研究目的
Preparation of nano silver impregnated TiO2 catalyst using green synthesis for application in the oxidation of thiophene, and evaluation of its catalytic activity and kinetics.
研究成果
Green synthesis using Tulsi leaf extract successfully produced silver nanoparticles impregnated on TiO2, which acted as an effective catalyst for thiophene oxidation. The reaction followed second-order kinetics and was endothermic, with surface reaction as the rate-controlling step in the Langmuir-Hinshelwood model. Optimal conditions included 10 wt% silver loading, 1000 rpm stirring, and specific oxidant ratios. The catalyst could be reused and regenerated but with some loss in activity.
研究不足
The catalyst showed decreased surface area with increased silver loading and agglomeration at higher loadings, limiting dispersion and activity. Reusability studies indicated a drop in conversion after multiple uses without regeneration, and regeneration only partially restored activity. The study is limited to batch reactions and model fuel, not real fuels.
1:Experimental Design and Method Selection:
The study involved green synthesis of silver nanoparticles using Tulsi leaf extract as a reducing and stabilizing agent, impregnation on TiO2, and catalytic oxidation of thiophene using TBHP as oxidant. Kinetic models (pseudo-homogeneous and Langmuir-Hinshelwood) were applied.
2:Sample Selection and Data Sources:
Fresh Tulsi leaves were used for extract preparation. Thiophene, TBHP, isooctane, TiO2, and silver nitrate were procured from specified suppliers. Model fuel with 500 ppm sulfur concentration was used.
3:List of Experimental Equipment and Materials:
Equipment includes BET surface area analyzer (AS1 MP/Chemi-LP), XRF (Panalytical, Axios), XRD (Panalytical 3050/60), SEM (Zeol and Zeiss with Oxford EDS Detector), TEM (Tecnai G2), UV-Vis spectroscope (Shimadzu UV-1800), TPR (CHEMBET-3000), XPS (PHI 5000 spectrometer), HPLC (Perkin Elmer Series 200 with Agilent SB C-18 column), microwave for reduction, and batch reactor setup with water bath and stirrer. Materials include silver nitrate, TiO2, Tulsi leaves, thiophene, TBHP, isooctane, distilled water, alcohol for washing, and N-methyl-2-pyrrolidone for regeneration.
4:Experimental Procedures and Operational Workflow:
Tulsi leaf extract was prepared by boiling dried leaves in water, filtering, and cooling. Silver nanoparticles were synthesized by adding extract to silver nitrate solution, microwaving, and allowing formation. TiO2 was impregnated by stirring with the nanoparticle solution, filtering, washing, and drying. Catalysts were characterized using various techniques. Oxidation reactions were conducted in a batch reactor at controlled temperature and stirring speed, with samples taken at intervals for HPLC analysis. Parameters like metal loading, stirrer speed, oxidant ratio, catalyst weight, temperature, and initial thiophene concentration were varied. Reusability and regeneration studies were performed.
5:Data Analysis Methods:
Data were analyzed using kinetic models (first and second order, Langmuir-Hinshelwood), with rate constants determined from plots. Software like Polymath 5.1 was used for nonlinear regression. Statistical measures such as R2 values were used to assess model fit.
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XRF Spectroscope
Axios
Panalytical
Elemental analysis of catalysts
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XRD
3050/60
Panalytical
Crystal phase analysis
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UV-Vis spectroscope
UV-1800
Shimadzu
Absorption spectroscopy for nanoparticle confirmation
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HPLC
Series 200
Perkin Elmer
Analysis of reaction samples
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BET surface area analyzer
AS1 MP/Chemi-LP
USA
Characterization of catalyst surface area
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SEM
Zeol and Zeiss
Imaging and particle size distribution
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TEM
Tecnai G2
Transmission electron microscopy for nanoparticle imaging
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TPR analyzer
CHEMBET-3000
Temperature programmed reduction for metal oxide estimation
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XPS spectrometer
PHI 5000
Surface characterization
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Microwave
Heating for bio-reduction of silver nitrate
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Batch reactor
Conducting oxidation reactions
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