研究目的
To synthesize and characterize a novel cardanol-based salophen ligand and its Mn(II) complex, and to study their structural, photophysical, and electrochemical properties, including the investigation of solvent effects and tautomeric equilibria.
研究成果
The novel cardanol-based salophen ligand and its Mn(II) complex were successfully synthesized with high yields using microwave-assisted methods. The ligand exhibits solvent- and concentration-dependent photophysical properties due to ketoenamine-enolimine tautomerism via ESIPT. Electrochemical studies showed quasi-reversible behavior for the complex. This work advances the use of renewable resources in coordination chemistry and suggests potential applications in optoelectronics and catalysis.
研究不足
The study is limited to specific solvents and conditions; the theoretical calculations simplified the alkyl chain to reduce computational costs, which may not fully represent the actual molecule. The photophysical properties are dependent on solvent and concentration, and the electrochemical measurements were conducted in dichloromethane only, potentially limiting generalizability.
1:Experimental Design and Method Selection:
The study involved microwave-assisted synthesis of the ligand and complex, followed by characterization using spectroscopic, electrochemical, and theoretical methods to analyze structural features, photophysical properties, and electrochemical behavior.
2:Sample Selection and Data Sources:
Samples included synthesized hpbp ligand and [Mn(hpbp)] complex, with materials sourced from Sigma-Aldrich and other suppliers, using solvents like ethanol and dichloromethane for various measurements.
3:List of Experimental Equipment and Materials:
Equipment included microwave reactor (Milestone StartSYNTH), NMR spectrometer (Bruker Avance DPX), FT-IR spectrometer (PerkinElmer Frontier), Raman spectrometer (HORIBA Jobin-Yvon LabRAM), UV-Vis spectrophotometer (Agilent Cary 60), fluorescence spectrophotometer (Shimadzu RF-6000), potentiostat (Autolab type III), and computational software (Gaussian 09). Materials included hydrogenated cardanol, o-phenylenediamine, Mn(II) acetate, and various solvents.
4:9). Materials included hydrogenated cardanol, o-phenylenediamine, Mn(II) acetate, and various solvents. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Synthesis involved microwave heating for specific times and temperatures, followed by purification. Characterization included NMR, FT-IR, Raman, UV-Vis, fluorescence, cyclic voltammetry, and DFT calculations. Procedures detailed solvent preparation, sample handling, and data collection steps.
5:Data Analysis Methods:
Data were analyzed using software like NOVA 2.0 for electrochemistry, GaussSum for computational outputs, and statistical methods for spectral deconvolution and linear regressions in electrochemical studies.
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NMR spectrometer
Avance DPX
Bruker
Used for obtaining 1H and 13C NMR spectra to confirm structural features of the compounds.
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FT-IR spectrometer
Frontier
PerkinElmer
Used for infrared spectroscopic analysis to characterize vibrational modes of the compounds.
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Raman spectrometer
LabRAM
HORIBA Jobin-Yvon
Used for Raman spectroscopic analysis to study vibrational modes.
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UV-Vis spectrophotometer
Cary 60
Agilent
Used for recording UV-Visible absorption spectra to study electronic transitions.
Cary 60 UV-Vis Spectrophotometer
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fluorescence spectrophotometer
RF-6000
Shimadzu
Used for emission studies to investigate photophysical properties.
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glassy carbon electrode
GCE
Metrohm
Used as working electrode in electrochemical measurements.
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microwave reactor
StartSYNTH
Milestone
Used for microwave-assisted synthesis of the ligand and complex, providing controlled heating.
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potentiostat
Autolab type III
Eco Chemie
Used for electrochemical measurements including cyclic voltammetry.
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software
Gaussian 09
Gaussian
Used for DFT and TD-DFT calculations to simulate spectra and optimize geometries.
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software
GaussSum 3.0
Used to extract FTIR, UV-Vis spectra, and electronic transition data from computational outputs.
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