Up-scaling a Sol-Gel Process for the Production of a Multi-Component Xerogel Powder

A sol-gel process for the synthesis of a multi-component oxide material from the system SiO2-ZrO2-Al2O3underwent optimization and up-scaling. Initially, on a laboratory scale, components including precursors, catalysts, and additives were methodically evaluated to ensure a safe and efficient transition to larger volumes. Subsequently, the equipment for the whole setup of the sol-gel process was strategically selected. Leveraging insights from these optimizations, the process was successfully scaled-up to pilot-scale operation, conducting hydrolysis, condensation reactions, gelation, aging, and drying within a single, integrated conical dryer system for an 80 L batch. A visual test and FTIR spectroscopy were applied for process control and monitoring

Synthesis and application of an electronically chiral mimic of CpFe

Le domaine des composés organométalliques optiquement actifs est plus que jamais un champ d'activité important. Dans ce domaine, le complexe (-)-(1S)-dicarbonyliode[μ5-(2,8,8-triméthylbicyclo[3.2.1]oct-3,6-diµene)2-yle] fer (1), appelé 2-Me-BOD-Fe(CO)2I, se profile comme une nouvelle étape dans le développement de complexes cyclopentadiènyles chiraux apparentés. L'étude de la réactivité du complexe 1 a démontré que le système μ5 discontinu ainsi que sa chiralité inhérente le différencient des complexes apparentés comme FpI (μ5-(C5H5)Fe(CO)2I). Plus stable que FpI, le seul moyen de l'activer de manière utile est l'utilisation de sels d'argent, par exemple AgBF4, qui génèrent un complexe cationique insaturé, capable de compléter sa sphère de coordination soit en acceptant un ligand fortement électrodonneur (par ex. CO) soit en complexant une double liaison. Dans le premier cas, le complexe tricarbonylé cationique ainsi obtenu est stable et peut subir une attaque régiosélective d'un nucléophile formant ainsi un complexe diènique, qui, après décomplexation, fournit d'intéressantes molécules organiques. Dans le deuxième cas, la faible acidité de Lewis de 2-Me-BOD-Fe(CO)2+ initie une cyclisation tandem cascade si la double liaison appartient à un polyène. Nous nous sommes particulièrement intéressés à la cyclisation de l'homofarnesol en Ambrox®, un important parfum. Malgré une faible induction asymétrique et un rendement plutôt modeste (42%), la diastéréosélèctivité s'avère très bonne (dr ≈= 80%). Une analyse du processus est présentée et des hypothèses concernant le mécanisme sont émises. Afin d'optimiser et de varier les applications décrites précédemment, plusieurs dérivés de 2-Me-BOD-Fe(CO)2I ont été synthétisés en substituant le groupe méthyle stéréogénique avec des groupes électrodonneurs et des groupes électroattracteurs. De plus, comme le rendement de la synthèse de 2-Me-BOD-Fe(CO)2I chute dramatiquement lors de l'augmentation de l'échelle de sa synthèse, le contrôle de tous les paramètres concevables ainsi qu'une investigation IR en temps réel nous ont aidés à améliorer et à mieux comprendre sa synthèse.The field of new optically active and reactive organometallic species is of tremendous interest. Within this area, (-)-(1S)-dicarbonyliodide[μ5-(2,8,8-tri-methylbicyclo[3.2.1]oct-3,6-diene)2-yl] iron (1), called 2-Me-BOD-Fe(CO)2I, emerges as a new stage in the development of chiral cyclopentadienyl-like complexes. Studying the reactivity of 1 has shown that both its non-contiguous μ5-system and its inherent chirality differentiate it from related complexes like FpI (μ5-(C5H5)Fe(CO)2I). Of higher stability than FpI, the only means to activate it in a controlled manner is the use of silver salts, like AgBF4, which generates an unsaturated cationic complex able then to complete its coordination sphere either with a strong electron donating ligand (e.g. CO), or by complexing a double bond. In the first case, the resulting stable tricarbonyl cationic complex can undergo a regiospecific attack of a nucleophile forming thereby a diene complex which, after decomplexation, yields interesting organic molecules. In the second case, the weak Lewis acidity of 2-Me-BOD-Fe(CO)2+ can initiate a tandem cascade cyclization if the double bond belongs to a polyene. We have focused our attention on the cyclization of homofarnesol into Ambrox®, a fragrance of importance. Although the asymmetric induction is very weak and the yield modest (42%), the diastereoselectivity is very good (dr ≈= 80%). An analysis of the process is presented and hypotheses about the mechanism are drawn. In order to optimize, and to vary the applications described above, a series of derivatives of 2-Me-BOD-Fe(CO)2I have been synthesized by substituting the stereogenic methyl group with electron donating as well as with electron withdrawing groups. Moreover, as the yield of 2-Me-BOD-Fe(CO)2I synthesis has dramatically decreased during the scale-up of its synthesis, control of all conceivable parameters and a real-time IR investigation helped us to improve its synthesis and to better understand its mechanism

Education in flow chemistry

Flow chemistry is a growing and promising technology that can be used in research, development, and production. Nowadays, properly trained staff in flow chemistry is lacking in industry. To efficiently work with this technology, a mix of engineering and chemical skills is required. Although, this dual education is well addressed in the chemistry major given at the Haute Ecole d’Ingénierie et d’Architecture de Fribourg, a school of the University of Applied Sciences and Arts, Western Switzerland, the teaching in flow chemistry should be enhanced and reinforced

125th anniversary of the School of Engineering and Architecture of Fribourg (HEIA-FR)

This year, on the 14th of January 2021 the School of Engineering and Architecture (HEIA-FR)[1] celebrated its 125th anniversary. To celebrate, many interactive events are organized from February to September 2021

125th Anniversary of the School of Engineering and Architecture of Fribourg (HEIA-FR): Chimia Report/Company News

This year, on the 14th of January 2021 the School of Engineering and Architecture (HEIA-FR) celebrated its 125th anniversary. To celebrate, many interactive events are organized from February to September 2021