactors with different liquid levels, and hence hydrostatic head at the gas-feed point. In this and the above ease, the increased OTE is paid by higher compressor power ‘kya is affected by many material properties and the operating condi- tions, which influenee issues such as bubble breakup, coalescence and diffusivity. It is sensitive to viscos- ity, surface tension, dissolved salts, diffusion coefficient of different gas- liquid combinations and so on *c® is also dependent on many of these parameters + Both Aya and e* are strongly depen- dent on the operating temperature + Evenslightly differingeoneentrations in a reaction mixture ean invalidate 1 comparison of impeller efficiencies In summary, data from plant and pilot model tests must be handled with care, Without a detailed knowledge of the operating parameters and the mea- surement methods, comparisons. are worthless and can easily lead to wrong, conclusions. However, if the pitfalls are avoided, a reliable comparison is possible from either pilot tests with a model system, or from the “real” rea tion in pilot or full scale. The OTE com- References 1. kato, “Handbook. of Mixing, Techn kate) Ruhr und” Michtechnik G Schopmetm, Germany, 2000 Himmelsbaeh, Houlton, Keller, Lavalla, Mixing systems: Design and scale up, Chem. Bg, 11, ‘4, pp 46-55, Apel 2008, 8, Himmelsbach, Houlton, Ortlieb, Lovalo fvances in agitation technology for ue reactions in very lange reactor, (Chom. ng. Set. 61, pp. 44-0, 2006, 4. Himmelsbach, Keller, Gezork, Krebs, Pro fessintensivierung in der Mioch- und Reak ‘onstechaiky Chee Dugeeur Tech 7, Nov? pp. 967-981, 2007 parison can then be used as the basis for the pay-back calculation, and help Justify revamping poorly performing reactors, Performing the comparisons {in cooperation with a world-class agi- tator supplier will enable the supplier to optimize the design and provide guarantees regarding performance im- provements in the ugraded reactors, Conclusions Recent. advances in agitator perfor mance and design technology mean that the performance of some existing, gas-liquid reactors can be improved by simply replacing the agitator. Special- ized vendors can contribute the latest know-how as well a5 extensive data- bases, design programs and simula tion capabilities. Modern designs and techniques can have a large impact on the pro- ductivity of a plant for a relatively modest investment, They also ensure high performance and cost-effective designs for new world-scale reactors Other developments not covered in this artiele, such as improved sealing technology and maintainability, further inerease the cost benefits. Edited by Dorothy ‘5. Himmelsbach, Lovalo, Increased producti “ct edible fate and ols Paul, Atiemo-Obeng, Kresta (Ede), “Hand book of industrial mixing: Science a Prac tie” Jon Wiley Ine, Ne, 2004 Warmoeskerken, Smith, The hollow blade nto fr npr and ae tans hom: nas Res Den, Vo. 81,1988 (at gato 5. Wiedmann, “Zim fsiddynamischen Ver: Talten von ats und dreiphacts betriebenen Reaktoren’, Dissertation, Dortmund, 182 9% Mlokarnik, Marko, “Stirring, theory and prac fice Wiley & Sons, Welnheliy 2001 58 CHEMICALENGINEERING WWW.CHE.COM OCTOBER 2007 Acknowledgements ‘The authors would like to thank David Houlton for his many contributions to this article, Authors Himnelsbach is Hats ata a Phone ‘Sess Boxe lence in process design evelopmcnt, plant design a, atin viously worked for ma Intemational manutactarer of apecality_ chem Himmelabach bold sn veruty of Rare ‘Shit rom the ue (Germany) Wolfgang, Keller is. seni rete engineer in ERATO INTs RED Department (Getopibelcs,” | tertoany Phones 197622 "aes Fa +49 7622 294 ‘eweteaco.sna He has over TO years experience a= plat engineer and rome de ‘elopment having previous worked for an iseernationa Iamalacturer of specialty polymer films. Keller holst masters dagre iu Pros einer ram the University ‘Maric Lovalle isthe techno gy manager for Beato Corp 8 Spruce Sty Oakland, NG 07036) Pha ex 314, B fom He ‘merienn fer fr the No. Loxallo. has. previo ‘worked for Union Carbide esearch engine nthe ane ariet aver ror he University of He holds « Php. Maseachuntis Amber Xe, | He holds « PhD. in ehemistry from the Univer: fy of Paderbuen (Germany) ‘Thorsten Grebe has wo for Thats RED Department since 2005 (Sehoptheim, Get many, Phone 29 S36" Fax 149.102 Email yuaekato responsible for reaction Eullancy and reactor de Grohe has previously srk the Uniweraty of Padeeee t veo -, ‘The EKATO GROUP provides their customers with the technical excellence and ‘experience of a global market leader The companies within the EKATO GROUP ‘operate across th spectrum of mixing technologies. From simple labaratry mart twrnkey roduetion plants, the EKATO GROUP provider a ange ot enginaering snes end custon-nade slrions forthe mest changing customer appllestons. The ‘synergiswithin the EKATO GROUP ensure hat reliable and cos-effocv sltion cn be provided {othe highest ql standard fx every appcaton, Tiss supported bya aba service nework. vewcomcnto EK ATO GROUP wiessnnis 9782290 Tol 21204 ‘mat latacon www.ekato.com ‘ema ecrpetaacom Circle 58 on p. 122 or go to adlinks.che.com/6900-58 CHEMICAL ENGINEERING WWW.CHE.COM OCTOBER 2007 73,EKATO. Leading Worldwide in Mixing Technologies: As market leader the EKATO Group offers cost-effective solutions ‘worldwide for all areas of the process-oriented industry with a broad range of products from industrial agitators to tailormade turnkey production units. Chemicals, plastics and polymers, pharmaceuticals, biotechnology, cosmetics, flue gas desutfurization, inks and paints, hydrometallurgy or food industry —EKATO agitators and production units are being Used successfully in almost all branches. Worldwide EKATO has already supplied more than 200,000 Units with quality “Made in Germany" being present with international subsidiaries in the USA, Australia, China, Japan, India, Singapore, France, Great Britain, Turkey, the Netherlands, as well as with more than 50 international representatives. With the new business area “RXT” (Reactors and Reaction Technology) EKATO offers a complete scope of services especially for reactors: from the process engineering design stage up to the delivery of complete units. The business activities of the EKATO Group are supported by a ‘worldwide global service network.