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Dynamische Untersuchungen Bei Intensivierter Fischer-Tropsch Synthese

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Dynamische Untersuchungen Bei Intensivierter Fischer-Tropsch Synthese Dynamische Untersuchungen bei intensivierter Fischer-Tropsch Synthese Zur Erlangung des akademischen Grades eines DOKTORS DER INGENIEURSWISSENSCHAFTEN (DR.-ING.) von der KIT-Fakultät für Chemieingenieurwesen und Verfahrenstechnik des Karlsruher Instituts für Technologie (KIT) genehmigte DISSERTATION von Marcel Loewert aus Rüsselsheim am Main Tag der mündlichen Prüfung: 14.01.2021 Erstgutachter: Prof. Dr.-Ing. Peter Pfeifer (IMVT) Zweitgutachter: Prof. Dr. Reinhard Rauch (EBI) Danksagung An dieser Stelle ergreife ich die Gelegenheit, den Menschen zu danken, die mich lange Jahre unterstützt, bereichert und geformt haben. Zuallererst danke ich Prof. Dr.-Ing. Peter Pfeifer für seine Bemühungen, die heterogene Katalyse im Bereich der Energiewende voran zu treiben. Seine Weitsicht ermöglichte das Bearbeiten dieser interessanten Aufgabenstellung, welche sich gut mit der Motivation der Ingenieurinnen und Ingenieure in der Energiewende verzahnt. Im Falle meiner Familie können Worte nicht ausdrücken, wie dankbar ich dafür bin, dass ich stets vollen Rückhalt und absolutes Vertrauen genoss. Vieles habe ich Svenja zu verdanken, die mich lange Jahre in jeder Gemütslage erlebte und mich immer wieder motivierte und förderte. Meine Freunde in allen Heimaten, die stets hinter mir standen, mich bereichert und inspi- riert haben. All den Kollegen, mit denen ich lernen, leiden und leisten dure. Ebenso den fleißigen und begabten Studenten, die ich einen Teil ihres Weges begleiten dure. Abstract Defossilization and the reduction of CO2 emissions from anthropogenic actions are some of the big topics of this century. Being the largest contributor to the greenhouse eect, CO2 emissions influence the global the carbon balance and thus the climate that makes this planet habitable. Renewable energy sources such as wind, solar and water power, as well as biomass, only play a secondary role in energy production. This needs to change in order to build up a sustainable energy system. A myriad of new applications and technologies emerged from that incentive. One of the most debated sectors is transportation and mo- bility which still relies mostly on fossil fuels and feedstock. The general consensus on new approaches to address this issue is the implementation of e-mobility and renewable fuels. The latter relies on chemical and process engineers to develop and produce synthetic alter- natives to fossil refinery products. Those combine all advantages of traditional fuels with the property of carbon neutrality. Significant technology readiness levels are reached for synthetic fuel production. Public ac- ceptance of those fuels relies on an aordable price per energy unit, which in turn requires a high production eiciency. Process intensification is key to the highest possible eiciency to impact process economics. In this regard, microstructured reactors show outstanding re- action properties, especially for exothermic reactions that usually prove to be challenging. The system size of those reactors is well-suited for dierent scales of energy to be converted. The system intensification and the modularity makes those reactors important for decen- tralized plant-scales. Sector coupling will allow the well distributed processing of energy flows in the near future. Moreover, the system size allows a fast and safe change of process parameters. Dynamic synthesis has yet to find its way into industrial processes. Quickly changing process streams and parameters are feared to bring unpredictable eects to the catalyst and the reactor in use. In the context of an increasing share of fluctuating primary energy coming from wind and solar plants, a constant supply of feed in the process is only possible by local energy storage. For standalone plant networks, this can be realized in the form of batteries or gas tanks. The amount of mass-related energy density of a battery is significantly smaller than the density of compressed hydrogen. For that reason, gas storage will play an important role as buer in synthesis processes. Since gas tanks are costly, an intelligent process control will contribute to reduce storage size significantly. In this regard, microstructured reactors are remarkably suited for fast process changes due to small internal dimensions and eective means to extract heat from or add heat to the system, for instance. This work is devoted to shed light on dierent approaches to intensify catalytic processes in the field of renewable fuels with a high volumetric energy density. The Fischer-Tropsch reac- tion is investigated in microstructured fixed-bed reactors. These systems show exceptional reaction properties that intensify processes which makes them applicable in decentralized plants. Two dierent system sizes of microstructured fixed-bed reactors for the Fischer-Tropsch synthesis were compared to evaluate the eectivity of a reactor scale-up. Both systems were tested on their versatility towards a range of dierent process parameters. The feed- stock for the experiments comprised biomass-typical syngas with a high dilution and low syngas ratio. Both systems showed good catalytic performance despite challenging reac- tion parameters, resulting in 44 - 62 % of CO conversion. The respective influence of dif- ferent process parameters was evaluated. The upscaled system had significantly more ef- fective options to control the system parameters due to less important heat losses and the addition of evaporation cooling in the microstructured system. Consequently, the larger system was used for dynamic synthesis. System dead times were determined prior to conducting periodic changes. Parameter changes were applied as dy- namic feed gas supply and temperature manipulation, using the advantages of the scaled- up system. It was designed to produce up to 7 L of condensable product per day. Feed gas oscillation was performed by changing the syngas ratio in 30 and 8 minute cycles, re- spectively, without any disadvantages or decrease in synthesis performance. Temperature manipulation was carried out in 5 min-steps, by means of pressure ramping in the cooling water cycle. The results showed promising capability for dynamic applications. Operational limitations needed to be determined. Insight about the highest possible load flexibility were found by using fluctuating input data derived from a 10 kW photovoltaic panel and a simulated electrolyzer. The setup resulted in a highly dynamic hydrogen flow that was fed to the system. It was assumed that all the electricity from the panel was con- verted instantaneously and given to the synthesis unit over the course of a day. Dierent assumptions for the carbon source were made, leading to two dierent experimental cases. Both were designed to put the system to its limits by either a high fluctuation in syngas ra- tio or residence time changes in the one minute-range. In a final experiment, temperature control was additionally added to control carbon monoxide conversion despite changes in syngas residence time and/ or syngas ratio. No limitation by the system could be deter- mined for the applied time scale. The system was flexible and stable. Technical limitations did not allow to further shorten feed gas changes below one minute. System modeling can reduce experimental eort, as well as forecast product characteristics and yields. Especially with volatile flows, the simulation environment should be as accu- rate as possible to describe the system at hand. In this context, a multi-level model for the description of relevant processes inside the test rig was developed. A residence time dis- tribution sub-routine described flow and mixing behavior for the whole test rig in order to calculate time-dependand productivity. A program for vapor-liquid equilibrium calculation decided the state of the product fractions in each respective product condenser. A micro- kinetic model was developed and validated for the present system. Together, those three subroutines were capable of predicting time-resolved product and system characteristics only based on a few input parameters. In order to have a look into the "catalytic black box", spectroscopic methods help to elab- orate on changes happening on the catalyst’s surface during reaction. The use of high- performance catalysts further improves intensified processes in microstructured reactors. Thus it is important to understand dierent reaction phenomena. During an experiment in the CAT-ACT beamline at the KIT synchrotron with time on stream for over 300 h, cata- lyst initiation phase was evaluated by in situ X-ray absorption spectroscopy (XAS) and X-ray diraction (XRD) techniques. Experiments were carried out in a novel reaction cell suited for experimental conditions usually found in Fischer-Tropsch synthesis. Concurrent online product measurements made an operando setup possible. During reaction, a slight carbur- ization of the active cobalt was observed. Wax fouling had a by far more pronounced influ- ence on catalyst activity. Aer initiation phase, a forced hydrogen dropout caused further formation of cobalt carbides and poorly ordered graphites on the catalyst surface but no oxidation. An ex situ temperature-programmed hydrogenation and oxidation (TPH/TPO) analysis suggested a regeneration procedure applying both an oxidation and a reduction sequence. The insight obtained by the dierent chapters of this work ultimately shows the potential this technology holds in respect to decentralized applications. Small- to medium-scale plants could contribute to the production of renewable fuels wherever
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