Chemical and kinetic study of acetophenone hydrogenation over Pt/Al2O3: Application of BTEM and other multivariate techniques to quantitative on-line FTIR measurements

Gao, Feng; Allian, Ayman D.; Zhang, Huajun; Cheng, Shuying; Garland, Marc

doi:10.1016/j.jcat.2006.04.024

Cited by 23 publications

(17 citation statements)

References 19 publications

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“…The selective conversion to PE is one of the major challenges encountered in the hydrogenation of ketones like AP, since competitive hydrogenation of the aromatic ring or hydrogenolysis of the corresponding alcohols can also occur [38,39]. AP hydrogenation has been studied with various heterogeneous catalysts using molecular hydrogen, sometimes with very good results in term of selectivity towards PE [40,41,42]. On the contrary, transfer hydrogenation of AP using different hydrogen donors has been typically accomplished by using transition metal complexes as homogeneous catalysts [43,44,45].…”

Section: Resultsmentioning

confidence: 99%

Preparation of Pd-Loaded Hierarchical FAU Membranes and Testing in Acetophenone Hydrogenation

et al. 2016

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Pd-loaded hierarchical FAU (Pd-FAU) membranes, containing an intrinsic secondary non-zeolitic (meso)porosity, were prepared and tested in the catalytic transfer hydrogenation of acetophenone (AP) to produce phenylethanol (PE), an industrially relevant product. The best operating conditions were preliminarily identified by testing different solvents and organic hydrogen donors in a batch hydrogenation process where micron-sized FAU seeds were employed as catalyst support. Water as solvent and formic acid as hydrogen source resulted to be the best choice in terms of conversion for the catalytic hydrogenation of AP, providing the basis for the design of a green and sustainable process. The best experimental conditions were selected and applied to the Pd-loaded FAU membrane finding enhanced catalytic performance such as a five-fold higher productivity than with the unsupported Pd-FAU crystals (11.0 vs. 2.2 mg product g cat´1¨h´1 ). The catalytic performance of the membrane on the alumina support was also tested in a tangential flow system obtaining a productivity higher than that of the batch system (22.0 vs. 11.0 mg product g cat´1¨h´1 ).

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Section: Resultsmentioning

confidence: 99%

Preparation of Pd-Loaded Hierarchical FAU Membranes and Testing in Acetophenone Hydrogenation

et al. 2016

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“…Spectroscopic techniques are increasingly being used as a method for rapidly analysing process streams as well as for on-line analysis of reacting systems [11][12][13]. In this example, Raman spectra were taken from calibration samples as well as during the reaction under study.…”

Section: Application Study To Raman Spectroscopy Datamentioning

confidence: 99%

Robust partial least squares regression—part III, outlier analysis and application studies

Krüger¹,

Zhou²,

Wang³

et al. 2008

Journal of Chemometrics

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This paper is the third part of the work on robust partial least squares (RPLS) regression. The paper focuses on implementation issues for outlier detection and diagnosis. Furthermore, the paper introduces a numerically more efficient algorithm for determining the Stahel-Donoho estimator (SDE). This has been identified as a potential drawback of the new proposed RPLS algorithm, detailed in Part II of this work. Finally, a total of three application studies are presented which involve data recorded from (i) a calibration experiment (similar number of variables/ observations), (ii) a distillation process for purifying benzene (considerably more observations than variables) and (iii) an experiment of a multi-component concentration determination using Raman spectroscopy (considerably more variables than observations).

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“…The hydrogenation of aromatic ketones has been extensively studied over the past years because of its major importance in chemistry. AP hydrogenation has been performed with various catalysts in liquid phase 10,[13][14][15][16][17] and in gas phase. 18 Selective hydrogenation of the carbonyl group yielding 1-phenylethanol (PE) is particularly interesting as PE is useful in the fragrance industry 19 or as an intermediate.…”

Section: Introductionmentioning

confidence: 99%

“…The best way to gain complete information about the kinetics is to follow in situ the concentration changes of each reactant and product during the process, using a nondestructive technique. Consumption of hydrogen, 8 chromatography, 9,10 and spectroscopy 3,[11][12][13] are some of the techniques generally employed to measure the progress of hydrogenation reactions. One of the main advantages of spectroscopy is its ability to detect and quantify several components and possible interactions, even under high pressure, without the need to take samples from the reaction system.…”

Section: Introductionmentioning

confidence: 99%

Simple in Situ Monitoring of a Complex Catalytic Reaction Network at High Pressure by Attenuated Total Reflection Fourier Transform Infrared Spectroscopy

2010

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Attenuated total reflection (ATR) Fourier transform infrared (FT-IR) in situ measurements were performed during the catalytic hydrogenation of acetophenone under high pressure (5.0 MPa). The catalyst used was a suspension of rhodium nanoparticles in an ionic liquid. At the highest temperature used (80 degrees C), the selectivity of the hydrogenation to 1-phenylethanol dropped from 80% in the beginning of the reaction, when acetylcyclohexane was the main side product, to less than 50% after a few hours of experiment because of the consecutive hydrogenation of 1-phenylethanol to ethylcyclohexane. The evolution of the concentrations of reactant and products was quantified using flawless spectra of pure components with a classical least squares (CLS) multivariate method applied to several ranges of the mid-infrared spectra. The only variable parameters of the analysis are the concentrations of each component themselves and the baseline shift of the spectrum during the reaction. The advantage of using multivariate analysis over the analysis of a single vibrational band, as well as the limitations of this type of spectral analysis, are discussed.

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Chemical and kinetic study of acetophenone hydrogenation over Pt/Al2O3: Application of BTEM and other multivariate techniques to quantitative on-line FTIR measurements

Cited by 23 publications

References 19 publications

Preparation of Pd-Loaded Hierarchical FAU Membranes and Testing in Acetophenone Hydrogenation

Preparation of Pd-Loaded Hierarchical FAU Membranes and Testing in Acetophenone Hydrogenation

Robust partial least squares regression—part III, outlier analysis and application studies

Simple in Situ Monitoring of a Complex Catalytic Reaction Network at High Pressure by Attenuated Total Reflection Fourier Transform Infrared Spectroscopy

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