scholarly journals FeCl3-Modified Carbonaceous Catalysts from Orange Peel for Solvent-Free Alpha-Pinene Oxidation

Materials ◽  
2021 ◽  
Vol 14 (24) ◽  
pp. 7729
Author(s):  
Adrianna Kamińska ◽  
Piotr Miądlicki ◽  
Karolina Kiełbasa ◽  
Jarosław Serafin ◽  
Joanna Sreńscek-Nazzal ◽  
...  

The work presents the synthesis of FeCl3-modified carbonaceous catalysts obtained from waste orange peel and their application in the oxidation of alpha-pinene in solvent-free reaction conditions. The use of waste orange peel as presented here (not described in the literature) is an effective and cheap way of managing this valuable and renewable biomass. FeCl3-modified carbonaceous materials were obtained by a two-stage method: in the first stage, activated carbon was obtained, and in the second stage, it was modified by FeCl3 in the presence of H3PO4 (three different molar ratios of these two compounds were used in the studies). The obtained FeCl3-modified carbon materials were subjected to detailed instrumental studies using the methods FT-IR (Fourier-transform Infrared Spectroscopy), XRD (X-ray Diffraction), SEM (Scanning Electron Microscope), EDXRF (Energy Dispersive X-ray Fluorescence) and XPS (X-ray Photoelectron Spectroscopy), while the textural properties of these materials were also studied, such as the specific surface area and total pore volume. Catalytic tests with the three modified activated carbons showed that the catalyst obtained with the participation of 6 M of FeCl3 and 3 M aqueous solutions of H3PO4 was the most active in the oxidation of alpha-pinene. Further tests (influence of temperature, amount of catalyst, and reaction time) with this catalyst made it possible to determine the most favorable conditions for conducting oxidation on this type of catalyst, and allowed study of the kinetics of this process. The most favorable conditions for the process were: temperature of 100 °C, catalyst content of 0.5 wt% and reaction time 120 min (very mild process conditions). The conversion of the organic raw material obtained under these conditions was 40 mol%, and the selectivity of the transformation to alpha-pinene oxide reached the value of 35 mol%. In addition to the epoxy compound, other valuable products, such as verbenone and verbenol, were formed while carrying out the process.

2021 ◽  
Vol 23 (2) ◽  
pp. 73-80
Author(s):  
Adrianna Kamińska ◽  
Nikola Maciejewska ◽  
Piotr Miądlicki ◽  
Karolina Kiełbasa ◽  
Joanna Sreńscek-Nazzal ◽  
...  

Abstract The presented work describes the autoxidation of alpha-pinene for the first time using a catalyst based on activated carbon from biomass with introduced Fe. The raw material for the preparation of the carbon material was waste orange peel, which was activated with a KOH solution. The following instrumental methods characterized the obtained catalyst (Fe/O_AC):N2 adsorption at 77 K, XRD, UV, SEM, TEM, X-ray microanalysis, and catalytic studies. It was shown that the Fe/O_AC catalyst was very active in the autoxidation of alpha-pinene. The main reaction products were: alpha-pinene oxide, verbenone, verbenol, and campholenic aldehyde.


Author(s):  
Anna Fajdek-Bieda ◽  
Agnieszka Wróblewska ◽  
Piotr Miądlicki ◽  
Jadwiga Tołpa ◽  
Beata Michalkiewicz

AbstractThis work presented the studies with the natural zeolite—clinoptilolite as the catalyst for the isomerization of geraniol. During the research, it turned out that the studied process is much more complicated, and not only isomerization takes place in it, but also dehydration, oxidation, dimerization, cyclization and fragmentation of the carbon chain. Geraniol is an organic raw material which can be obtained not only by a chemical synthesis but also from plants (renewable biomass) by distillation or extraction method, for example a source of geraniol can be a plant—geranium. Before catalytic tests clinoptilolite was characterized by the instrumental methods, such as: XRD, porosity studies—nitrogen adsorption at 77 K, SEM, EDXRF, and FT-IR. Gas chromatography analyses showed that the main products of geraniol isomerization process were 6,11-dimethyl-2,6,10-dodecatrien-1-ol and thumbergol. The selectivity of 6,11-dimethyl-2,6,10-dodecatrien-1-ol and thumbergol depended on the temperature, catalyst content and reaction time. These parameters were changed in the following ranges: 80–150 °C (temperature), 5–15 wt% (catalyst content) and 15–1440 min. (reaction time). The most favorable conditions for 6,11-dimethyl-2,6,10-dodecatrien-1-ol and thumbergol obtaining were: temperature 140 ºC, catalyst content 12.5 wt% and reaction time 180 min. At these conditions, the conversion of geraniol amounted to 98 mol%, and the selectivities of 6,11-dimethyl-2,6,10-dodecatrien-1-ol and thumbergol amounted to 14 and 47 mol%, respectively.


Energies ◽  
2021 ◽  
Vol 14 (15) ◽  
pp. 4483
Author(s):  
Yuyingnan Liu ◽  
Xinrui Xu ◽  
Bin Qu ◽  
Xiaofeng Liu ◽  
Weiming Yi ◽  
...  

In this study, corn cob was used as raw material and modified methods employing KOH and KMnO4 were used to prepare activated carbon with high adsorption capacity for mercury ions. Experiments on the effects of different influencing factors on the adsorption of mercury ions were undertaken. The results showed that when modified with KOH, the optimal adsorption time was 120 min, the optimum pH was 4; when modified with KMnO4, the optimal adsorption time was 60 min, the optimal pH was 3, and the optimal amount of adsorbent and the initial concentration were both 0.40 g/L and 100 mg/L under both modified conditions. The adsorption process conforms to the pseudo-second-order kinetic model and Langmuir model. Scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM-EDS), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and Zeta potential characterization results showed that the adsorption process is mainly physical adsorption, surface complexation and ion exchange.


Reactions ◽  
2021 ◽  
Vol 2 (4) ◽  
pp. 457-472
Author(s):  
Jasmine Kaur ◽  
Sundaramurthy Vedachalam ◽  
Philip Boahene ◽  
Ajay K. Dalai

Pyrolysis oil derived from waste tires consists of sulfur content in the range of 7000 to 9000 ppm. For use in diesel engines, its sulfur content must be lowered to 10 to 15 ppm. Though conventional hydrodesulfurization is suitable for the removal of sulfur from tire pyrolysis oil, its high cost provides an avenue for alternative desulfurization technologies to be explored. In this study, oxidative desulfurization (ODS), a low-cost technology, was explored for the desulfurization of tire pyrolysis oil. Two categories of titanium-incorporated mesoporous supports with 20 wt% loaded heteropoly molybdic acid catalyst (HPMo/Ti-Al2O3 and HPMo/Ti-TUD-1) were developed and tested for ODS of tire pyrolysis oil at mild process conditions. Catalysts were characterized by X-ray diffraction, BET-N2 physisorption, and X-ray photoelectron spectroscopy (XPS). The incorporation of Ti into Al2O3 and TUD-1 frameworks was confirmed by XPS. The surface acidity of catalysts was studied by the temperature-programmed desorption of NH3 and pyridine FTIR analyses. HPMo/Ti-Al2O3 and HPMo/Ti-TUD-1 catalysts contained both Lewis and Brønsted acid sites. The presence of titanium in catalysts was found to promote the ODS activity of phosphomolybdic acid. The Ti-TUD-1-supported catalysts performed better than the Ti-Al2O3-supported catalysts for the ODS of tire pyrolysis oil. Hydrogen peroxide and cumene peroxide were found to be better oxidants than tert-butyl hydroperoxide for oxidizing sulfur compounds of tire pyrolysis oil. Process parameter optimization by the design of experiments was conducted with an optimal catalyst along with the catalyst regeneration study. An ANOVA statistical analysis demonstrated that the oxidant/sulfur and catalyst/oil ratios were more significant than the reaction temperature for the ODS of tire pyrolysis oil. It followed the pseudo-first-order kinetics over HPMo/Ti-TUD-1.


2019 ◽  
Vol 6 (3) ◽  
pp. 238-247
Author(s):  
Swapnil R. Bankar

<P>Background: In recent years, green organic transformation has become a challenge for a chemist in areas like social sector, health, and environment. Literature survey revealed that a nano magnetite supported heterogeneous catalysis is an emergent field with huge application in chemical synthesis. </P><P> Objective: In the present article, the aim was to develop a simple and facile method to carry organic reaction under benign media. So, the focus was on the synthesis of nano-magnetite supported molybdenum catalyst and its application in β-enaminones synthesis. </P><P> Methods: Magnetically recyclable heterogeneous ferrite-molybdenum catalyst was prepared by simple impregnation method. The synthesized nanocatalyst Fe-Mo was well analysed by spectroscopic techniques like X-ray diffraction analysis, X-ray photoelectron spectroscopy, transmission electron microscopy, field-emission gun scanning electron microscopy and vibrating-sample magnetometry. The functionalized nanocatalyst Fe-Mo was employed in the synthesis of β-enaminones under solvent free condition. </P><P> Results: The competency of synthesized nanocatalyst-Fe-Mo was observed to be good for the synthesis of β-enaminones derivatives under microwave irradiation and gave excellent yield (86-96%) of the product. The catalyst was recycled for more than five consecutive runs without significant loss in its activity. </P><P> Conclusion: In the present research article, synthesis of highly active, magnetically recyclable Fe- Mo nanocatalyst was obtained from easily available precursor. The MNP was stable under investigated conditions and effective in β-enaminones synthesis. The simple eco-friendly method, low catalyst loading, short transformation time, and reusability of the catalyst thoroughly follow the sustainable protocol.</P>


2015 ◽  
Vol 659 ◽  
pp. 216-220 ◽  
Author(s):  
Achanai Buasri ◽  
Thaweethong Inkaew ◽  
Laorrut Kodephun ◽  
Wipada Yenying ◽  
Vorrada Loryuenyong

The use of waste materials for producing biodiesel via transesterification has been of recent interest. In this study, the pork bone was used as the raw materials for natural hydroxyapatite (NHAp) catalyst. The calcination of animal bone was conducted at 900 °C for 2 h. The raw material and the resulting heterogeneous catalyst were characterized using X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and the Brunauer-Emmett-Teller (BET) method. The effects of reaction time, microwave power, methanol/oil molar ratio, catalyst loading and reusability of catalyst were systematically investigated. The optimum conditions, which yielded a conversion of oil of nearly 94%, were reaction time 5 min and microwave power 800 W. The results indicated that the NHAp catalysts derived from pork bone showed good reusability and had high potential to be used as biodiesel production catalysts under microwave-assisted transesterification of Jatropha Curcas oil with methanol.


2013 ◽  
Vol 815 ◽  
pp. 317-320 ◽  
Author(s):  
Li Jing Min ◽  
Min Xing Zhao

[ObjectivTo study the extraction technology of flavonoids from orange peel in order to provide some theoretical guidance for the industrial production of flavonoids from orange peel. [Metho Taking orange peel as raw material, which was citrus fruit processing waste and the flavonoid yield as index, with ultrasonic assisted extraction, through single factor experiments and orthogonal tests to optimization of the extraction technology, obtain optimum process conditions of orange flavonoid by ultrasonic assisted extraction. [Result As for ultrasonic assisted extraction, the yield of orange flavonoid reached 9.6% under extraction conditions of extracting time 30 min, alcohol concentration 60%, sedimentation ratio 1:25.


2011 ◽  
Vol 287-290 ◽  
pp. 1735-1743 ◽  
Author(s):  
Yi Dong Shi ◽  
Qiong Guo ◽  
Yuan Song Xie

The C, N, S tri-doped TiO2 with high visible-light photo-catalysis effect was successfully prepared by mixing thiourea with the self-prepared TiO2 powder through calcining for 2h at 450°C. The TiO2 powder was obtained by homogeneous precipitation method using the metatitanic acid instead of expensive chemical reagents contained Ti as raw material. The effect of doping materials and methods on the photo-degradation rate of methylene blue and dyes was studied. The characterizations of the doped TiO2 were analyzed using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-visible absorption spectra (UV-vis). The results showed that this sample was the anatase TiO2 and contained elements C, N, S. The sample exhibited a significant response to ultraviolet and visible light. In the photo-degradation experiment, the C, N, S, tridoped-TiO2 could decolorize methylene blue and textile dyes quickly, and the photo-degradation rate of methylene blue could reach upward 98% after 3 hours under the different light sources.


2021 ◽  
Vol 4 (3) ◽  
pp. 234-244
Author(s):  
Amelia Olivas Sarabia ◽  
Marlene N Cardoza-Contreras ◽  
Gonzalo Lastra Medina ◽  
Marcos Alan Cota Leal ◽  
Selene Sepúlveda Guzmán

In this work, nanowires and nanorods of WOx have been synthesized by the solvothermal method. The effect of reaction time and acetic acid as solvent were studied. X-ray diffraction (XRD) patterns showed the monoclinic WO2.72, WO2.79, and orthorhombic WO3 crystalline structures. Scanning Electron Microscopy (SEM) and High-Resolution Transmission Electronic Microscopy (HRTEM) images presented nanostructures such as nanowires and nanorods at different sizes. Band gap energies were supplied by Ultra Violet visible (UV-vis) absorption spectra. The Photoluminescence (PL) spectra exhibited three emission peaks in the blue zone at 440, 460, and 484 nm. X-ray Photoelectron Spectroscopy (XPS) was used to calculate W6+, W5+, and W4+ oxidation states. The results showed that increasing the reaction time from 10 h to 24 h affected the crystalline structure from monoclinic to orthorhombic. Moreover, with the addition of acetic acid as solvent, the crystal structure is not affected but stabilizes the monoclinic phase in the course of time.


2019 ◽  
Vol 6 (2) ◽  
pp. 181116 ◽  
Author(s):  
Qian Kang ◽  
Yimin Zhang ◽  
Shenxu Bao ◽  
Guobin Zhang

VO 2 (B) has shown excellent cathode performance in lithium batteries and become a hot research topic in recent years. A stripped vanadium solution extracted from vanadium-bearing shale containing a high concentration of vanadium and certain amounts of impurities was used as a vanadium source to synthesize VO 2 (B) by hydrothermal process. The VO 2 conversion rate can reach as high as 99.47% in a reaction time of 8 h, and this is the highest result reported. The crystalline structure and morphology of the synthesized products were characterized by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). Furthermore, the electrochemical properties of VO 2 (B) in lithium-ion batteries were investigated. The results indicated that the VO 2 (B) has the initial specific discharge capacity of 192.0 mAh g −1 . Stripped vanadium solution is a raw material for producing V 2 O 5 and NH 4 VO 3 , which are indispensable vanadium sources in VO 2 synthesis. Therefore, synthesis of VO 2 via hydrothermal reduction by oxalic acid using stripped vanadium solution extracted from vanadium-bearing shale as a direct vanadium source is an eco-friendly, innovative and efficient method, and will have a great impact on VO 2 synthesis.


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