研究目的
To examine the influence of various operating parameters, to exhibit the discoloration of the dye solution, and to identify, for the first time, the degradation products of sulfur black dye oxidized by photocatalysis.
研究成果
Cerium doping enhances the photocatalytic activity of TiO2 by reducing band gap energy and inhibiting electron-hole recombination. Optimal conditions (1% Ce-TiO2, [H2O2] = 2×10?2 M, pH=9.5, [dye]=200 ppm) achieved 92% color removal. LC/MS identified degradation products, proposing a novel pathway for sulfur black dye degradation, providing an effective method for textile wastewater treatment.
研究不足
The study is limited to UV irradiation and specific experimental conditions; it may not be directly applicable to visible light or other pollutants. The identification of all degradation intermediates was not complete, and some could not be determined due to rapid oxidation.
1:Experimental Design and Method Selection:
The study involved synthesizing TiO2 and Ce-TiO2 photocatalysts via sol–gel method, characterizing them using XRD, Raman spectroscopy, BET surface area analysis, TEM, EDX, H2-TPR, UV-visible diffuse reflectance, and PL spectroscopy. Photocatalytic degradation experiments were conducted under UV light with H2O2, and degradation products were identified using LC/MS.
2:Sample Selection and Data Sources:
Sulfur black dye was purchased from Clariant. Aqueous solutions of the dye at various concentrations (50-400 ppm) were used.
3:List of Experimental Equipment and Materials:
Equipment includes autoclave (Equilabo), XPERT-PRO diffractometer, DILOR RTI 30 Raman spectrometer, MICROMERITICS ASAP 2020 surface area analyzer, Tecnai G20 UltraTwin TEM, ThermoFinnigan 1100 TPD/R/O gas chromatograph, Perkin-Elmer UV-visible spectrometer, Perkin-Elmer Lambda S55 spectrofluorometer, UV lamp (Apelex, VL-15C), SHIMADZU UV-1800 spectrophotometer, Agilent 1100 LC/MS, and centrifuge. Materials include titanium(IV) isopropoxide, cerium(III) nitrate hexahydrate, ethanol, ethylacetoacetate, nitric acid, hydrogen peroxide, and sulfur black dye.
4:Experimental Procedures and Operational Workflow:
Photocatalysts were synthesized via sol–gel, calcined, and characterized. For photocatalytic experiments, catalyst was dispersed in dye solution, stirred in dark for 30 min, irradiated with UV light, samples withdrawn at intervals, centrifuged, and analyzed by spectrophotometry and LC/MS.
5:Data Analysis Methods:
Color removal percentage calculated from absorbance measurements. Degradation products identified by interpreting mass spectra from LC/MS.
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X-ray diffractometer
XPERT-PRO
PANalytical
Used to determine the crystallographic structure of synthesized catalysts.
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transmission electron microscope
Tecnai G20 UltraTwin
FEI
Used to investigate surface morphology and chemical composition of powders.
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gas chromatograph
ThermoFinnigan 1100 TPD/R/O
Thermo Fisher Scientific
Used for H2-TPR experiments to check H2 consumption.
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UV-visible spectrometer
Perkin-Elmer Instrument with RSA-PE-20 integrating sphere
PerkinElmer
Used to obtain UV-visible diffuse reflectance spectra.
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spectrofluorometer
Perkin-Elmer Lambda S55 (LS55)
PerkinElmer
Used for photoluminescence spectroscopy.
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spectrophotometer
SHIMADZU UV-1800
Shimadzu
Used to follow the evolution of photocatalytic reaction by UV-visible spectrophotometry.
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LC/MS instrument
Agilent 1100
Agilent
Used for identification of degradation products by liquid chromatography coupled with mass spectrometry.
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autoclave
Equilabo
Equilabo
Used for heating gels under supercritical conditions to drive off volatile components during photocatalyst synthesis.
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Raman spectrometer
DILOR RTI 30
DILOR
Used for Raman spectroscopy analysis to define materials lattice structure.
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surface area analyzer
MICROMERITICS ASAP 2020
Micromeritics
Used to measure surface areas of catalysts via BET theory.
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UV lamp
VL-15C
Apelex
Used as radiation source for photocatalytic experiments.
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centrifuge
Used to centrifuge samples to remove suspended catalyst particles.
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