Abstract
Layered double hydroxides (LDHs) materials finds extensive applications in numerous fields such as medical science, industrial sector, agriculture and food, catalysis, polymers, nanotechnology, etc. The LDHs properties (structural, textural, morphological, spectroscopic and theoretical insights) can be design for achieving required materials for particular application in scientific areas. In the current investigation, we have synthesized mesoporous nanostructured LDHs materials via microwave, sonication and stirring method. The nanostructured LDHs was scientifically characterized by various physico-chemical techniques like XRD, N2 sorption, TGA, solid state one-dimensional 27Al magic angle spinning NMR spectroscopy, XPS, Raman Spectroscopy, FT-IR, ICP-OES, Electron Microscopy (SEM, FE-SEM, TEM and HR-TEM), EDX, elemental analysis, etc. On the basis of experimental study, it can be evidently witnessed that nanostructured LDHs materials was formed with good crystalline mesoporous nature. Solid state 27Al NMR showed single and sharp 27Al NMR signal at chemical shift value of + 1.4 ppm, strongly suggesting the presence of octahedral (Oh) AlO6 coordination site in all as-synthesized LDHs. Microwave and sonication techniques furnishes regularly dispersed well-developed flower-shaped nanocrystals however, stirring method gives mostly agglomerated nano-sized platelets. The mechanistic insights for the fabrication of nanostructures LDHs via microwave, sonication and stirring process were also highlighted. The different LDHs materials were utilized in the aldol condensation reaction of furfural with acetone for understanding structure–activity correlation. Microwave and sonication methodologies can be further exploited for the synthesis of many other inorganic–organic nanocomposites materials with stable and good dispersion of nanocrystals in addition to desired morphology and catalytic activity.
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Acknowledgements
Dr. Atul S. Nagpure acknowledged CSIR-National Chemical Laboratory (CSIR-NCL), Pune-411008, INDIA for support with instrumentation techniques. We thank University Grant Commission (UGC), New Delhi, INDIA for financial support. Authors also acknowledged assistance from Dr. Ajay Saini (Scientific Officer, Central Analytical Facilities, Manipal University, Jaipur, Rajasthan) and Mr. Moti Kumar Jha (Scientific Officer, SAIF, Manipal University, Jaipur, Rajasthan) for materials characterizations.
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ASN: conceptualization, synthesis of materials, data curation, methodology, investigation, validation, visualization, supervision, writing—original draft, writing—review & editing. SKB: synthesis of materials, investigation, funding acquisition, validation and resources. NGG: synthesis of materials, investigation, funding acquisition, validation and resources. MRL: conceptualization, methodology, visualization and supervision. SRT: conceptualization and supervision.
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Bhagat, S.K., Nagpure, A.S., Lanjewar, M.R. et al. Investigation of structural and morphological insights of nanostructured layered double hydroxides: catalytic activity in aldol condensation. J Porous Mater 31, 759–778 (2024). https://doi.org/10.1007/s10934-023-01545-w
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DOI: https://doi.org/10.1007/s10934-023-01545-w