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Miroslaw Szukiewicz, Speaker at Catalysis Conference
Rzeszow University of Technology, Poland
Title : Optimization of Experiments for Heterogeneous Reactor Processes

Abstract:

The study of chemical kinetics is concerned with the measurement and interpretation of the rates of chemical reactions in the so-called process window. It tracks how quickly, the transition from an initial to the  final states of reaction occurs and what compounds are formed. This know-how is necessary to commercialize any reactor process, it helps to determine proper temperature and concentration of substances, amounts of desirable products and by-products produced that is helps designing of chemical reactors and optimization experimental conditions. The necessary condition of correct design and optimization is precision of mapping of the influence of process variables (usually: pressure, temperature, concentrations, etc) on the rate of the process. Kinetic studies can link with determination of reaction mechanism, so they can give a deeper insight into process nature. Further analysis will be presented for two heterogeneous hydrogenation processes namely hydrogenation of propylene and hydrogenation of carbon dioxide on nickel catalysts.

Let's accept, that expenditure of money, time, and other resources can be treated as a total cost of the kinetic research. Kinetic studies are tedious and resulting expensive. For heterogeneous reactor processes, many authors recommended a full research plan (FRP) as a method of determination of the kinetic dependences. FRP assumes that for all process variables the process window is divided on the grids and for each combination of the variables the rate of the process is determined experimentally. This idea is costly, especially for many process variables and the wide process window. For instance, for the first considered here process there are three process variables (temperature, total flow and propene concentration) and number of necessary measurements (NoM) is equal to 49. Designing of experiments (DoE) is one of the most powerful quality improvement techniques for reducing process variation and enhancing investigation effectiveness. It helps to reduce number of experiments that is a cost reduction without or with small precision reduction. To show how simple and efficient this manner of planning experiments is, we propose the application of factorial-design method (FP). This technique speeds up the problem solution by permitting evaluations to be made before completing all experiments. Additionally, it also indicates the relative importance of process variables and possible interactions. The most often DoE method applied in heterogeneous catalysis basis on the FP. Since heterogeneous processes are usually highly nonlinear full factorial plan (FFP) or 3k factorial plan (3kFP) are used, however the 3k design predominates. 2k factorial plan are not used. The goal of the work is presentation of steps taken to determine a kinetic equation of the mentioned hydrogenation processes, application of DoE methods and verification of results. We show that application of factorials of mixed levels - factors at two and three levels - (MFP) helps to the further reduction of costs comparing with the FFP and the 3kFP. For instance, the FFP for the first considered here process includes 27 measurement points, while the MFP – only 8. Experimental verification confirmed the correctness of the concept.

Biography:

Dr. Szukiewicz studied Chemical Engineering at the Rzeszow University of Technology (RUT), Poland and graduated as MS in 1986. He then joined the research group of Prof. Petrus at the Department of Chemical and Process Engineering, RUT. He received his PhD degree in 1995 at Cracow University of Technology. Furthermore, he obtained DSc (Habilitation) from ?ód? University of Technology in Chemical Engineering in 2009. Since 2009 he works as a Professor in the Department of Chemical and Process Engineering (RUT). His main research interests are chemical reactor engineering and mathematical methods in chemical kinetics and engineering.

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