Applied Catalysis A: General 221 (2001) 389396

New developments in FCC catalyst technology

R.H. Harding a, , A.W. Peters b , J.R.D. Nee a
b a Grace GmbH and Co. KG, In der Hollerhecke 1, 67547 Worms, Germany Grace Davison, Washington Research Center, 7500 Grace Drive, Columbia, MD 21044, USA

Abstract Fluid catalytic cracking (FCC) is a central technology in rening. The present paper will focus on recent progress in FCC catalyst and process technology and will analyze the driving forces for such improvements. Thereby, the direct response to environmental regulations will become obvious. Another target of new developments has been to process heavier crude sources with higher levels of contaminants. Short contact time (SCT) cracking will also be discussed, reecting signicant developments in the reactor hardware. 2001 Elsevier Science B.V. All rights reserved.
Keywords: Fluid catalytic cracking; Zeolite; Catalyst

1. Introduction Fluid catalytic cracking (FCC) is a central technology in modern rening [1,2]. The FCC unit is used to upgrade heavy gas oils and resid fuels to gasoline, diesel fuel, and light gases. An extension of the Houdry process, the unit was rst implemented in the early 1940s. A brief history of the important events in the development of FCC catalysts is shown in Table 1. In the 1960s, the introduction of zeolite Y revolutionized the process by increasing gasoline selectivity, adding almost US$ 2 of value per barrel of feed processed [3]. In the 1980s, the introduction of zeolite ZSM-5 dramatically improved the ability of reners to increase both gasoline octane number and the yields of light olens. In the early 1990s, the introduction of new alumina technologies further increased the exibility of the FCC unit to process heavier crude sources with a higher tolerance to the contaminant metals Ni and V. In this paper, we focus on recent improvements in FCC catalyst technology and the driving forces be Corresponding author. Tel.: +49-6241-403-685; fax: 49-6241-403-630. E-mail address: robert.h.harding@grace.com (R.H. Harding).

hind them. Although the FCC process has been used for more than half a century, new and important developments continue to be made in several areas. Some of these new developments are a direct response to environmental regulation. Another important driving force is the goal to process heavier crude sources with higher levels of contaminants. Changes in hardware, such as the increasing use of advanced riser termination technology to further reduce catalyst/oil contact time have also resulted in signicant changes in FCC catalyst technology. With the increasing integration of petroleum rening and chemicals production, the value of specic molecules in the product spectrum are driving FCC catalysts towards specic selectivities. Each of these trends has long term implications for the development of future catalysts and hardware for the FCC unit.

2. Environmental One of the most inuential drivers for new FCC catalysts has been the changing objective function that reners must meet in order to satisfy even more

0926-860X/01/$ see front matter 2001 Elsevier Science B.V. All rights reserved. PII: S 0 9 2 6 - 8 6 0 X ( 0 1 ) 0 0 8 1 4 - 6

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Table 1 Important dates in FCC catalyst development [4] Development Aluminum chloride catalyst Activated clay catalysts (Houdry) Silica/alumina catalyst (Houdry) First commercial production of FCC catalyst (Davison) Commercial production of microspheroidal catalysts (Davison) Last run of powdered catalyst Commercial production of zeolite Y (Union Carbide) Introduction of zeolitic FCC catalyst (Mobil) Introduction of USY and REUSY (Davison) Introduction of combustion promotion (Mobil) Feed-added Ni passivation technology (Phillips) Introduction of ZSM-5 (Mobil) Introduction of Ni-tolerant matrix technologies (Davison) Introduction of SOx reduction technology (Amoco) Introduction of additives for gasoline sulfur reduction (Davison) Introduction of CSSN zeolite (Davison) Date 1915 1928 1940 1942 1948 1956 1959 1962 1964 1974 1975 1986 1990 1992 1995 1996

stringent environmental regulations. The regulations that inuence renery operation include air and water quality emission standards and clean fuels initiatives [5]. Air quality emission standards require lower particulate emissions and lower emission of pollutants such as CO, NOx and SOx . Clean fuels initiatives are reducing the amount of sulfur, olens, and aromatics in transportation fuels. In Europe, the regulations phases over time are with the following schedule of Table 2. Some of these regulations are local (California Air Resources Board), some are national (EU gasoline quality standards), and some reect international agreements (e.g., the Kyoto Protocol to the United Nations Framework Convention on Climate). The wide variation in environmental standards, implementation measures and enforcement translates to very different results for each renery. The current EU standards for air quality are listed in Table 3.
Table 2 European gasoline specications 1997a Sulfur (mg/kg) Olens (%v/v) Benzene (%v/v) Aromatics (%v/v) Oxygen
a b

2.1. Particulates During normal operation, an average FCC unit may replace approximately 1% of its catalyst inventory to make up for particle attrition. The physical properties of FCC catalysts are designed for optimum uidization and low attrition. A trade-off exists between the mechanical strength of the catalyst and the desire to limit erosion of FCC hardware [79]. Catalyst manufacturers have recently developed methods of limiting the losses due to attrition. There are also trade-offs between the hardness of the particle (which is related to the amount of binder in the formulation) and the catalyst selectivity. Too much binder, which increases attrition resistance, can
Table 3 Emissions standards for EU countries [6] New plants (authorized or built after 1 July 1987)a SO2 (mg/N m3 ) 800 NOx (mg/N m3 ) 350 100 Particulates (mg/N m3 ) Old plants (authorized or built before 1 July 1987) SO2 Reduce by 4070% from 1980 levels by 2003 Nox Reduce by 2440% from 1980 levels by 1998 Particulates N/A (to be issued later)
a

2000 150 18 1 42 2.7

2005 50 1014b b 35 b

300 18 2.3 45 0.6

Typical values. To be determined.

FCC emission limits.

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increase the ratio of matrix to zeolite activity, leading to higher coke and gas production. Particulate emissions are expected to be further reduced as catalyst research focuses on this area. 2.2. SOx Sulfur oxides (SOx ) are a major atmospheric pollutant and precursors for acid rain. The majority of SOx produced from the FCC unit comes from the sulfur in coke that is burned off during hydrothermal regeneration of the catalyst in the FCC regenerator. In the 1990s additive technology was developed in order to adsorb the SOx in the regenerator and carry it over to the riser side of the FCC unit where it can be released as H2 S [10]. H2 S is conveniently treated with the Claus process to convert it to elemental sulfur. A successful SOx transfer additive must have three primary components. The rst step in the mechanism of SOx transfer additives is the oxidation of SO2 . Under FCC regenerator conditions, SO2 is favored over SO3 . Thus, SOx transfer additives contain catalytic ingredients that promote the oxidation of SO2 . A metal oxide component, such as magnesium alumina spinel is also included to strongly chemisorb the SO3 in the regenerator. A metal with multiple valence states such as vanadium should be included to catalyze the release of sulfur as H2 S in the riser [11]. Use of SOx additive technology will be an important tool, in addition to scrubbing hardware, to help

reners meet increasingly stringent specications for SOx emissions. 2.3. CO and NOx Regulations limiting the release of nitrogen oxides from stationary sources affect the FCC regenerator and are expected to phase in within the next decade. As NOx reduction becomes more important, the relationship between NO and CO production in the regenerator is becoming better understood [12,13]. Carbon monoxide can be readily converted to carbon dioxide with the introduction of a combustion promoter based on platinum or other noble metals. When the level of CO in the regenerator is reduced through the use of combustion promoter, nitrogen oxides have been observed to increase. The simplest explanation for this observation is that the direct reaction of NO and CO to form N2 and CO2 . As CO is eliminated from the system by the combustion promoter, there is less CO to reduce NO to N2 . Recent experiments have shown that this reaction, while it exists, is not the dominant one under FCC regenerator conditions. A reaction mechanism adapted from Yaluris et al. is shown in Fig. 1 [14]. Nitrogen-containing species in coke are one of the last species burned off the catalyst due to the strong acid-base interaction between nitrogen and the acidic catalyst. A signicant proportion of the nitrogen is burned to nitrogen gas, some is burned to NOx and some is burned to hydrocarbon species such as HCN.

Fig. 1. Expanded reaction mechanism of NOx formation in FCC.

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Pt-based combustion promoters have been found to catalyze the reaction of HCN to NO. Non-platinum combustion (such as X-NOx ) catalyze the reaction of HCN-type species to nitrogen. Thus, a non-Pt-based combustion promoter is desired for the combined objective of reducing CO and NO from the regenerator ue gas.The importance of nitrogen oxide removal technology is expected to increase as environmental regulations become more stringent. 2.4. Gasoline sulfur control The class of environmental regulations with the most far-reaching implications is the reduction of sulfur in transportation fuels. The reduction is motivated by studies, such as the Auto Oil II study, which have shown that sulfur in gasoline reversibly deactivates automobile catalytic converters, and thus has a large impact on a broad range of environmental pollutants. The most recent European Union legislation on gasoline requires a reduction in gasoline sulfur to 50 ppm. A number of European Union countries are currently producing gasoline with <50 ppm sulfur to benet from tax concessions. Germany, for example, is planning to produce 30 ppm gasoline from 2001 and 10 ppm from 2003 to make full use of tax incentives. The U.S. EPA has recently recommended a reduction to 30 ppm S to be phased in between 2004-2008. Additionally, Californias CARB Phase 3 gasoline (2003) will have 15 ppm S. In order to achieve these low levels, reners have a number of choices including gas oil hydrotreating, FCC feed hydrotreating, gasoline sulfur adsorption processes, and gasoline hydronishing. Each of these techniques has debits associated with it. Some, like gasoline hydronishing, lead to a reduction in gasoline olens and thereby reduce gasoline octane. Some, like feed hydrotreating, have a high demand for molecular hydrogen, which is often in short supply in the renery. Several strategies have been shown to reduce the level of sulfur in gasoline. While several basic FCC catalyst properties such as zeolite unit cell size, matrix activity and alumina content can be adjusted to provide sulfur reduction of about 10%, these adjustments also produce yield selectivity changes which may or may not be desirable. As a more targeted approach, catalysts have also been designed specically for the

removal of gasoline sulfur. These catalysts; GSR-1, SuRCA (with GSR-4 technology) and GFS-2000 have provided commercial gasoline sulfur reductions in the 1535% range. While we expect these catalytic technologies to improve signicantly over time, it is not likely that they will provide the very high reductions required by legislation. However, we expect that catalysts designed to reduce sulfur in gasoline and diesel fuel will work in concert with the hardware solutions to provide more cost effective clean fuels. The sulfur reduction catalysts introduce another degree of freedom for the rener, and allow less severe operation of the hardware solutions or less capital investment. For example, lowering the level of sulfur in the gasoline stream input to hydrotreaters would result in lowering the hydrotreating severity, which would reduce both hydrogen consumption and octane loss. 2.5. Gasoline olens An upper limit of 18% olens in the gasoline has been set for the European Union, and levels as low as 1014% have been proposed. In the U.S., gasoline olen level is one of the variables used in the complex model to predict emissions of volatile organic compounds (VOCs), NOx and toxic air pollutants (TAPs). RFG regulations mandating minimum levels of VOC/NOx /TAP reduction have pushed reners to produce gasoline with very low levels of olens. Federal U.S. RFG typically contains about 7% olens while California CARB gasoline contains about 5% olens. Catalyst manufacturers are meeting this challenge by extending current technology to limit the formation of gasoline olens and increase their destruction rate. One effective approach to the reduction of gasoline olens is the use of extremely high hydrogen transfer catalysts combined with matrix technology that limits the production of gasoline olens and has strong metals trapping functionality. New technologies are also being developed. A particular challenge in this area is reducing these gasoline range olens while maintaining the yield of light (C3 and C4) olens and gasoline octane. Grace Davison RFG Catalyst technology has provided commercial gasoline olens reduction of 15% (absolute) while maintaining the yield of light olens and gasoline octane.

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2.6. Interaction with hydrotreated feeds As reners invest in new hardware to meet the low gasoline sulfur requirements, a greater percentage of FCC units will be treating hydrotreated feedstocks with lower sulfur content, lower metals levels, and lower nitrogen content. One signicant technical challenge is the ability to maintain the heat balance of the FCC reactor/regenerator as hydrotreated feeds are included in the blend. With the intrinsically low coke make of these feedstocks, catalysts with higher delta coke may be required. We believe these high delta coke catalysts will probably only be required in the transition period between the installation of feed hydrotreating and the installation of additional hardware exibility to take full advantage of the low coke production. 2.7. CO2 emission One of the most difcult environmental challenges for the renery in the next century is the reduction of CO2 emissions required by the Kyoto Protocol to the United Nations Framework Convention on Climate [15]. The solution to this problem is not likely to be found in the FCC catalyst, but rather from elimination of energy inefciencies in the integrated renery system. The primary reason is the heat balance of reactor/regenerator combination. The endothermic FCC process requires a predictable amount of heat to convert a gas oil to gasoline and other products. The amount of coke required per unit of feedstock to supply this reaction energy is constant.

3.1. Contaminant metals In the 1990s, a wide range of technologies were developed to improve the tolerance of FCC catalysts to contaminant metals in the feed, primarily vanadium and nickel [17]. The dearomatization function of nickel is responsible for an increase in coke yield as the Ni level increases on the equilibrium catalyst. Moreover, the dehydrogenation activity of the Ni leads to the formation of molecular hydrogen. Since hydrogen is the most difcult gas to compress, an increase in the FCC unit can quickly limit the wet gas compressor. In order to increase the tolerance of FCC catalysts to Ni contamination, a set of aluminas based on special selective active matrix aluminas were developed. Oxygen TPD measurements provide evidence for the solid state diffusion of Ni into the alumina away from the surface and therefore the reactants. Vanadium forms vanadic acid in the regenerator, which destroys the zeolitic component of the catalyst [18]. Vanadium mobility varies from unit to unit, depending on, among other things, the level of excess oxygen in the regenerator [19]. Catalyst manufacturers have developed more stable zeolites (for example: CSSN and CSX) and a series of vanadium traps to increase the ability of the zeolite to handle vanadium. These traps are based on Ba, Ti, Rare Earth, and other elements. Some are more effective than others, but the basic idea is the same, i.e. to keep the vanadium away from the zeolite by binding to the surface of an inactive particle. Catalyst manufacturers are continuously striving to improve the stability of their catalysts to metals poisoning as resid processing becomes more important in the future. 3.2. Catalyst connectivity and transport limitations Another change in FCC catalysts in the 1990s was the introduction of materials that have good bottoms cracking performance. At constant conversion of feed, these materials convert a greater percentage of >370 C boiling range material to products. The ability of the feed molecules to reach the active sites of the catalyst is important and for heavy resid molecules, mass transport limitations play an important role [20]. In order to handle the challenges associated with cracking of resid molecules, catalyst manufacturers

3. Residual oil processing In addition to environmental regulations, several other driving forces are emerging to determine the direction of new technologies for FCC catalysts. Feed sources are expected to evolve towards heavy resids, which contain higher metals levels, and higher levels of polynuclear aromatics and heteroatom species [16]. In the 1990s, several new catalytic technologies were introduced in response to these trends. Well focus on the inuential effects of metals tolerance and bottom of the barrel processing.

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have increased the use of high surface area alumina in the catalyst. These aluminas have a small crystal size and signicant pore volume in the 50600 range. Very small pores 50100 increase bottoms cracking, but do so at the expense of coke formation. Catalysts with the intermediate pores 100300 have a lower matrix surface area for the same pore volume, but tend to convert resid molecules into more useful products. There is increasing evidence that the external surface area of the zeolite is responsible for a portion of the bottoms cracking activity of the catalyst. Therefore, it is important to construct the catalyst in such a way as to ease mass transport limitations to the surface of the zeolite. New technologies are emerging in the area of bottoms cracking designed to reduce the mass transport limitations of larger molecules. We expect this area to grow signicantly over time

Contact time over the length of the riser is ca. 58 s. At the end of the riser, the catalyst and products are separated in the disengager. It is here that product vapor can undergo non-selective (essentially thermal) cracking as hydrocarbon vapors come into contact with hot, coked catalyst. In the early 1990s, a closed cyclone system was introduced that featured cyclones directly coupled to the end of the riser [21]. This allowed rapid separation of the catalyst and products, reducing post riser cracking in the disengager. Today, all major process licensors offer advanced riser termination technologies of one sort or another with one objective in common - reduction of non-selective post-riser cracking. New processes are emerging where the catalyst/feed contact time is reduced to less than 2 s. The so-called millisecond catalytic cracking (MSCC) process was introduced in the early 1990s in the U.S. [22]. The rst MSCC unit in Europe is expected to be on-stream in 2001. 5. FCC catalysts for SCT operations Catalysts for SCT operations must be designed taking into account the following considerations [23]: catalyst/oil contact time is shorterleading to lower intrinsic conversion and bottoms cracking;

4. Short contact time (SCT) cracking In order to minimize non-selective post riser cracking many reners are revamping their units to operate in the so-called short contact time mode. In the FCC operation, catalyst and feed are contacted at the bottom of the riser with cracking reactions proceeding along the length of the riser as depicted in Fig. 2.

Fig. 2. Basic proles of kinetic trajectories along the FCC riser. Schematic adapted from [2].

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reactor temperature is generally higherleading to increased conversion and light olens yields (including increased gasoline olenicity); catalyst circulation rate is generally increased leading to an overall increase in selective conversion; regenerator/regenerated catalyst temperatures are generally lowerleading to cooler catalyst/oil mix zone temperature, hence the need for improved feed nozzles to ensure efcient feed vaporisation. To compensate for the reduced catalyst/feed contact time and consequently loss in conversion, high activity catalysts are needed. The zeolite component within the catalyst has the greatest effect on activity and therefore, proper zeolite selection is very important. In addition, it is very important to choose a matrix with the right level of activity for a particular application to address the reduction in bottoms upgrading that occurs with shorter contact time. Excess matrix activity is undesirable because it leads to poorer coke and gas selectivities. In addition to providing bottoms cracking activity, the matrix should be selected to provide low coke and gas selectivities, particularly in the presence of contaminant metals.

isobutane) and moderate matrix activity (to increase the C4-olenicity of the product) [26]. The addition of ZSM-5 is the single most important method to increase the yields of light olens at the expense of gasoline. Catalyst producers have developed methods to increase the concentration of the ZSM-5 in their additives in order to avoid dilution effects at high levels of additive. The breakthrough technologies in this area involve the stabilization of the ZSM-5 to hydrothermal deactivation at higher concentrations in the additive. Current commercial technologies range from 1025% ZSM-5, although techniques are expected to allow much higher levels in an additive particle. Several recent efforts have also been made to change the selectivity of ZSM-5 by increasing the Si/Al ratio to increase the ratio of butene to propene. However, this approach reduces the overall activity quite signicantly. In addition to C3 and C4 olens, FCC catalysts can also be designed to increase ethylene yield. Worldwide demand for ethylene is expected to increase by 50% between 1998 and 2010 [27]. With the correct application of current catalyst technologies, increases of 6 wt.% ethylene can be observed. 6.2. Production of chemical precursors In addition to light olens, the FCC catalyst can be designed to enhance the production of several other chemical precursors. The yields of xylenes and BTX, for example, can be selectively increased in the FCC gasoline range [28]. Effective use of these technologies depends on efcient separation technologies.

6. Product and selectivity control Petroleum reners that have close connection to chemical plants have a strong economic incentive to produce chemical feed stocks. This area has a particular application in the production of light olens (propylene and butylene) which have driven the recent growth of ZSM-5 usage in FCC units worldwide. 6.1. Light olen production The market for propenes and butenes is cyclical, and depends on the local demand for plastics precursors and alkylate feed [24]. In 1998, 45% of U.S. propylene was produced by the FCC unit [25]. The production of MTBE has declined due to environmental concerns, but is still a strong driver for isobutylene. There are several key determinants of light olen selectivity. In addition to increasing reactor temperature and using ZSM-5, catalysts can be designed with lower hydrogen transfer (to reduce the conversion of isobutylene to

7. Conclusions Over the last decade, the eld of uid catalytic cracking has advanced considerably in the areas of alumina technology (for improved binding and improved cracking of heavy resid molecules), zeolite stability (for improved activity and surface area retentions), and tolerance to catalytic poisons (for improved processing of heavy feeds containing high levels of Ni, Fe, and V). Current developments are improving the catalyst technology in response to environmental regulations on emissions (particulates, NOx , SOx , and CO) and the composition of transportation fuels (e.g., sulfur in diesel fuel, gasoline sulfur, benzene and olens

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R.H. Harding et al. / Applied Catalysis A: General 221 (2001) 389396 [12] X. Zhao, A.W. Peters, G.D. Weatherbee, Nitrogen Chemistry and Nox Control in a Fluid Catalytic Cracking Regenerator, I&EC Res. 36 (11) (1997) 45354542. [13] A.W. Peters, G.D. Weatherbee, X. Zhao, Origin of NOx in the FCCU Regenerator, Fuel Reformulation 5 (3) (1995) 4550. [14] G. Yaluris, A.W. Peters, X. Zhao, FCCU Regenerator Lab-Scale Simulator for Testing New Catalytic Additives for Reduction of Emissions from the FCC Regenerator, in: Proceedings of the 212th ACS National Meeting, Orlando, FL, 2529 August 1999, 41 (3), p. 901. [15] Intergovernmental Panel on Climate Change (IPCC) WGI, Climate Change 1995: The Science of Climate Change, J.T. Houghton, et al. (Eds.), Cambridge University Press, New York, 1996, 572 pp. [16] U.S. Hattiangadi, Reneries of the Future, Hydrocarbon Engineering, 1998, p. 11. [17] T.J. Dougan, U. Alkemade, L.T. Boock, B. Lakhanpal, Advances in CC Vanadium Tolerance, Oil Gas J. 92(39) 1994. [18] R.F. Wormsbecher, W.-C. Cheng, G. Kim, R.H. Harding, Vanadium Mobility in Fluid Catalytic Cracking, in: Proceedings of the 210th ACS National Meeting, Chicago, IL, 1995. [19] J.A. Rudesill, A.W. Peters, The Effect of Oxidation State of Vanadium on the Selectivity of Fluid Catalytic Cracking Catalysts, Fluid Catalytic Cracking Technology, M. Occelli, P.OConnor, Marcel Dekker, New York, 1998. [20] S.-I. Andersson, T. Myrstad, Optimum Performance of Residue FCC Catalysts, Oil Gas Eur. 23 (4) (1997) 1922. [21] J.H. Haddad, H. Owen, K.W. Schatz, US Patent 4,909,993 (1990). [22] M.W. Schnaith, A. Sexson, D. True, D.B. Bartholic, Y.K. Lee, I.S. Yoo, H.S. Kang, Oil Gas J. 96 (25) (1998) 53. [23] P.A. Diddams, H. Haave, Grace Davison FCC Technology Conference, Lisbon, 1998. [24] Advances in Rening Alkylation Technology, 1996. [25] Chemical Week, 11 August 1999, p. 36. [26] A. Haas, J.R.D. Nee, B. Kanz, FCC Catalysts Designed for C4 Hydrocarbon Maximization, in: Proceedings of the DGMK Conference, 68 October 1997, Aachen, Germany. [27] G. Martino, Catalysis for Oil Rening and Petrochemistry, Recent Developments and Future Trends, Stud. Surf. Sci. Catal. 130 (2000) 83. [28] X. Zhao, T.G. Roberie, K. Rajagopalan, p-Xylene yield in Fluid Catalytic Cracking Products, Appl. Catal. A. 145 (1996) 407418.

content). In addition, breakthroughs in the stabilization and composition of ZSM-5-based additives have given more control over light olens selectivity. Future catalyst developments in the area in FCC are likely to continue to be driven by response to environmental regulation, changes in feed quality, and advances in reactor hardware. Acknowledgements The authors thank Grace GmbH and Co. KG for permission to publish this work. References
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