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Synthesis of a MOF Supported Polyoxotungstate and its Application as Catalyst in C-C Coupling Reaction

Etessamifar, Fatemeh | 2020

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  1. Type of Document: M.Sc. Thesis
  2. Language: Farsi
  3. Document No: 52855 (03)
  4. University: Sharif University of Technology
  5. Department: Chemistry
  6. Advisor(s): Bagherzadeh, Mojtaba
  7. Abstract:
  8. In this study, a polyoxotungestate containing copper was impregnated as catalyst on a magnetic metal-organic framework (Fe3O4/MIL-101(Cr)). Initially, the desired polyoxotungestate was synthesized using sodium tungestate and sodium metasilicate salts and then copper(ІІ) ion was fixed on it. Subsequently, the MIL-101(Cr) metal-organic framework was prepared by solvothermal method; using chromium nitrate salt and 1,4-benzen dicarboxylic acid at 220 ◦C and was magnetized by co-precipitation method. Finally, the corresponding polyoxotungestate was stirred at ambient temperature for 24 h with MIL-101(Cr) and then the brown precipitate was separated using a magnet. Different techniques such as IR, ICP-OES, CHN, XRD, FE-SEM and EDX were used to identify this catalyst. Then, this catalyst was used in ternary coupling reaction of amine, alkyne and aldehyde (A3 coupling reaction). At first, factors affecting the catalytic reaction such as temperature, solvent, catalyst amount and reaction time were optimized. The optimization results showed the best reaction conditions at 100 ◦C, solvent free, the catalyst amount of 5.5×10-3 mmol and 18 h. This reaction was then carried out under optimum conditions for various substrates and it was found that the oxygen-free substrate would have a higher reaction efficiency and the steric hindrance had little effect on the reaction
  9. Keywords:
  10. Polyoxtungstate ; Copper (II) Ion ; Metal-Organic Framework ; Carbon-Carbon Coupling ; Co-Precipitation ; Polyoxometalates ; Catalytic Reactions

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