This work describes the synthesis and characterization of a heterogeneous catalyst consisting of piperazine-functionalized reduced graphene oxide decorated with Fe3O4 nanoparticles ( Fe3O4@rGO-NH), and the study of its catalytic activity as a magnetic heterogeneous catalyst for the Pechmann synthesis of coumarins. Catalyst Fe3O4@ rGO-NH was fully characterized by various techniques, including IR, XRD, TEM, VSM, TGA, and elemental analysis. Then, the catalyst was used as an efficient and easy-separable heterogeneous catalyst for the solvent-free synthesis of some coumarins by Pechmann reaction. The reaction was optimized in terms of reaction time and temperature, catalyst dosage, and the presence/absence of the solvent. Finally, the reusability of the catalyst was studied.

This study focused on the development of Fe–Co/kaolin catalyst by a wet impregnation method. Response surface methodology was used to study the influence of operating variables such as drying temperature, drying time, mass of support and stirring speed on the yield of the catalyst. The catalyst composite at best synthesis conditions was then calcined in an oven at varied temperature and time using 22 factorial design of experiment. The catalyst with optimum surface area was then utilized to grow carbon nanofiber (CNF) in a chemical vapour deposition (CVD) reactor. Both the catalyst and CNF were characterized using high-resolution scanning electron microscopy, high-resolution transmission electron microscopy, thermogravimetric analysis (TGA), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy. On the influence of operating variables on the yield of catalyst, the results showed that an optimum yield of 96.51% catalyst was obtained at the following operating conditions: drying time (10 h), drying temperature (110 °C), stirring speed (100 rpm) and mass of support (9 g). Statistical analysis revealed the existence of significant interactive effects of the variables on the yield of the catalyst. The HRSEM/XRD/BET/TGA analysis revealed that the particles are well dispersed on the support, with high surface area (376.5 m2/g) and thermally stable (330.88 °C). The influence of operating parameters on the yield of CNF was also investigated and the results revealed an optimum yield of 348% CNF at the following operating conditions: reaction temperature (600 °C), reaction time (40 min), argon flow rate (1416 mL/min) and acetylene/hydrogen flow rate (1416 mL/ min). It was found from statistical analysis that the reaction temperature and acetylene/hydrogen flow rates exerted significant effect on the CNF yield than the other factors. The contour and surface plots bi-factor interaction indicated functional relationship between the response and the experimental factors. The characterization results showed that the synthesized CNF is thermally stable, twisted and highly crystalline and contain surface functional groups. It can be inferred from the results of various analyses that the developed catalyst is suitable for CNF growth in a CVD reactor.

본 연구에서는 배가스 내 존재하는 오염물질인 NO의 처리효율을 증대시키기 위하여 NO 산화 공정을 연구하였으며, 강력한 산화력의 건식산화제를 제조하는 방법으로 H2O2 촉매분해가 도입되었다. H2O2 분해공정 상에서 적용 가능한 K-Mn/Fe2O3 불균일계 촉매가 제조되었으며, 이들이 가지는 물리화학 적 특성이 H2O2 분해반응에 미치는 영향이 조사되었다. 제조된 건식산화제는 NO가 포함된 모사 배가스를 처리하기 위한 NO 산화공정에 적용되었으며, 다양한 모사 배가스의 유량(5, 10, 20 L/min)에서 약 100% 가까운 NO 전환율을 확인 하였다.

In this study, Fe-Ni bimetallic catalyst supported on kaolin is prepared by a wet impregnation method. The effects of mass of kaolin support, pre-calcination time, pre-calcination temperature and stirring speed on catalyst yields are examined. Then, the optimal supported Fe-Ni catalyst is utilised to produce multi-walled carbon nanotubes (MWCNTs) using catalytic chemical vapour deposition (CCVD) method. The catalysts and MWCNTs prepared using the optimal conditions are characterized using high resolution transmission electron microscope (HRTEM), high-resolution scanning electron microscope (HRSEM), electron diffraction spectrometer (EDS), selected area electron diffraction (SAED), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET), and X-ray diffraction (XRD). The XRD/EDS patterns of the prepared catalyst confirm the formation of a purely crystalline ternary oxide (NiFe2O4). The statistical analysis of the variance demonstrates that the combined effects of the reaction temperature and acetylene flow rate predominantly influenced the MWCNT yield. The N2 adsorption (BET) and TGA analyses reveal high surface areas and thermally stable MWCNTs. The HRTEM/HRSEM micrographs confirm the formation of tangled MWCNTs with a particle size of less than 62 nm. The XRD patterns of the MWCNTs reveal the formation of a typical graphitized carbon. This study establishes the production of MWCNTs from a bi-metallic catalyst supported on kaolin.

The sol-gel technique has been studied to fabricate a homogeneous Fe-Mo/MgO catalyst. Ambient effects (air, Ar, and H2) on thermal decomposition of the citrate precursor have been systematically investigated to fabricate an Fe-Mo/MgO catalyst. Severe agglomeration of metal catalyst was observed under thermal decomposition of citrate precursor in air atmosphere. Ar/H2 atmosphere effectively restricted agglomeration of bimetallic catalyst and formation of highly-dispersed Fe-Mo/MgO catalyst with high specific surface-area due to the formation of Fe-Mo nanoclusters within MgO support. High-quality thin-multiwalled carbon nanotubes (t-MWCNTs) with uniform diameters were achieved on a large scale by catalytic decomposition of methane over Fe-Mo/MgO catalyst prepared under Ar-atmosphere. The produced t-MWCNTs had outer diameters in the range of 4-8 nm (average diameter ~6.6 nm) and wall numbers in the range of 4-7 graphenes. The as-synthesized t-MWCNTs showed product yields over 450% relative to the utilized Fe-Mo/MgO catalyst, and indicated a purity of about 85%.

The synthetic behaviors of carbon nanotubes (CNTs) by Fe/MgO catalysts were investigated in 0~90 wt.% range of MgO mixture ratios by catalytic chemical vapor deposition (CCVD) process. The CNTs were synthesized with 40 minutes of synthetic time, and 923 K of synthetic temperature using 0.1 L/min of ethylene gas and 1.0 L/min of hydrogen gas as synthetic and carrier gas, respectively. As the increase of synthetic temperatures and times, the diameters of CNTs become thicker. The carbon yield showed in a parabolic curve as MgO content increased and the maximum carbon yield was obtained at 30 wt.% of MgO. There were no obvious changes in the diameters of CNTs respect to the change of MgO content. Fe/MgO CNTs showed good crystalinity by High Resolution Transmission Electron microscope (HR-TEM) analysis. The behaviors of Fe/MgO CNTs have a tendency of depending on synthetic time and temperature rather than MgO content.

The aim of this study is to evaluate the environmental impacts of recovery of valuable metals from the desulfurizing spent catalyst. Molybdenum, vanadium and nickel widely used in the area of catalysis. But the demand of these metals is full filled by industries. Every year, more than 18,000 tons spent catalysts are discarded. In most countries, spent catalyst is classified as a harmful waste. Thus, metal recovery from spent catalyst has been processed. The recovery process of molybdenum, vanadium and nickel from spent catalyst was mainly carried out wet process. However, this process are not suitable for economics and environmental aspects. Because environmental costs for removal of sulfur in the spent catalyst is high and huge amount of industrial wastewater occurs. Thus, it is necessary to develop a process which is efficient and does not cause pollution than the wet process. Thus, we have studied life cycle assessment about the dry process for the recovery of valuable metals.