Reaction mechanism and in situ ATR spectroscopic studies of the 1-decene ozonolysis in micro- and semibatch reactors / Norbert Steinfeldt in Industrial & engineering chemistry research, Vol. 49 N° 1 (Janvier 2010)  

Public ISBD [article]  inIndustrial & engineering chemistry research > Vol. 49 N° 1 (Janvier 2010) . - pp. 72–80 Titre : Reaction mechanism and in situ ATR spectroscopic studies of the 1-decene ozonolysis in micro- and semibatch reactors Type de document : texte imprimé Auteurs : Norbert Steinfeldt, Auteur ; Ursula Bentrup, Auteur ; Klaus Jähnisch, Auteur Année de publication : 2010 Article en page(s) : pp. 72–80 Note générale : Industrial chemistry Langues : Anglais (eng) Mots-clés : Reaction Mechanism and in Situ ATR Spectroscopic Studies of the 1-Decene Ozonolysis Micro- Semibatch Reactors Résumé : The ozonolysis of 1-decene (1) was performed in a falling film microreactor and in a semibatch reactor using different solvents (CH2Cl2, CH3OH, or a mixture of both). The main products of ozonolysis were 3-octyl-1,2,4-trioxolane (7) in CH2Cl2 and 1-hydroperoxy-1-methoxynonane (8) in CH3OH or in a CH2Cl2/CH3OH mixture. In both cases the selectivities were higher than 70% and almost independent of 1-decene conversion and reaction temperature. The ozonolysis proceeds mainly via the cleavage of the primary ozonide into the long-chain carbonyl oxide (6) and formaldehyde (4). Besides off-line analysis in situ ATR-FTIR spectroscopic measurements using a diamond ATR probe were applied to follow the reaction progress. Integral intensities of characteristic IR bands correlate well with quantitative results obtained from gas chromatography/high-performance liquid chromatography analysis. Thus, in situ ATR proved to be a suitable method for fast and real-time monitoring of liquid-phase reactions even in the presence of unstable or explosive intermediates like ozonides and/or hydroperoxides. ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie900726s [article] Reaction mechanism and in situ ATR spectroscopic studies of the 1-decene ozonolysis in micro- and semibatch reactors [texte imprimé] / Norbert Steinfeldt, Auteur ; Ursula Bentrup, Auteur ; Klaus Jähnisch, Auteur . - 2010 . - pp. 72–80. Industrial chemistry Langues : Anglais (eng) in Industrial & engineering chemistry research > Vol. 49 N° 1 (Janvier 2010) . - pp. 72–80 Mots-clés : Reaction Mechanism and in Situ ATR Spectroscopic Studies of the 1-Decene Ozonolysis Micro- Semibatch Reactors Résumé : The ozonolysis of 1-decene (1) was performed in a falling film microreactor and in a semibatch reactor using different solvents (CH2Cl2, CH3OH, or a mixture of both). The main products of ozonolysis were 3-octyl-1,2,4-trioxolane (7) in CH2Cl2 and 1-hydroperoxy-1-methoxynonane (8) in CH3OH or in a CH2Cl2/CH3OH mixture. In both cases the selectivities were higher than 70% and almost independent of 1-decene conversion and reaction temperature. The ozonolysis proceeds mainly via the cleavage of the primary ozonide into the long-chain carbonyl oxide (6) and formaldehyde (4). Besides off-line analysis in situ ATR-FTIR spectroscopic measurements using a diamond ATR probe were applied to follow the reaction progress. Integral intensities of characteristic IR bands correlate well with quantitative results obtained from gas chromatography/high-performance liquid chromatography analysis. Thus, in situ ATR proved to be a suitable method for fast and real-time monitoring of liquid-phase reactions even in the presence of unstable or explosive intermediates like ozonides and/or hydroperoxides. ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie900726s

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