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Bücher Wissen & Bildung Englische Bücher Naturwissenschaft, Medizin, Informatik, Technik Chemie Anorganische Chemie Heterogeneous Dirhodium Catalysts: From supported to self-supported systems
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Heterogeneous Dirhodium Catalysts: From supported to self-supported systems
Jiquan Liu (Taschenbuch, Englisch)
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Beschreibung
To further the goal of sustainable chemistry, this thesis is focused on the development of heterogenized dirhodium catalysts which can be applied in carbene transfer reactions such as cyclopropanation. Two series of heterogenized dirhodium catalysts are developed, namely supported and self-supported dirhodium catalysts by employing dirhodium complexes as precursors (e.g. rhodium trifluoroacetate… dimer (Rh2(TFA)4) and rhodium acetate dimer (Rh2(OAc)4)).
In the case of supported dirhodium catalysts, bi-functional SBA-15 with both amine and carboxyl groups is synthesized. The presence of functional ligands on SBA-15 is studied by 29Si CP MAS NMR and 13C CP MAS NMR. The covalent binding via amine and/or carboxyl groups is investigated by 15N CP MAS DNP NMR and 13C CP MAS DNP NMR (or 13C CP MAS NMR). Evidence is given that the dirhodium unit may be bound via both carboxyl and amine groups by 13C NMR and X-ray photoelectron spectroscopy (XPS) where the signals for carboxyl-amine ion pairs changes after introducing Rh2(TFA)4. Quantitative 19F MAS NMR spectra are recorded to identify the chemical environment of fluorine and number of exchanged ligands. Additionally, the physical structure of both carriers and corresponding immobilized catalysts are investigated by N2 adsorption-desorption isotherm, small angle X-ray diffraction (SAXRD) and transmission electron microscope (TEM). The morphology is studied by scanning electron microscope (SEM).
As a second example of supported dirhodium catalysts, one type of abundant natural nanoparticles namely cellulose nanocrystals (CNC) with large surface area and enriched carboxyl groups are used to anchor Rh2(TFA)4 via ligand substitution. The carboxyl binding site is confirmed by 13C CP MAS NMR. The residual trifluoroacetate group is confirmed by 19F MAS NMR. Both pristine CNC and immobilized catalyst are investigated by SEM and atomic force microscope (AFM).
In the case of self-supported dirhodium catalyst, terephthalic acid is employed to synthesize a dirhodium coordination polymer (Rh2-T) via ligand exchange. In a following case study, various types of modified terephthalic acids are introduced to bridge the dirhodium units (Rh2-TOR). 13C CP MAS NMR and XPS are performed to confirm the carboxyl binding sites. Then, diffuse reflectance ultraviolet-visible spectroscopy (DR-UV-vis) and XPS are arranged to reveal the stability of the dirhodium units during the formation of the coordination polymer. The 3D structured solid is studied by X-ray diffraction (XRD) and SEM.
The standard cyclopropanation reaction between styrene and ethyl diazoacetate (EDA) is employed to evaluate the performance of all the heterogenized dirhodium catalysts. The diastereoselectivity of the reaction is monitored by GC analysis. Finally, leaching and recyclability tests are conducted to study the stability of the binding and the reusability feature of the catalysts. Dieses Produkt haben wir gerade leider nicht auf Lager.
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Technische Daten
Erscheinungsdatum
16.09.2016
Sprache
Englisch
EAN
9783863877521
Herausgeber
Mensch & Buch
Sonderedition
Nein
Autor
Jiquan Liu
Seitenanzahl
144
Auflage
1
Einbandart
Taschenbuch
Einbandart Details
Laminiert
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