TY - CONF A1 - Paul, Andrea A1 - Müller, D. A1 - Esche, E. A1 - Wozny, G. A1 - Maiwald, Michael T1 - Chemometric modeling of on-line Raman spectra from miniplant operation T2 - Tagungsband - 10. Kolloquium Arbeitskreis Prozessanalytik N2 - The project InPROMPT aims to establish a robust hydroformylation reaction process of the alkene n-dodecene to the aldehyde n-tridecanal using a rhodium complex as catalyst in the presence of syngas. This industrial relevant production process demands further research for optimization and expansion. For that purpose, the fiber optic coupled probe of a process Raman spectrometer is directly introduced in the product stream, which enables the recording of spectra within short control intervals. T2 - 10. Kolloquium Arbeitskreis Prozessanalytik CY - Gerlingen, Germany DA - 25.11.2014 KW - Reaction monitoring KW - Chemometrics KW - Raman spectroscopy KW - Hydroformylation PY - 2014 UR - http://arbeitskreis-prozessanalytik.de/images/stories/Veranstaltungen/Kolloquien/10_kolloquium_2014/tagungsband_10_kolloquium_ak_prozessanalytik_2014_hq-druck_f.pdf SP - P12, 34 EP - 34 PB - BAM Bundesanstalt für Materialforschung und -prüfung CY - Berlin AN - OPUS4-38361 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Meyer, Klas A1 - Ruiken, Jan-Paul A1 - Illner, M. A1 - Müller, D.-N. A1 - Esche, E. A1 - Wozny, G. A1 - Westad, Frank A1 - Maiwald, Michael T1 - Process spectroscopy in microemulsions — Raman spectroscopy for online monitoring of a homogeneous hydroformylation process JF - Measurement Science and Technology N2 - A major industrial reaction based on homogeneous catalysis is hydroformylation for the production of aldehydes from alkenes and syngas. Hydroformylation in microemulsions, which is currently under investigation at Technische Universität Berlin on a mini-plant scale, was identified as a cost efficient approach which also enhances product selectivity. Herein, we present the application of online Raman spectroscopy on the reaction of 1-dodecene to 1-tridecanal within a microemulsion. To achieve a good representation of the operation range in the mini-plant with regard to concentrations of the reactants a design of experiments was used. Based on initial Raman spectra partial least squares regression (PLSR) models were calibrated for the prediction of 1-dodecene and 1-tridecanal. Limits of predictions arise from nonlinear correlations between Raman intensity and mass fractions of compounds in the microemulsion system. Furthermore, the prediction power of PLSR models becomes limited due to unexpected by-product formation. Application of the lab-scale derived calibration spectra and PLSR models on online spectra from a mini-plant operation yielded promising estimations of 1-tridecanal and acceptable predictions of 1-dodecene mass fractions suggesting Raman spectroscopy as a suitable technique for process analytics in microemulsions. KW - Raman KW - Online KW - Chemometrics KW - Hydroformylation KW - Mini-plant KW - Microemulsion PY - 2017 DO - https://doi.org/10.1088/1361-6501/aa54f0 SN - 1361-6501 SN - 0957-0233 VL - 28 IS - 3 SP - 035502-1 EP - 035502-11 PB - IOP Publishing Ltd CY - UK AN - OPUS4-39032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -