Effect of calcination temperature on properties of waste alkaline battery-based catalysts for deep oxidation of toluene and o-xylene

2020 ◽  
pp. 0958305X2093255
Author(s):  
Young-Kwon Park ◽  
Min Ki Kim ◽  
Sang Chul Jung ◽  
Wang Geun Shim ◽  
Seong Ho Jang ◽  
...  

To evaluate waste alkaline battery (WB) as a catalyst for deep oxidation of toluene and o-xylene, we investigated how calcination temperature influenced the catalytic activity of WB-based catalyst for catalyst preparation. Physicochemical properties of WB-based catalysts were characterized by BET (Brunauer Emmett Teller) analysis, XRD (X-ray diffraction), SEM/EDX (scanning electron microscope/energy dispersive X-ray), TGA/DTA (thermo gravimetric analysis/differential thermal analysis), and H2-TPR (hydrogen temperature programmed reduction). Major elements of WB-based catalysts were carbon, manganese, zinc, and iron. The catalytic activity of WB-based catalyst was significantly influenced by calcination temperatures ranging from 300 °C–600°C. An increase calcination temperature resulted in a significant decrease in the BET surface area and concentrations of surface carbon and chlorine of the WB-based catalyst, while levels of other components increased. The average pore diameter of the WB-based catalyst calcined at 400 °C (WB (400) catalyst) was the smallest. The concentrations of manganese and iron in WB (400) catalyst were the highest, while those of manganese and iron in the WB-based catalyst calcined at 300 °C (WB (300) catalyst) were the lowest. Therefore, a good performance of WB (400) catalyst was likely due to its higher concentrations of manganese and iron and smaller pore size. When GHSV (gas hourly space velocity) was 40,000 h−1, toluene and o-xylene were completely oxidized on WB (400) catalyst at 430 °C and 440 °C, respectively.

2015 ◽  
Vol 1112 ◽  
pp. 489-492
Author(s):  
Ali Mufid ◽  
M. Zainuri

This research aims to form particles of hematite (α-Fe2O3) with a basis of mineral iron ore Fe3O4 from Tanah Laut. Magnetite Fe3O4 was synthesized using co-precipitation method. Further characterization using X-ray fluorescence (XRF) to obtain the percentage of the elements, obtained an iron content of 98.51%. Then characterized using thermo-gravimetric analysis and differential scanning calorimetry (TGA-DSC) to determine the calcination temperature, that at a temperature of 445 °C mass decreased by 0.369% due to increase in temperature. Further Characterization of X-ray diffraction (XRD) to determine the phases formed at the calcination temperature variation of 400 °C, 445 °C, 500 °C and 600 °C with a holding time of 5 hours to form a single phase α-Fe2O3 hematite. Testing with a particle size analyzer (PSA) to determine the particle size distribution, where test results indicate that the α-Fe2O3 phase of each having a particle size of 269.7 nm, 332.2 nm, 357.9 nm, 412.2 nm. The best quantity is shown at a temperature of 500 °C to form the hematite phase. This result is used as the calcination procedure to obtain a source of Fe ions in the manufacture of Lithium Ferro Phosphate.


2021 ◽  
Author(s):  
Zohreh Razmara

Abstract A 2D heterometallic copper(II)–sodium(I) complex based on pyridine 2,6-dicarboxylato (dipic2-) formulated as [Cu(μ-dipic)2{Na2(µ-H2O)4}]n. 2nH2O (1) has been synthesized. Thermal stability of complex 1 was studied by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA). Single-crystal X-ray diffraction (SC-XRD) analysis showed that the parallelepiped colorless crystal of complex 1 crystallizes in a monoclinic system with the space group P2/c . A highly dispersed truncated octahedral catalyst formulated as Cu-Na/Al2O3 (CNM) was prepared by thermal decomposition of complex 1. Besides, the reference catalyst of Cu-Na/Al2O3 (CNR) was prepared by impregnation conventional method. The catalysts were examined by FT-IR, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer–Emmett–Teller (BET) surface area, and subjected to water-gas shift (WGS) reaction in the temperature range of 150-400 °C. The catalysts showed strong surface structure-activity dependence in WGS reaction. Improved catalytic performance during the water-gas shift reaction was observed for CNM compared to CNR due to its high dispersion, smaller particle size, and higher BET specific surface area.


2020 ◽  
Vol 58 (7) ◽  
pp. 495-500
Author(s):  
Young Min Jin ◽  
Joon Hyuk Lee ◽  
Sang Sun Choi

This study examined the effect of alkalis on lyocell-based activated carbon fibres (ACFs) with high Brunauer-Emmett-Teller (BET) surface areas, using X-ray diffraction (XRD). Here, alkali treatments were conducted using 10 ~ 25 % NaOH and KOH on lyocell samples for 3 h at ambient room temperature. A secondary treatment with 4 % each of KOH and H3PO4 for an additional 3 h followed. An activated form of the samples was prepared by oxidation (stabilisation), carbonisation, and activation. The final ACF form of the samples showed a porous structure with high BET surface areas (> 1,000 m<sup>2</sup> g<sup>-1</sup>). A 25 % dosage of NaOH produced the highest BET surface area compared to other samples. In terms of crystallinity, a 15 % dosage of KOH was found to be the optimum dosage to secure the highest degree of crystallinity among all samples. Meanwhile, the NaOH was successfully shifted the samples into the most distinct form of cellulose II. 15 % NaOH was found to secure the most stable thermal characteristics, as determined via thermo-gravimetric analysis. The present work demonstrates the various physio-chemistries of ACFs prepared with different proportions and types of alkalis, leading to intriguing potential applications.


2015 ◽  
Vol 1087 ◽  
pp. 30-34 ◽  
Author(s):  
KANAGESWARY SOCKALINGAM ◽  
Mohd Azha Yahya ◽  
Hasan Zuhudi Abdullah

Hydroxyapatite (HAp), classified as bioceramic materials is the major mineral constituent of vertebrate bones and teeth. In this study, the effect of temperature on isolation and characterization of HAp from tilapia fish scales have been investigated. Scales were subjected to heat treatment at different temperatures (800°C and 1000°C) and microstructure of both raw and calcined scales were observed under Scanning Electron Microscopy (SEM). Thermo Gravimetric Analysis (TGA) and Energy Dispersive X-Ray Spectroscopy (EDX) results have revealed the best calcination temperature of tilapia scales to be 800°C due to the calculated calcium to phosphorous weight ratio (Ca/P). The Ca/P ratio for scales treated at 800°C and 1000°C were 1.598 and 1.939 respectively. The phase purity and crystallinity of produced HAp was further confirmed by X-Ray Diffraction (XRD) analysis. Based on the study, it can be concluded that tilapia fish scale is a good natural source of HAp with 800°C as the optimum calcination temperature in HAp production.


Molekul ◽  
2016 ◽  
Vol 11 (1) ◽  
pp. 61
Author(s):  
Witri Wahyu Lestari ◽  
Joni Hartono ◽  
Marisa Adreane ◽  
Khoirina Dwi Nugrahaningtyas ◽  
Candra Purnawan ◽  
...  

Electro-synthesis of Metal-Organic Frameworks types of MIL-100(Fe) (MIL = Material Institute of Lavoisier) in ethanol: water (1: 1) with electrolyte TBATFB 0.1 M has been optimized by varying voltage (12, 13, 14 and 15 Volt) and temperature (room temperature, 40, 60 and 80 °C). The product showed light brown powder which upon activation becomes dark brown. Optimum condition achieved during use voltage of 15 Volts and at a temperature of 40 °C with 33% yield. The obtained material was characterized by XRD and compared to CCDC 640536 simulated patterns to confirm the phase purity of the product. As comparison hydrothermal and reflux method have been carried out. Characterization by FTIR has also undertaken to ensure the coordination between the metal cation (Fe3+) and the BTC ligand (BTC = 1,3,5-Benzene Tri Carboxylate). Meanwhile pore analysis using SAA confirmed that MIL-100(Fe) obtained by electrolysis method has a BET surface area reached till 569.191 m²/g with a total pore volume of 0.4540 cc/g and an average pore diameter reached 16 Å. Based on SEM analysis, morphology material show particle size between 0.4-8.6 μm and has a thermal stability up to 350 °C according thermo-gravimetric analysis. Due to the presence of Lewis acid sites on Fe-trimeric unit, porosity features on MIL-100(Fe) and a fairly high thermal stability, this material is potentially used as the host material for the catalyst in the conversion reactions model for green diesel production.


BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Arefeh Dehghani Tafti ◽  
Bi Bi Fatemeh Mirjalili ◽  
Abdolhamid Bamoniri ◽  
Naeimeh Salehi

AbstractNano-eggshell/Ti(IV) as a novel naturally based catalyst was prepared, characterized and applied for the synthesis of dihydropyrano[2,3-c]pyrazole derivatives. The characterization of nano-eggshell/Ti(IV) was performed using Fourier Transform Infrared spectroscopy, X-ray Diffraction, Field Emission Scanning Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and Thermo Gravimetric Analysis. Dihydropyrano[2,3-c]pyrazoles were synthesized in the presence of nano-eggshell/Ti(IV) via a four component reaction of aldehydes, ethyl acetoacetate, malononitrile and hydrazine hydrate at room temperature under solvent free conditions. The principal affairs of this procedure are mild condition, short reaction times, easy work-up, high yields, reusability of the catalyst and the absence of toxic organic solvents.


Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1712
Author(s):  
Appusamy Muthukrishnaraj ◽  
Salma Ahmed Al-Zahrani ◽  
Ahmed Al Otaibi ◽  
Semmedu Selvaraj Kalaivani ◽  
Ayyar Manikandan ◽  
...  

Towards the utilization of Cu2O nanomaterial for the degradation of industrial dye pollutants such as methylene blue and methyl orange, the graphene-incorporated Cu2O nanocomposites (GCC) were developed via a precipitation method. Using Hummers method, the grapheme oxide (GO) was initially synthesized. The varying weight percentages (1–4 wt %) of GO was incorporated along with the precipitation of Cu2O catalyst. Various characterization techniques such as Fourier-transform infra-red (FT-IR), X-ray diffraction (XRD), UV–visible diffused reflectance (UV-DRS), Raman spectroscopy, thermo gravimetric analysis (TGA), energy-dispersive X-ray analysis (EDX), and electro chemical impedance (EIS) were followed for characterization. The cabbage-like morphology of the developed Cu2O and its composites were ascertained from field-emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HR-TEM). In addition, the growth mechanism was also proposed. The results infer that 2 wt % GO-incorporated Cu2O composites shows the highest value of degradation efficiency (97.9% and 96.1%) for MB and MO at 160 and 220 min, respectively. Further, its catalytic performance over visible region (red shift) was also enhanced to an appreciable extent, when compared with that of other samples.


2017 ◽  
Vol 50 ◽  
pp. 18-31 ◽  
Author(s):  
Rudzani Sigwadi ◽  
Simon Dhlamini ◽  
Touhami Mokrani ◽  
Patrick Nonjola

The paper presents the synthesis and investigation of zirconium oxide (ZrO2) nanoparticles that were synthesised by precipitation method with the effects of the temperatures of reaction on the particles size, morphology, crystallite sizes and stability at high temperature. The reaction temperature effect on the particle size, morphology, crystallite sizes and stabilized a higher temperature (tetragonal and cubic) phases was studied. Thermal decomposition, band structure and functional groups were analyzed by Brunauer-Emmett-Teller (BET), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA) and Fourier transform infrared (FT-IR). The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR spectra showed the strong presence of ZrO2 nanoparticles.


Materials ◽  
2018 ◽  
Vol 11 (12) ◽  
pp. 2457 ◽  
Author(s):  
Haifeng Zhao ◽  
Jing Lv ◽  
Junshan Sang ◽  
Li Zhu ◽  
Peng Zheng ◽  
...  

In this work, a mixing-calcination method was developed to facilely construct MXene/CuO nanocomposite. CuO and MXene were first dispersed in ethanol with sufficient mixing. After solvent evaporation, the dried mixture was calcinated under argon to produce a MXene/CuO nanocomposite. As characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and X-ray photoelectron spectra (XPS), CuO nanoparticles (60–100 nm) were uniformly distributed on the surface and edge of MXene nanosheets. Furthermore, as evaluated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the high-temperature decomposition (HTD) temperature decrease of ammonium perchlorate (AP) upon addition of 1 wt% CuO (hybridized with 1 wt% MXene) was comparable with that of 2 wt% CuO alone, suggesting an enhanced catalytic activity of CuO on thermal decomposition of AP upon hybridization with MXene nanosheets. This strategy could be further applied to construct other MXene/transition metal oxide (MXene/TMO) composites with improved performance for various applications.


2015 ◽  
Vol 50 (1) ◽  
pp. 21-28 ◽  
Author(s):  
F Hassan ◽  
MS Miran ◽  
HA Simol ◽  
MAB H Susan ◽  
MYA Mollah

ZnO nanoparticles (NPs) with size less than 100 nm were successfully prepared by a hybrid electrochemical-thermal method using metallic zinc and NaHCO3 without the use of any zinc salt, template or surfactant. The NPs were characterized by Fourier transform infra-red (FT-IR) spectroscopy, UV-visible spectroscopy, photoluminescence spectroscopy (PL), thermo-gravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy. UV-visible spectral analysis indicated that the particle size increased with increasing calcination temperature. The band gap (3.91-3.83 eV) was higher for synthesized ZnO NPs than their bulk counterparts (3.37 eV). The FT-IR spectra at different calcination temperatures showed the characteristic band for ZnO at 450 cm-1 to be prominent with increasing temperature due to the conversion of precursor into ZnO. The wurtzite hexagonal phase was confirmed by XRD analyses for ZnO NPs calcined at 700oC. The green photoluminescent emission from ZnO NPs at different calcination temperatures is considered to be originated from the oxygen vacancy or interstitial related defects in ZnO. SEM images clearly showed that the NPs are granular and of almost uniform size when calcined at higher temperatures. EDX spectra further confirmed the elemental composition and purity of ZnO obtained on calcination at 700oC. The NPs are well dispersed near or above calcination temperature of 700oC.Bangladesh J. Sci. Ind. Res. 50(1), 21-28, 2015


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