The laboratory practical will take 2 weeks. The laboratory will be carried out at the Institute of Inorganic Chemistry (IIC), Czech Academy of Science, which has long-term expertise in the synthesis, characterization and applications of porous hybrids, important materials used in various environmental applications. The practical content listed below is just a guideline for the possible work - laboratory tasks will be updated annually according to the latest trends and challenges. Practical will also reflect the student's research topic with an emphasis on individualization. IIC CAS is equipped with devices necessary for sensitive organic synthesis (Schlenk line, glove-box), solvothermal synthesis of porous hybrids (autoclaves, programmable ovens), and instruments for the characterization of organic compounds (NMR JEOL 600 MHz) and porous hybrids (PANalytical X'Pert PRO diffractometers, 3P Instruments adsorption analyser). Motivation Hybrid materials are widely studied group of compounds, which nowadays find use in many different fields including environmental applications, for example, for adsorption or catalytic degradation of various pollutants. In recent years, IIC CAS has published several papers on the synthesis of new structures of porous hybrids by using a unique class of organic ligands, their stability under the operational conditions of various applications, and applications of porous hybrids for the removal of pollutants from water. Therefore, IIC has relevant advanced expertise in the field of materials synthesis. Objectives During practical, students will be introduced to the preparation and characterization of ligands and porous hybrids. Students will learn the standard methods of synthesis (reactions under an inert atmosphere, Schlenk techniques), purification methods used for the isolation of compounds (column chromatography, crystallization methods), and the basics of nuclear magnetic resonance (NMR) spectroscopy as the most important method of characterization. Students will also learn the standard methods of synthesis of porous hybrids (solvothermal synthesis in autoclave under autogenous pressure) and the materials characterization (powder X-ray diffraction, measurement and analysis of gas adsorption isotherms). Possible laboratory tasks the student may be involved in are the preparation of different derivatives of the methylester of 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin, metal complexes (e.g., Ni(II), Pd(II)), derivatives with substituents on beta-position of the porphyrin ring (formyl, hydroxymethyl, phosphonate etc.), and the deprotected carboxylic acid, which can be used for the synthesis of porous hybrids. Performing the syntheses, students will encounter different types of organic reactions (porphyrin condensation, metalation, Vilsmaier reaction, hydrolysis etc.). Alternatively, students will synthesize phosphinate ligands by using predominantly Pd(0)-catalysed P-C cross-coupling reactions. Students will further use the obtained organic ligands for the synthesis of respective porous hybrids. Students will study their basic properties (crystallinity, porosity). The particular laboratory tasks will be chosen individually according to the students' research topic and the ongoing research in the laboratory. Acquired skills and knowledge Students will learn the basic procedures used for the synthesis and characterization of hybrid materials. This includes methods of organic synthesis used for the preparation of ligands, common methods of characterization of organic compounds, especially NMR spectroscopy, solvothermal methods used for the synthesis of hybrid materials, and powder X-ray diffraction and adsorption measurements, which are used for the characterization of porous crystalline materials.
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