研究目的
To synthesize polymer-TiO2 organic-inorganic composite microgels and load silver nanoparticles onto them for regulated catalytic activity, specifically investigating the temperature-dependent catalytic performance in the reduction of 4-nitrophenol.
研究成果
The polymer-TiO2/Ag composite microgels were successfully synthesized with controllable AgNP sizes and loading. They exhibited tunable SPR and enhanced catalytic activity for 4-NP reduction, modulated by temperature. The composites showed good reusability, with over 80% conversion after four cycles. The method is significant for developing thermosensitive composite catalysts.
研究不足
The study notes that the catalytic activity decreased after reuse cycles due to blockage of active sites and AgNP leaching. The effect of temperature on optical properties was relatively weak due to the rigid inorganic TiO2. The approach may have limitations in scalability or application to other reactions.
1:Experimental Design and Method Selection:
The study involved synthesizing core-shell structured P(St-NIPAM)/P(NIPAM-co-MAA) polymer microgels via soap-free and seeded emulsion polymerization. Polymer-TiO2 composites were formed by hydrolysis and condensation of TBOT in ethanol/acetonitrile using the polymer microgels as templates. AgNPs were loaded by in situ reduction of [Ag(NH3)2]+ with ethanol and NaOH. Catalytic activity was tested in the reduction of 4-NP by NaBH
2:Sample Selection and Data Sources:
Samples included polymer microgels, polymer-TiO2 composites, and polymer-TiO2/Ag composites with varying TBOT and [Ag(NH3)2]+ concentrations. Data were obtained from synthesis and characterization experiments.
3:List of Experimental Equipment and Materials:
Materials included NIPAM, St, MAA, APS, MBA, NaOH, TBOT, acetonitrile, AgNO3, ammonia, NaBH4, 4-NP, ethanol, and redistilled water. Equipment included TEM, FE-TEM, FT-IR spectrometer, XRD diffractometer, XPS instrument, TGA analyzer, laser particle analyzer, and UV-Vis spectrophotometer.
4:Experimental Procedures and Operational Workflow:
Synthesis steps involved dispersion, reaction, centrifugation, and drying. Catalytic tests involved mixing reactants in a cuvette, adding catalyst, and monitoring with UV-Vis spectroscopy. Characterization included morphology, composition, and thermal analysis.
5:Data Analysis Methods:
Data were analyzed using TEM for size distribution, UV-Vis for SPR and catalytic kinetics (pseudo-first-order model), FT-IR for functional groups, XPS for elemental composition, XRD for crystal structure, TGA for thermal stability, and particle size analysis for swelling behavior.
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Transmission Electron Microscope
JEM-2100
JEOL
Observing morphology and size of composite materials
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Field-Emission Transmission Electron Microscope
Tecnai G2 F20
FEI
Examining energy-dispersive X-ray spectroscopy (EDS)
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X-ray Photoelectron Spectrometer
AXIS ULTRA
Kratos Analytical Ltd.
XPS measurements with monochromatic Al Kα X-ray source
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Ultraviolet-Visible Spectrophotometer
U-3900/3900H
Hitachi
Recording UV-Vis spectra with temperature controller
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Fourier Transform Infrared Spectrometer
Avatar 360
Nicolet
Recording infrared spectra using KBr pellet technique
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X-ray Diffractometer
D/Max-3C
Rigalcu
X-ray powder diffraction analysis
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Thermo-gravimetric Analyzer
Q50
TA
Thermo-gravimetric analyses under N2 atmosphere
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Laser Particle Analyzer
BI-90 Plus
Brooke
Measuring swelling behavior of composite microgels
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