Solid state nuclear magnetic resonance (ssNMR) is a powerful and attractive characterization method for obtaining insights into the chemical structure and dynamics of a wide range of materials. Current interest in cellulose-based materials, as sustainable and renewable natural polymer products, requires deep investigation and analysis of the chemical structure, molecular packing, end chain motion, functional modification, and solvent–matrix interactions, which strongly dictate the final product properties and tailor their end applications. In comparison to other spectroscopic techniques, on an atomic level, ssNMR is considered more advanced, especially in the structural analysis of cellulose-based materials; however, due to a dearth in the availability of a broad range of pulse sequences, and time consuming experiments, its capabilities are underestimated. This critical review article presents the comprehensive and up-to-date work done using ssNMR, including the most advanced NMR strategies used to overcome and resolve the structural difficulties present in different types of cellulose-based materials.
Solid-state NMR has proven to be a versatile technique for studying the chemical structure, 3D structure and dynamics of all sorts of chemical compounds. In nanotechnology and particularly in thin films, the study of chemical modification, molecular packing, end chain motion, distance determination and solvent-matrix interactions is essential for controlling the final product properties and applications. Despite its atomic-level research capabilities and recent technical advancements, solid-state NMR is still lacking behind other spectroscopic techniques in the field of thin films due to the underestimation of NMR capabilities, availability, great variety of nuclei and pulse sequences, lack of sensitivity for quadrupole nuclei and time-consuming experiments. This article will comprehensively and critically review the work done by solid-state NMR on different types of thin films and the most advanced NMR strategies, which are beyond conventional, and the hardware design used to overcome the technical issues in thin-film research.
Three zeolites (H‐Beta, H‐ZSM‐5 and H‐Y) were synthesized in the form of binder‐free macroscopic beads (d=215–840 μm) using a hydrothermal method employing anion‐exchange resin beads as hard template. The beads obtained after removal of the hard template by calcination consisted of crystalline zeolite domains connected with each other to form a hierarchical porous network in which the zeolitic micropores are accessible through meso‐ and macropores, as proven by characterization with XRD, N2 physisorption, SEM, and TEM. The composition, the nature and amount of acid sites and the degree of hydrophobicity of these beads were investigated by means of XRF, solid‐state NMR, pyridine‐FTIR and TGA. The zeolite beads were tested as heterogeneous catalysts in the Friedel‐Crafts acylation of anisole with acetic anhydride to produce para‐methoxyacetophenone. H‐Beta‐Beads displayed the best catalytic performance with 95 % conversion of acetic anhydride and 76 % yield of para‐methoxyacetophenone in a batch reactor test (90 °C, 6 h). Next, the catalytic performance of H‐Beta‐Beads was compared in both batch and continuous‐flow mode to extrudates prepared by mixing zeolite Beta powder with either kaolin or bentonite binders. H‐Beta‐Beads outperformed the extrudates in batch‐mode reactions and could be reused in multiple runs without discernible loss of activity. In the continuous‐flow test, H‐Beta‐Beads demonstrated higher average activity but deactivated more rapidly than the extrudates.
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