journal article·2019-12

Pd-KIT-6: synthesis of a novel three-dimensional mesoporous catalyst and studies on its enhanced catalytic applications

Suman Chirra, Suresh Siliveri, Ajay Kumar Adepu, Srinath Goskula, Sripal Reddy Gujjula, Venkatathri Narayanan

Journal of Porous Materials· Volume 26· Issue 6
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Abstract

Synthesis of a novel three-dimensional mesoporous Pd-KIT-6 is carried out by a room temperature sol–gel method. The synthesised material is well crystalline observed from the Small angle powder X-ray diffraction. Calcination at 550 °C for 8 h retains the structure. The particle sizes are in the micron range. Si/Pd ratio of the as-synthesized material is found to be 45 against the input ratio 100. Transmission electron micrograph reveals the presence of the porous hexagonal structure. Thermogravimetric studies reveal that the KIT-6 (Korea Advanced Institute of Science and Technology number 6) undergo less weight-loss compared to Pd-KIT-6, which indicates the material is more crystalline than its metal-free counterpart due to the enhanced crystallisation rate. These results also supported by BET-surface area and Transmission electron microscopic picture. The 960 cm−1 band at Fourier transform Infrared spectroscopic analysis shows that the incorporation of Pd in the framework. These FT-IR results also supported by Raman Spectroscopic analysis. Electron spin resonance spectroscopic analysis shows that the Palladium is present in the +2 oxidation state in as-synthesized samples. Diffused reflectance Ultraviolet–Visible spectroscopic results show that Palladium is in tetrahedral coordination. Microwave irradiated Suzuki–Miyaura (SM) cross-coupling reactions studied by using the Pd-KIT-6 catalyst in detail without any organic solvent at 100 °C for 10 min. The reaction carried out in the presence of phenyl iodide, phenylboronic (PhB(OH)2), and K2CO3 produce biphenyl, with 98% yield. Change of halide to Phenyl bromide gave similar results, but Phenyl chloride gave lesser conversion (20%). It is due to the electronegativity difference between the halides. A plausible reaction mechanism is also proposed.
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Research context

OpenAlex topics: Metal-Organic Frameworks: Synthesis and Applications · Mesoporous Materials and Catalysis · Polyoxometalates: Synthesis and Applications

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