研究目的
To synthesize and characterize two new zinc(II) coordination polymers based on dicarboxylates and flexible bis(benzimidazole) ligands, and investigate their luminescence, UV-vis diffuse reflection spectra, and photocatalytic properties for the degradation of methylene blue dye.
研究成果
Two zinc(II) coordination polymers were successfully synthesized and characterized. CP 1 forms a 3D dia framework, while CP 2 has a 2D hcb network. Both exhibit luminescence and semiconductor properties with band gaps of 2.98 eV and 3.93 eV, respectively. CP 2 shows higher photocatalytic activity for MB degradation (88.1% efficiency) than CP 1 (84.2%), with hydroxyl radicals playing a major role. The structures remain stable after photocatalysis, indicating potential for reuse.
研究不足
The study focuses on specific ligands and dicarboxylates, which may limit generalizability to other systems. Photocatalytic experiments were conducted under UV light only, and the stability and reusability were briefly checked but not extensively tested. The mechanism proposed is based on scavenger experiments and may require further validation.
1:Experimental Design and Method Selection:
Hydrothermal synthesis was used to prepare the coordination polymers. Characterization methods included elemental analysis, infrared spectroscopy, single crystal X-ray diffraction, powder X-ray diffraction, thermogravimetric analysis, luminescence spectroscopy, UV-vis diffuse reflectance spectroscopy, and photocatalytic degradation experiments.
2:Sample Selection and Data Sources:
Ligands L1 and L2 were synthesized following a literature procedure. Other reagents were commercially available and used without further purification.
3:List of Experimental Equipment and Materials:
Equipment included Perkin-Elmer 240C analyzer, Rigaku D/Max-2500PC diffractometer, Avatar 360 (Nicolet) spectrophotometer, Netzsch STA449 F1 thermal analyzer, FS5 luminescence spectrophotometer, UV-Vis Puxi T9 UV-visible spectrophotometer, Bruker Smart 1000 CCD diffractometer, and a 300 W mercury lamp. Materials included Zn(NO3)2·6H2O, ZnSO4·7H2O, H2PA, H2PDA, NaOH, H2O, KBr, BaSO4, methylene blue, tertiary butyl alcohol, benzoquinone, ammonium oxalate.
4:Experimental Procedures and Operational Workflow:
For synthesis, mixtures of metal salts, ligands, dicarboxylic acids, and water with adjusted pH were heated in Teflon-lined containers, then cooled to obtain crystals. For photocatalytic experiments, CP samples were added to MB solution, stirred in the dark for adsorption-desorption equilibrium, then exposed to UV light with sampling at intervals for absorbance measurement.
5:Data Analysis Methods:
Elemental analysis for C, H, N; PXRD for phase purity; IR for functional groups; TGA for thermal stability; luminescence spectra for emission properties; UV-vis for absorption and band gap calculation using Kubelka-Munk function; photocatalytic efficiency calculated from absorbance changes; pseudo-first-order kinetics for rate constants; scavenger experiments to identify reactive species.
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Elemental Analyzer
240C
Perkin-Elmer
Determination of C, H, and N elements in samples
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X-ray Diffractometer
D/Max-2500PC
Rigaku
Powder X-ray diffraction analysis for phase purity
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FT-IR Spectrophotometer
Avatar 360
Nicolet
Infrared spectroscopy for functional group analysis
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Thermal Analyzer
STA449 F1
Netzsch
Thermogravimetric analysis for thermal stability
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Luminescence Spectrophotometer
FS5
Recording luminescence spectra of solid samples
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UV-Vis Spectrophotometer
T9
Puxi
Solid-state UV/Vis diffuse reflectance spectra measurement
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CCD Diffractometer
Smart 1000
Bruker
Single crystal X-ray diffraction analysis
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Mercury Lamp
300 W
UV light source for photocatalytic experiments
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