Control of Continuous Flow Chemical Reactors: - CPAC - University ...

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Raman Validated Against HPLC8000RAMAN SCORE PLOT(region 1560 to 1720 cm -1 )and HPLC reference data10090600080Scores40002000PC1PC2AlcoholProductIntermediate7060504030HPLC determined Yield (%)02010-200060 65 70 75 80 0Time (min)
Concluding Remarks onSpectroscopic AnalysisnnnnInfrared shows much promise – CF and Data Fusion¨ More heavily impacted by temperature variation¨ Further work needed to separate temperature effectsnIn continuous flow, this will not be an issue.Raman is very promising for quantitative measurement of productionyield in batch¨ Good selective regions¨ No fluorescence¨ Minimally affected by temperature¨ Capable of monitoring side productsRaman will work well in a continuous setup¨ Multiple probes, multiplexing and very informativeSuccess of PCA modeling of spectral data indicates that HPLC willbe required only for model construction and periodic maintenance39
Page 1 and 2: Control of ContinuousFlow Chemical
Page 3 and 4: Analytical Control System DesignOpt
Page 5 and 6: Sampling Systems• NeSSI Component
Page 7 and 8: NeSSI Sampling System for ReactorRa
Page 9 and 10: NeSSI Reagent Sampling SystemNeSSI
Page 11 and 12: Corning ® Advanced-Flow TM LFLow-F
Page 13 and 14: Full Reactor System w/Control2.5 ft
Page 15 and 16: Chemical Reactionn Esterification o
Page 17 and 18: Temperature vs. Reaction Progress
Page 19 and 20: Catalyst Conc. Vs. Reaction Progres
Page 21 and 22: PLS Raman Validation ModelYield Pre
Page 23 and 24: Real-Time Quantitative Yieldn Able
Page 25 and 26: Real-Time Quantitative Analysisn Ra
Page 27 and 28: Moffat Swern Oxidation of Alcoholn
Page 29 and 30: Experimental Batch - Developmentn R
Page 31 and 32: IR Reaction Progressn Reaction prog
Page 33 and 34: Infrared Conclusionsn Spectral chan
Page 35 and 36: Pre-processed Raman Data7000Reactio
Page 37: Raman Reaction PlotRAMAN SCORE PLOT
Page 41 and 42: Swern Reactor w/sampling + Analytic
Page 43 and 44: Data Fusionn There is no one perfec
Page 45 and 46: ResultsComparison of Individual Mod

Control of Continuous Flow Chemical Reactors: - CPAC - University ...

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