Search results for: sulfuric%20acid

Authors: M. Unis, S. Turky, A. Elalem, A. Meshrghi

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The Esterification kinetics of acetic acid with isopropnol in the presence of sulfuric acid as a homogenous catalyst was studied with isothermal batch experiments at 60,70 and 80°C and at a different molar ratio of isopropnol to acetic acid. Investigation of kinetics of the reaction indicated that the low of molar ratio is favored for esterification reaction, this is due to the reaction is catalyzed by acid. The maximum conversion, approximately 60.6% was obtained at 80°C for molar ratio of 1:3 acid : alcohol. It was found that increasing temperature of the reaction, increases the rate constant and conversion at a certain mole ratio, that is due to the esterification is exothermic. The homogenous reaction has been described with simple power-law model. The chemical equilibrium combustion calculated from the kinetic model in agreement with the measured chemical equilibrium.

Keywords: artificial flavors, esterification, chemical equilibria, isothermal

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Authors: H. Hajmohammadi , A. H. Jafari, M. Eskandari Nasab

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The ion exchange method was used to assess the absorption of sulfate media from laboratory-grade materials. The Taguchi method was employed for determining the optimum conditions for scandium adsorption. Results show that optimum conditions for scandium adsorption from sulfate were obtained by Purolite C100 cationic resin in 0.1 g/l sulfuric acid and scandium concentration of 2 g/l at 25 °C. Studies also showed that lowering H₂SO₄ concentration and aqueous phase temperature leads to an increase in Sc adsorption. Visual Minteq software was used to ascertain the various possible cation types and the effect of concentration of scandium ion species on scandium adsorption by cationic resins. The simulation results of the above software show that scandium ion species are often cationic species that are consistent with experimental data.

Keywords: scandium, ion exchange resin, simulation, leach copper

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Authors: Gulmira Zhakupova, Tamara Tultabayeva, Aknur Muldasheva, Assem Sagandyk

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The development of technology and production of products with increased biological value based on the use of natural food raw materials are important tasks in the policy of the food market of the Republic of Kazakhstan. For Kazakhstan, livestock farming, in particular sheep farming, is the most ancient and developed industry and way of life. The history of the Kazakh people is largely connected with this type of agricultural production, with established traditions using dairy products from sheep's milk. Therefore, the development of new technologies from sheep’s milk remains relevant. In addition, one of the most promising areas for the development of food technology for therapeutic and prophylactic purposes is sheep milk products as a source of protein, immunoglobulins, minerals, vitamins, and other biologically active compounds. This article presents the results of research on the study of milk processing technology. The objective of the study is to study the possibilities of processing sheep milk and its role in human nutrition, as well as the results of research to improve the technology of sheep milk products. The studies were carried out on the basis of sanitary and hygienic requirements for dairy products in accordance with the following test methods. To perform microbiological analysis, we used the method for identifying Salmonella bacteria (Horizontal method for identifying, counting, and serotyping Salmonella) in a certain mass or volume of product. Nutritional value is a complex of properties of food products that meet human physiological needs for energy and basic nutrients. The protein mass fraction was determined by the Kjeldahl method. This method is based on the mineralization of a milk sample with concentrated sulfuric acid in the presence of an oxidizing agent, an inert salt - potassium sulfate, and a catalyst - copper sulfate. In this case, the amino groups of the protein are converted into ammonium sulfate dissolved in sulfuric acid. The vitamin composition was determined by HPLC. To determine the content of mineral substances in the studied samples, the method of atomic absorption spectrophotometry was used. The study identified the technological parameters of sheep milk products and determined the prospects for researching sheep milk products. Microbiological studies were used to determine the safety of the study product. According to the results of the microbiological analysis, no deviations from the norm were identified. This means high safety of the products under study. In terms of nutritional value, the resulting products are high in protein. Data on the positive content of amino acids were also obtained. The results obtained will be used in the food industry and will serve as recommendations for manufacturers.

Keywords: dairy, milk processing, nutrition, colostrum

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Authors: N. Hasbullah, K. A. Sekak

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The sulfonated poly (ether ether ketone) SPEEK nanofiber membrane were successfully electrospun for Polymer Electrolyte Membrane (PEM) in Proton Exchange Membrane Fuel Cell (PEMFC) and their nanosized properties were investigated. The poly (ether ether ketone) PEEK victrex® grade 90p was sulfonated with concentrated sulfuric acid (95-98% w/w) at room temperature for 60 hours sulfonation times. The degree sulfonation of SPEEK are 70% was determined by H1 NMR and the functional groups of the SPEEK were characterize using FTIR. Then, the SPEEK nanofiber membrane were prepared via electrospinning method using DMAC as a solvent. The SPEEK sample were successfully electrospun using predetermine set up. FESEM show the electrospun fiber mat surface and confirmed the nanostructure membrane cell.

Keywords: polymer electrolyte membrane (PEM), sulfonated poly (ether ether ketone) (SPEEK), degree sulfonation, Electrospinning, Nanofibers

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Authors: Mustafa Ümi̇t Ünal, Nafi̇z Çeli̇ktaş, Aysun Şener, Sara Betül Dolgun, Duygu Keser

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The aim of this study was to compare acid and base pretreatment of switchgrass for bioethanol production. Switchgrass was pretreated with sulfuric acid and sodium hydroxide at 0.5, 1.0 and 1.5% (v/v) at 120, 140, 180 °C for 10, 60 and 90. Optimization of enzymatic hydrolysis of the pretreated switchgrass samples were carried out using three different enzyme mixtures (22.5 mg cellulase and 75 mg cellobiase /g biomass; 45 mg cellulase and 150 mg cellobiase /g biomass; 90 mg cellulase and 300 mg cellobiase /g biomass). Samples were removed at 24-h interval for fermentable sugar analyses with HPLC. The results showed that use of 90 mg cellulase and 300 mg cellobiase/g biomass resulted in the highest fermentable sugar formation. Furthermore, the highest fermentable sugar yield was obtained by pretreatment at 120 °C for 10 min using 1.0 % sodium hydroxide.

Keywords: switchgrass, acid pretreatment, enzymatic hydrolysis, base pretreatment, ethanol production

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Authors: Sina Aghili, Ali Arasteh Nodeh

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Tamarisk usage as a new group of lignocelluloses material to produce fermentable sugars in bio-ethanol process was studied. The overall aim of this work was to establish the optimum condition for acid hydrolysis of this new material and a mathematical model predicting glucose release as a function of operation variable. Sulfuric acid concentration in the range of 20 to 60%(w/w), process temperature between 60 to 95oC, hydrolysis time from 120 to 240 min and solid content 5,10,15%(w/w) were used as hydrolysis conditions. HPLC was used to analysis of the product. This analysis indicated that glucose was the main fermentable sugar and was increased with time, temperature and solid content and acid concentration was a parabola influence in glucose production.The process was modeled by a quadratic equation. Curve study and model were found that 42% acid concentration, 15 % solid content and 90oC were in optimum condition.

Keywords: fermentable sugar, saccharification, wood, hydrolysis

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Authors: Saba Pajuhan, Afshin Farahbakhsh, S. M. M. Dastgheib

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Biosurfactants and bioemulsifiers are a structurally diverse group of surface-active molecules synthesized by microorganisms, they are amphipathic molecules which reduce surface and interfacial tensions and widely used in pharmaceutical, cosmetic, food and petroleum industries. In this paper, several methods of bioemulsifer synthesis and purification by Bacillus licheniformis strains (namely ACO1, PTCC 1595 and ACO4) were investigated. Strains were grown in nutrient broth with different conditions in order to get maximum production of bioemulsifer. The purification of bio emulsifier and the quality evaluation of the product was done by adding sulfuric acid (H₂SO₄) (98%), Ethanol or HCl to the solution followed by centrifuging. To determine the optimal conditions yielding the highest bioemulsifier production, the effect of various carbon and nitrogen sources, temperature, NaCl concentration, pH, O₂ levels, incubation time are indispensable and all of them were highly effective in bioemulsifiers production.

Keywords: biosurfactant, bioemulsifier, purification, surface tension, interfacial tension

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Authors: Damien Rinsant, Eugen Andreiadis, Michael Carboni, Daniel Meyer

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Different types of materials have been developed for the solid/liquid uranium extraction processes, such as functionalized organic polymers, hybrid silica or inorganic adsorbents. In general, these materials exhibit a moderate affinity for uranyl ions and poor selectivity against impurities like iron, vanadium or molybdenum. Moreover, the structural organization deficiency of these materials generates ion diffusion issues inside the material. Therefore, the aim of our study is to developed efficient and organized materials, stable in the acid media encountered in uranium extraction processes. Metal organic frameworks (MOFs) are hybrid crystalline materials consisting of an inorganic part (cluster or metal ions) and tailored organic linkers connected via coordination bonds. These hierarchical materials have exceptional surface area, thermal stability and a large variety of tunable structures. However, due to the reversibility of constitutive coordination bonds, MOFs have moderate stability in strongly complexing or acidic media. Only few of them are known to be stable in aqueous media and only one example is described in strong acidic media. However, these conditions are very often encountered in the environmental pollution remediation of mine wastewaters. To tackle the challenge of developing MOFs adapted for uranium extraction from acid mine waters, we have investigated the stability of several materials. To ensure a good stability we have synthetized and characterized different materials based on highly coordinated metal clusters, such as LnOFs and Zirconium based materials. Among the latter, the UiO family shows a great stability in sulfuric acid media even in the presence of 1.4 M sodium sulfate at pH 2. However, the stability in phosphoric media is reduced due to the high affinity between zirconium and phosphate ligand. Based on these results, we have developed a tertiary amine functionalized MOF denoted UiO-68-NMe2 particularly adapted for the extraction of anionic uranyl (VI) sulfate complexes mainly present in the acid mine solutions. The adsorption capacity of the material has been determined upon varying total sulfate concentration, contact time and uranium concentration. The extraction tests put in evidence different phenomena due to the complexity of the extraction media and the interaction between the MOF and sulfate anion. Finally, the extraction mechanisms and the interaction between uranyl and the MOF structure have been investigated. The functionalized material UiO-68-NMe2 has been characterized in the presence and absence of uranium by FT-IR, UV and Raman techniques. Moreover, the stability of the protonated amino functionalized MOF has been evaluated. The synthesis, characterization and evaluation of this type of hybrid material, particularly adapted for uranium extraction in sulfuric acid media by an anionic exchange mechanism, paved the way for the development of metal organic frameworks functionalized by different other chelating motifs, such as bifunctional ligands showing an enhanced affinity and selectivity for uranium in acid and complexing media. Work in this direction is currently in progress.

Keywords: extraction, MOF, ligand, uranium

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Authors: Farid Amidi-Fazli

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Problems and disadvantages of using conventional plastics are more apparent in recent years and have attracted researchers' attention. Polymers from natural resources or bio polymers represent a suitable replacement to overcome to the disadvantages of plastics. But due to the some flaws of bio polymers, using suitable filler almost seems necessary. Nanocrystalline cellulose with low cost and availability can be applied as appropriate filler. In this study nanocrystalline cellulose was produced from cotton Linter and was characterized. The cotton Linter was hydrolyzed in sulfuric acid then neutralized by the two different concentrations of NaOH. The resulted suspension was treated by ultrasound waves. Process efficiency was determined as 90%. The final product was studied using scanning electron microscopy and x-ray diffraction technique. The obtained diagram of XRD experiment confirmed that the produced material was nanocrystalline cellulose. Also percentage of crystallinity was calculated as 84% in the obtained material as well as the size of crystals. It can be said that the applied method is a rapid and easy method for the production of nanocrystalline cellulose.

Keywords: nanocrystalline cellulose, crystallinity, XRD, cotton linter

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Authors: Samira Gharehkhani, Seyed Farid Seyed Shirazi, Abdolreza Gharehkhani, Hooman Yarmand, Ahmad Badarudin, Rushdan Ibrahim, Salim Newaz Kazi

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Nanocrystalline cellulose (NCC) were prepared by acid hydrolysis and ultrasound treatment of bleached Acacia mangium fibers. The obtained rod-shaped nanocrystals showed a uniform size. The results showed that NCC with high crystallinity can be obtained using 64 wt% sulfuric acid. The effect of synthesis condition was investigated. Different reaction times were examined to produce the NCC and the results revealed that an optimum reaction time has to be used for preparing the NCC. Morphological investigation was performed using the transmission electron microscopy (TEM). Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA) were performed. X-ray diffraction (XRD) analysis revealed that the crystallinity increased with successive treatments. The NCC suspension was homogeneous and stable and no sedimentation was observed for a long time.

Keywords: acid hydrolysis, nanocrystalline cellulose, nano material, reaction time

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Authors: Fang Lian, Zefang Chenli, Laijun Ma, Lei Mao

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Up to now, electrolytic process is a popular way to prepare Mn and MnO2 (EMD) with high purity. However, the conventional preparation process of manganese oxide such as Mn3O4 with high purity from electrolytic manganese metal is characterized by long production-cycle, high-pollution discharge and high energy consumption especially initially from low-grade rhodochrosite, the main resources for exploitation and applications in China. Moreover, Mn3O4 prepared from electrolytic manganese shows large particles, single morphology beyond the control and weak chemical activity. On the other hand, hydrometallurgical method combined with thermal decomposition, hydrothermal synthesis and sol-gel processes has been widely studied because of its high efficiency, low consumption and low cost. But the key problem in direct preparation of manganese oxide series from low-grade rhodochrosite is to remove completely the multiple impurities such as iron, silicon, calcium and magnesium. It is urgent to develop a sustainable approach to high pure manganese oxide series with character of short process, high efficiency, environmentally friendly and economical benefit. In our work, the preparation technique of high pure Mn3O4 directly from low-grade rhodochrosite ore (13.86%) was studied and improved intensively, including the effective leaching process and the short purifying process. Based on the same ion effect, the repeated leaching of rhodochrosite with sulfuric acid is proposed to improve the solubility of Mn2+ and inhibit the dissolution of the impurities Ca2+ and Mg2+. Moreover, the repeated leaching process could make full use of sulfuric acid and lower the cost of the raw material. With the aid of theoretical calculation, Ba(OH)2 was chosen to adjust the pH value of manganese sulfate solution and BaF2 to remove Ca2+ and Mg2+ completely in the process of purifying. Herein, the recovery ratio of manganese and removal ratio of the impurity were evaluated via chemical titration and ICP analysis, respectively. Comparison between conventional preparation technique from electrolytic manganese and a sustainable approach directly from low-grade rhodochrosite have also been done herein. The results demonstrate that the extraction ratio and the recovery ratio of manganese reached 94.3% and 92.7%, respectively. The heavy metal impurities has been decreased to less than 1ppm, and the content of calcium, magnesium and sodium has been decreased to less than 20ppm, which meet standards of high pure reagent for energy and electronic materials. In compare with conventional technique from electrolytic manganese, the power consumption has been reduced to ≤2000 kWh/t(product) in our short-process approach. Moreover, comprehensive recovery rate of manganese increases significantly, and the wastewater generated from our short-process approach contains low content of ammonia/ nitrogen about 500 mg/t(product) and no toxic emissions. Our study contributes to the sustainable application of low-grade manganese ore. Acknowledgements: The authors are grateful to the National Science and Technology Support Program of China (No.2015BAB01B02) for financial support to the work.

Keywords: leaching, high purity, low-grade rhodochrosite, manganese oxide, purifying process, recovery ratio

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Authors: Hojat Heidari-Bafroui, Amer Charbaji, Constantine Anagnostopoulos, Mohammad Faghri

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Phosphorus is an essential nutrient for plant life which is most frequently found as phosphate in water. Once phosphate is found in abundance in surface water, a series of adverse effects on an ecosystem can be initiated. Therefore, a portable and reliable method is needed to monitor the phosphate concentrations in the field. In this paper, an inexpensive dip strip device with the ascorbic acid/antimony reagent dried on blotting paper along with wet chemistry is developed for the detection of low concentrations of phosphate in water. Ammonium molybdate and sulfuric acid are separately stored in liquid form so as to improve significantly the lifetime of the device and enhance the reproducibility of the device’s performance. The limit of detection and quantification for the optimized device are 0.134 ppm and 0.472 ppm for phosphate in water, respectively. The device’s shelf life, storage conditions, and limit of detection are superior to what has been previously reported for the paper-based phosphate detection devices.

Keywords: phosphate detection, paper-based device, molybdenum blue method, colorimetric assay

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Authors: Min-Hwa Lim, Mi-Jeong Park, Ho-Young Jung

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Imidazolium-brominated polyphenylene oxide (Im-bPPO) is based on the functionalization of bromomethylated poly(2,6-dimethyl-1,4-phenylene oxide) (BPPO) using 1-Methylimdazole. For the purpose of long cycle life of vanadium redox battery (VRB), the chemical stability of Im-bPPO, sPPO (sulfonated 2,6-dimethyl-1,4-phenylene oxide) and Fumatech membranes were evaluated firstly in the 0.1M vanadium (V) solution dissolved in 3M sulfuric acid (H2SO4) for 72h, and UV analyses of the degradation products proved that ether bond in PPO backbone was vulnerable to be attacked by vanadium (V) ion. It was found that the membranes had slightly weight loss after soaking in 2 ml distilled water included in STS pressure vessel for 1 day at 200◦C. ATR-FT-IR data indicated before and after the degradation of the membranes. Further evaluation on the degradation mechanism of the menbranes were carried out in Fenton’s reagent solution for 72 h at 50 ◦C and analyses of the membranes before and after degradation confirmed the weight loss of the membranes. The Fumatech membranes exhibited better performance than AEM and CEM, but Nafion 212 still suffers chemical degradation.

Keywords: vanadium redox flow battery, ion exchange membrane, permeability, degradation, chemical stability

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Authors: Ashish Kumar Singh, Preeti Tiwari, Shubham Srivastava, Rajiv Prakash, Herman Terryn, Gopal Ji

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Corrosion inhibition potential of azo dyes namely Allura red (AR), Sunset Yellow (SY) and Amaranth (AN) have been investigated in 0.5 M H2SO4 solutions by electrochemical impedance spectroscopy (EIS), Tafel polarization curves, linear polarization curves, open circuit potential (ocp) curves, UV-Visible spectroscopy, Fourier Transform Infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) techniques. Amaranth dye is found to provide highest corrosion inhibition (90 %) against mild steel corrosion in sulfuric acid solutions among all the tested dyes; while SY and AR dye shows 80% and 78% corrosion inhibition efficiency respectively. The electrochemical measurements and surface morphology analysis reveal that molecular adsorption of dyes at metal acid interface is accountable for inhibition of mild steel corrosion in H2SO4 solutions. The adsorption behavior of dyes has been investigated by various isotherms models, which verifies that it is in accordance with Langmuir isotherm.

Keywords: mild steel, Azo dye, EIS, Langmuir isotherm

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Authors: Khrizelle Angelique Sablan, Rizalinda De Leon, Jaeyoung Lee, Joey Ocon

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The impending water shortage drives us to find alternative sources of water. One of the possible solutions is desalination of seawater. There are numerous processes by which it can be done and one if which is capacitive deionization. Capacitive deionization is a relatively new technique for water desalination. It utilizes the electric double layer for ion adsorption. Carbon-based materials are commonly used as electrodes for capacitive deionization. In this study, carbon nanotubes (CNTs) were treated in a mixture of nitric and sulfuric acid. The silver addition was also facilitated to incorporate antimicrobial action. The acid-treated carbon nanotubes (f-CNTs) and silver-decorated f-CNTs (Ag@f-CNTs) were used as electrode materials for seawater deionization and compared with CNT and acid-treated CNT. The synthesized materials were characterized using TEM, EDS, XRD, XPS and BET. The electrochemical performance was evaluated using cyclic voltammetry, and the deionization performance was tested on a single cell with water containing 64mg/L NaCl. The results showed that the synthesized Ag@f-CNT-10 H could have better performance than CNT and a-CNT with a maximum ion removal efficiency of 50.22% and a corresponding adsorption capacity of 3.21 mg/g. It also showed antimicrobial activity against E. coli. However, the said material lacks stability as the efficiency decreases with repeated usage of the electrode.

Keywords: capacitive deionization, carbon nanotubes, desalination, acid functionalization, silver

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Authors: Zamouche Meriem, Mehcene Ismahan, Temmine Manel, Bencheikh Lehocine Mosaab, Meniai Abdeslam Hassen

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In this study, the adsorption of Malachite Green (MG) by chemical treated sewage sludge has been studied. The sewage sludge, collected from drying beds of the municipal wastewater treatment station of IBN ZIED, Constantine, Algeria, was treated by different acids such us HNO₃, H₂SO₄, H₃PO₄ for modifying its aptitude to removal the MG from aqueous solutions. The results obtained shows that the sewage sludge activated by sulfuric acid give the highest elimination amounts of MG (9.52 mg/L) compared by the other acids used. The effects of operation parameters have been investigated, the results obtained show that the adsorption capacity per unit of adsorbent mass decreases from 18.69 to 1.20 mg/g when the mass of the adsorbent increases from 0.25 to 4 g respectively, the optimum mass for which a maximum of elimination of the dye is equal to 0.5g. The increasing in the temperature of the solution results in a slight decrease in the adsorption capacity of the chemically treated sludge. The highest amount of dye adsorbed by CSSS (9.56 mg/g) was observed for the optimum temperature of 25°C. The chemical activated sewage sludge proved its effectiveness for the removal of the Red Congo (RC), but by comparison the adsorption of the two dyes studies, we noted that the sludge has more affinity to adsorb the (MG).

Keywords: adsorption, chemical activation, malachite green, sewage sludge

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Authors: Rajiv Arora

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Biodiesel may be economical if produced from inexpensive feedstock which commonly contains high level of free fatty acids (FFA) as an inhibitor in production of methyl ester. In this study, a two-step process for biodiesel production from high FFA spent bleach earth oil in a batch reactor is developed. Oil sample extracted from spent bleaching earth (SBE) was utilized for biodiesel process. In the first step, FFA of the SBE oil was reduced to 1.91% through sulfuric acid catalyzed esterification. In the second step, the product prepared from the first esterification process was carried out transesterification with an alkaline catalyst. The influence of four variables on conversion efficiency to methyl ester, i.e., methanol/ SBE oil molar ratio, catalyst amount, reaction temperature and reaction time, was studied in the second stage. The optimum process variables in the transesterification were methanol/oil molar ratio 6:1, heterogeneous catalyst conc. 5 wt %, reaction temperature 65 °C and reaction time 60 minutes to produce biodiesel. Major fuel properties of SBE biodiesel were measured to comply with ASTM and EN standards. Therefore, an optimized process for production of biodiesel from a low-cost high FFA source was accomplished.

Keywords: biodiesel, esterification, free fatty acids, residual oil, spent bleaching earth, transesterification

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Authors: Nurlan Akhmetov, Abilmansur Yeshmuratov, Aliya Kurbanova, Gulnar Sugurbekova, Murat Baisariyev

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Extraction of the vanadium and nickel compounds is complex due to the high stability of porphyrin, nickel is catalytic poison which deactivates catalysis during the catalytic cracking of the oil, while vanadyl is abrasive and valuable metal. Thus, high concentration of the Ni and V in the crude oil makes their removal relevant. Two methods of the demetallization of crude oil were tested, therefore, the present research is conducted for comparative analysis of the deasphalting with organic solvents (cyclohexane, carbon tetrachloride, chloroform) and electrochemical method. Percentage of Ni extraction reached maximum of approximately 55% by using the electrochemical method in electrolysis cell, which was developed for this research and consists of three sections: oil and protonating agent (EtOH) solution between two conducting membranes which divides it from two capsules of 10% sulfuric acid and two graphite electrodes which cover all three parts in electrical circuit. Ions of metals pass through membranes and remain in acid solutions. The best result was obtained in 60 minutes with ethanol to oil ratio 25% to 75% respectively, current fits in to the range from 0.3A to 0.4A, voltage changed from 12.8V to 17.3V. Maximum efficiency of deasphalting, with cyclohexane as the solvent, in Soxhlet extractor was 66.4% for Ni and 51.2% for V. Thus, applying the voltammetry, ICP MS (Inductively coupled plasma mass spectrometry) and AAS (atomic absorption spectroscopy), these mentioned types of metal extraction methods were compared in this paper.

Keywords: electrochemistry, deasphalting of crude oil, demetallization of crude oil, petrolium engineering

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Authors: Mahmoud A. Rabah, Said El Sheikh

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This work shows the preparation of chromium nanoparticles from tannery waste solution on glassy carbon by chemical method compared to electrokinetic process. The waste solution contains free and soluble fats, calcium, iron, magnesium and high sodium in addition to the chromium ions. Filtration helps removal of insoluble matters. Diethyl ether successfully extracted soluble fats. The method started by removing calcium as insoluble oxalate salts at hot conditions in a faint acidic medium. The filtrate contains iron, magnesium, chromium ions and sodium chloride in excess. Chromium was separated selectively as insoluble hydroxide sol-gel at pH 6.5, filtered and washed with distilled water. Part of the gel reacted with sulfuric acid to produce chromium sulfate solution having 15-25 g/L concentration. Electrokinetic deposition of chromium nanoparticles on a carbon cathode was carried out using platinum anode under different galvanostatic conditions. The chemical method involved impregnating the carbon specimens with chromium hydroxide gel followed by reduction using hydrazine hydrate or by thermal reduction using hydrogen gas at 1250°C. Chromium grain size was characterized by TEM, FT-IR and SEM. Properties of the Cr grains were correlated to the conditions of the preparation process. Electrodeposition was found to control chromium particles to be more identical in size and shape as compared to the chemical method.

Keywords: chromium, electrodeposition, nanoparticles, tannery waste solution

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Authors: Ayfer Kilicarslan, Kubra Onol, Sercan Basit, Muhlis Nezihi Saridede

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Chalcopyrite (CuFeS2) is the most common primary mineral used for the commercial production of copper. The low dissolution efficiency of chalcopyrite in sulfate media has prevented an efficient industrial leaching of this mineral in sulfate media. Ferric ions, bacteria, oxygen and other oxidants have been used as oxidizing agents in the leaching of chalcopyrite in sulfate and chloride media under atmospheric or pressure leaching conditions. Two leaching methods were studied to evaluate chalcopyrite (CuFeS2) dissolution in acid media. First, the conventional oxidative acid leaching method was carried out using sulfuric acid (H2SO4) and potassium dichromate (K2Cr2O7) as oxidant at atmospheric pressure. Second, microwave-assisted acid leaching was performed using the microwave accelerated reaction system (MARS) for same reaction media. Parameters affecting the copper extraction such as leaching time, leaching temperature, concentration of H2SO4 and concentration of K2Cr2O7 were investigated. The results of conventional acid leaching experiments were compared to the microwave leaching method. It was found that the copper extraction obtained under high temperature and high concentrations of oxidant with microwave leaching is higher than those obtained conventionally. 81% copper extraction was obtained by the conventional oxidative acid leaching method in 180 min, with the concentration of 0.3 mol/L K2Cr2O7 in 0.5M H2SO4 at 50 ºC, while 93.5% copper extraction was obtained in 60 min with microwave leaching method under same conditions.

Keywords: extraction, copper, microwave-assisted leaching, chalcopyrite, potassium dichromate

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Authors: Reena D. Souza, Tripti Vats, Prem F. Siril

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Esterification of free fatty acid (oleic acid) and transesterification of waste cooking oil (WCO) with ethanol over graphene oxide (GO), GO-Fe2O3, sulfonated GO (GO-SO3H), and Fe2O3/GO-SO3H catalysts were examined in the present study. Iron oxide supported graphene-based acid catalyst (Fe2O3/GO-SO3H) exhibited highest catalytic activity. GO was prepared by modified Hummer’s process. The GO-Fe2O3 nanocomposites were prepared by the addition of NaOH to a solution containing GO and FeCl3. Sulfonation was done using concentrated sulfuric acid. Transmissionelectron microscopy (TEM) and atomic force microscopy (AFM) imaging revealed the presence of Fe2O3 particles having size in the range of 50-200 nm. Crystal structure was analyzed by XRD and defect states of graphene were characterized using Raman spectroscopy. The effects of the reaction variables such as catalyst loading, ethanol to acid ratio, reaction time and temperature on the conversion of fatty acids were studied. The optimum conditions for the esterification process were molar ratio of alcohol to oleic acid at 12:1 with 5 wt% of Fe2O3/GO-SO3H at 1000C with a reaction time of 4h yielding 99% of ethyl oleate. This is because metal oxide supported solid acid catalysts have advantages of having both strong Brønsted as well as Lewis acid properties. The biodiesel obtained by transesterification of WCO was characterized by 1H NMR and Gas Chromatography techniques. XRD patterns of the recycled catalyst evidenced that the catalyst structure was unchanged up to the 5th cycle, which indicated the long life of the catalyst.

Keywords: Fe₂O₃/GO-SO₃H, Graphene Oxide, GO-Fe₂O₃, GO-SO₃H, WCO

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Authors: Mahmoud A. Abdulhamid

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Poly(ether-ether-ketone) (PEEK) has received increased attention due to its outstanding performance in different membrane applications including gas and liquid separation. However, it suffers from a semi-crystalline morphology, bad solubility and low porosity. To fabricate membranes from PEEK, the usage of harsh acid such as sulfuric acid is essential, regardless its hazardous properties. In this work, we report the molecular design of poly(ether-ether-ketones) (iPEEKs) with intrinsic porosity character, by incorporating kinked units into PEEK backbone such as spirobisindane, Tröger's base, and triptycene. The porous polymers were used to fabricate stable membranes for organic solvent nanofiltration application. To better understand the mechanism, we conducted molecular dynamics simulations to evaluate the possible interactions between the polymers and the solvents. Notable enhancement in separation performance was observed confirming the importance of molecular engineering of high-performance polymers. The iPEEKs demonstrated good solubility in polar aprotic solvents, a high surface area of 205–250 m² g⁻¹, and excellent thermal stability. Mechanically flexible nanofiltration membranes were prepared from N-methyl-2-pyrrolidone dope solution at iPEEK concentrations of 19–35 wt%. The molecular weight cutoff of the membranes was fine-tuned in the range of 450–845 g mol⁻¹ displaying 2–6 fold higher permeance (3.57–11.09 L m⁻² h⁻¹ bar⁻¹) than previous reports. The long-term stabilities were demonstrated by a 7 day continuous cross-flow filtration.

Keywords: molecular engineering, polymer synthesis, membrane fabrication, liquid separation

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Authors: Aliya Kurbanova, Nurlan Akhmetov, Abilmansur Yeshmuratov, Yerzhigit Sugurbekov, Ramiz Zulkharnay, Gulzat Demeuova, Murat Baisariyev, Gulnar Sugurbekova

Abstract:

Last decades crude oils have tended to become more challenge to process due to increasing amounts of sour and heavy crude oils. Some crude oils contain high vanadium and nickel content, for example Pavlodar LLP crude oil, which contains more than 23.09 g/t nickel and 58.59 g/t vanadium. In this study, we used two types of metal removing methods such as solvent extraction and electrochemical. The present research is conducted for comparative analysis of the deasphalting with organic solvents (cyclohexane, carbon tetrachloride, chloroform) and electrochemical method. Applying the cyclic voltametric analysis (CVA) and Inductively coupled plasma mass spectrometry (ICP MS), these mentioned types of metal extraction methods were compared in this paper. Maximum efficiency of deasphalting, with cyclohexane as the solvent, in Soxhlet extractor was 66.4% for nickel and 51.2% for vanadium content from crude oil. Percentage of Ni extraction reached maximum of approximately 55% by using the electrochemical method in electrolysis cell, which was developed for this research and consists of three sections: oil and protonating agent (EtOH) solution between two conducting membranes which divides it from two capsules of 10% sulfuric acid and two graphite electrodes which cover all three parts in electrical circuit. Ions of metals pass through membranes and remain in acid solutions. The best result was obtained in 60 minutes with ethanol to oil ratio 25% to 75% respectively, current fits into the range from 0.3A to 0.4A, voltage changed from 12.8V to 17.3V.

Keywords: demetallization, deasphalting, electrochemical removal, heavy metals, petroleum engineering, solvent extraction

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Authors: B. S. Boyanov, A. B. Peltekov, K. I. Ivanov

Abstract:

The ferrites of Zn, Cd, Cu, and mixed ferrites with NiO, MnO, MgO, CoO, ZnO, BaO combine the properties of dielectrics, semiconductors, ferro-magnets, catalysts, etc. The ferrites are used in an impressive range of applications due to their remarkable properties. A specific disadvantage of ferrites is that they are undesirably obtained in a lot of processes connected with metal production. They are very stable and poorly soluble compounds. The obtained ZnFe2O4 in zinc production connecting about 15% of the total zinc remains practically insoluble in dilute solutions of sulfuric acid. This decreases the degree of recovery of zinc and necessitates to further process the zinc-containing cake. In this context, the ferrites; ZnFe2O4, CdFe2O4, and CuFe2O4 are synthesized in laboratory conditions using ceramic technology. Their homogeneity and structure are proven by X-Ray diffraction analysis and Mössbauer spectroscopy. The synthesized ferrites are subjected to strong acid and high temperature leaching with solutions of H2SO4, HCl, and HNO3 (7, 10 and 15 %). The results indicate that the highest degree of leaching of Zn, Cd, and Cu from the ferrites is achieved by use of HCl. The resulting values for the degree of leaching of metals using H2SO4 are lower, but still remain significantly higher for all of the experimental conditions compared to the values obtained using HNO3. Five zinc sulfide concentrates are characterized for iron content by chemical analysis, Web-based Information System, and iron phases by Mössbauer spectroscopy. The charging was optimized using the criterion of minimal amount of zinc ferrite produced when roasting the concentrates in a fluidized bed. The results obtained are interpreted in terms of the hydrometallurgical zinc production and maximum recovery of zinc, copper and cadmium from initial zinc sulfide concentrates after their roasting.

Keywords: hydrometallurgy, inorganic acids, solubility, zinc ferrite

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Authors: M. Gómez-Ramírez, A. Rivas-Castillo, I. Rodríguez-Pozos, R. A. Avalos-Zuñiga, N. G. Rojas-Avelizapa

Abstract:

Among the diverse types of pollutants produced by anthropogenic activities, metals represent a serious threat, due to their accumulation in ecosystems and their elevated toxicity. The mine tailings of abandoned mines contain high levels of metals such as arsenic (As), zinc (Zn), copper (Cu), and lead (Pb), which do not suffer any degradation process, they are accumulated in environment. Abandoned mine tailings potentially could contaminate rivers and aquifers representing a risk for human health due to their high metal content. In an attempt to remove the metals and thereby mitigate the environmental pollution, an environmentally friendly and economical method of bioremediation has been introduced. Bioleaching has been actively studied over the last several years, and it is one of the bioremediation solutions used to treat heavy metals contained in sewage sludge, sediment and contaminated soil. Acidithiobacillus thiooxidans, an extremely acidophilic, chemolithoautotrophic, gram-negative, rod shaped microorganism, which is typically related to Cu mining operations (bioleaching), has been well studied for industrial applications. The sulfuric acid produced plays a major role in bioleaching. Specifically, Acidithiobacillus thiooxidans strain DSM 26636 has been able to leach Al, Ni, V, Fe, Mg, Si, and Ni contained in slags from coal combustion wastes. The present study reports the ability of A. thiooxidans DSM 26636 for the bioleaching of metals contained in two different mine tailing samples (MT1 and MT2). It was observed that Al, Fe, and Mn were removed in 36.3±1.7, 191.2±1.6, and 4.5±0.2 mg/kg for MT1, and in 74.5±0.3, 208.3±0.5, and 20.9±0.1 for MT2. Besides, < 1.5 mg/kg of Au and Ru were also bioleached from MT1; in MT2, bioleaching of Zn was observed at 55.7±1.3 mg/kg, besides removal of < 1.5 mg/kg was observed for As, Ir, Li, and 0.6 for Os in this residue. These results show the potential of strain DSM 26636 for the bioleaching of metals that came from different mine tailings.

Keywords: A. thiooxidans, bioleaching, metals, mine tailings

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Authors: Jae-Yong Park, Gwancheol Seo, Young-Ho Kim

Abstract:

Microvoids, sometimes called Kikendall voids, generally form in the interfaces between Sn-based solders and Cu and degrade the mechanical and electrical properties of the solder joints. The microvoid formation is known as the rapid interdiffusion between Sn and Cu and impurity content in the Cu. Cu electroplating from the acid solutions has been widely used by microelectronic packaging industry for both printed circuit board (PCB) and integrated circuit (IC) applications. The quality of electroplated Cu that can be optimized by the electroplating conditions is critical for the solder joint reliability. In this paper, the influence of electroplating conditions on the microvoid growth in the interfaces between Sn-3.0Ag-0.5Cu (SAC) solder and Cu layer was investigated during isothermal aging. The Cu layers were electroplated by controlling the additive of electroplating bath and current density to induce various microvoid densities. The electroplating bath consisted of sulfate, sulfuric acid, and additives and the current density of 5-15 mA/cm2 for each bath was used. After aging at 180 °C for up to 250 h, typical bi-layer of Cu6Sn5 and Cu3Sn intermetallic compounds (IMCs) was gradually growth at the SAC/Cu interface and microvoid density in the Cu3Sn showed disparities in the electroplating conditions. As the current density increased, the microvoid formation was accelerated in all electroplating baths. The higher current density induced, the higher impurity content in the electroplated Cu. When the polyethylene glycol (PEG) and Cl- ion were mixed in an electroplating bath, the microvoid formation was the highest compared to other electroplating baths. On the other hand, the overall IMC thickness was similar in all samples irrespective of the electroplating conditions. Impurity content in electroplated Cu influenced the microvoid growth, but the IMC growth was not affected by the impurity content. In conclusion, the electroplated conditions are properly optimized to avoid the excessive microvoid formation that results in brittle fracture of solder joint under high strain rate loading.

Keywords: electroplating, additive, microvoid, intermetallic compound

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Authors: Dalvir Kataria, Khushminder Kaur Chahal, Amit Kumar

Abstract:

The carrot seed essential oil was obtained by hydrodistillation. Hexane, dichloromethane, and methanol solvents were used for extraction of carrot seed by Soxhlet extraction methods. The major and minor compounds identified in carrot seed essential oil were carotol (52.73), daucol (5.10), daucene (5.68), (E)-β-farnesene (5.40), β-cubebene (3.19), longifolenaldehyde (3.23), β-elimene (3.23), (E)-caryophyllene (1.22), β-bisabolene (2.95) etc. The chemical composition of hexane, dichloromethane, and methanol extracts was different. Carotol was the common compound present. Major compounds isolated were from the carrot seed essential oil by column chromatography. Chemical transformations of carotol (2) with mercuric acetate/sodium borohydride, dry hydrochloric acid gas, acetonitrile/sulfuric acid, selenium dioxide/t-butyl hydrogen peroxide, N-bromosuccinimide, hydrogen iodide, and phenol were carried out. The derivatives of carotol were designed to explore the significance of some structural modifications in relation to antioxidant activities. The structures of major compounds and derivatives were confirmed on the basis of FT-IR, 1HNMR and 13CNMR spectroscopy. Antioxidant activity of carrot seed essential oil, various extracts and isolated compounds were tested by in vitro models involving 2, 2-diphenyl-1-picrylhydrazyl (DPPH•), hydroxyl (OH•), nitric oxide (NO•), superoxide radical scavenging methods and ferric reducing antioxidant power assay (FRAP). Chemical transformations of major isolated compound carotol were carried out, and antioxidant activity of all compounds was undertaken. The major sesquiterpenoidcarotol isolated from carrot seed essential oil showed the highest antioxidant activity in all the methods. The methanol extract showed higher antioxidant potential as compared to carrot seed essential oil, hexane, and dichloromethane extracts.

Keywords: antioxidant, carotol, carrot, DPPH

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Authors: Pratikno Hidayat, Khamdan Cahyari

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Hydrogen is the ultimate choice of energy carriers in future. It contents high energy density (42 kJ/g), emits only water vapor during combustion and has high energy conversion up to 50% in fuel cell application. One of the promising methods to produce hydrogen is from organic waste through dark fermentation method. It utilizes sugar-rich organic waste as substrate and hydrogen-producing microorganisms to generate the hydrogen. Solid waste of sago processing industries in Indonesia is one of the promising raw materials for both producing biofuel hydrogen and mitigating the environmental impact due to the waste disposal. This research was meant to investigate the effect of chemical and biological pretreatment i.e. acid treatment and mushroom cultivation toward lignocellulosic waste of these sago industries. Chemical pretreatment was conducted through exposing the waste into acid condition using sulfuric acid (H2SO4) (various molar i.e. 0.2, 0.3, and 0.4 M and various duration of exposure i.e. 30, 60 and 90 minutes). Meanwhile, biological treatment was conducted through utilization of the solid waste as growth media of mushroom (Oyster and Ling-zhi) for 3 months. Dark fermentation was conducted at pH 5.0, temperature 27℃ and atmospheric pressure. It was noticed that chemical and biological pretreatment could improve hydrogen yield with the highest yield at 3.8 ml/g VS (31%v H2). The hydrogen production was successfully performed to generate high percentage of hydrogen, although the yield was still low. This result indicated that the explosion of acid chemical and biological method might need to be extended to improve degradability of the solid waste. However, high percentage of hydrogen was resulted from proper pretreatment of residual sludge of biogas plant to generate hydrogen-producing inoculum.

Keywords: hydrogen, sago waste, chemical, biological, dark fermentation, Indonesia

Procedia PDF Downloads 344

Authors: Marisa Chrysochoou, James Mahoney, Kay Wille

Abstract:

Pyrrhotite is an iron-sulfide mineral which releases sulfuric acid when exposed to water and oxygen. The presence of this mineral in concrete foundations across Connecticut and Massachusetts in the US is causing in some cases premature failure. This has resulted in a devastating crisis for all parties affected by this type of failure which can take up to 15-25 years before internal damage becomes visible on the surface. This study shares laboratory results aimed to investigate the fundamental mechanisms of pyrrhotite reaction and to further the understanding of its deterioration kinetics within concrete. This includes the following analyses: total sulfur, wavelength dispersive X-ray fluorescence, expansion, reaction rate combined with ion-chromatography, as well as damage evolution using electro-chemical acceleration. This information is coupled to a statistical analysis of over 150 analyzed concrete foundations. Those samples were obtained and process using a developed and validated sampling method that is minimally invasive to the foundation in use, provides representative samples of the concrete matrix across the entire foundation, and is time and cost-efficient. The processed samples were then analyzed using a developed modular testing method based on total sulfur and wavelength dispersive X-ray fluorescence analysis to quantify the amount of pyrrhotite. As part of the statistical analysis the results were grouped into the following three categories: no damage observed and no pyrrhotite detected, no damage observed and pyrrhotite detected and damaged observed and pyrrhotite detected. As expected, a strong correlation between amount of pyrrhotite, age of the concrete and damage is observed. Information from the laboratory investigation and from the statistical analysis of field samples will aid in forming a scientific basis to support the decision process towards sustainable financial and administrative solutions by state and local stakeholders.

Keywords: concrete, pyrrhotite, risk of failure, statistical analysis

Procedia PDF Downloads 38

Authors: Zineb Kassab, Nassima El Miri, A. Aboulkas, Abdellatif Barakat, Mounir El Achaby

Abstract:

Recently, more attention has been given to biopolymers with a focus on sustainable development and environmental preservation. Following this tendency, the attempt has been made to replace polymers derived from petroleum with superior biodegradable polymers (biopolymers). In this context, biopolymers are considered potential replacements for conventional plastic materials. However, some of their properties must be improved for better competitiveness, especially regarding their mechanical, thermal and barrier properties. Bio-nanocomposite technology using nanofillers has already been proven as an effective way to produce new materials with specific properties and high performances. With the emergence of nanostructured bio-composite materials, incorporating elongated rod-like cellulose nanocrystals (CNC) has attracted more and more attention in the field of nanotechnology. This study is aimed to develop bio-composite films of biopolymer matrices [Carboxymethyle cellulose (CMC), Starch (ST), Chitosan (CS) and Polyvinyl alcohol (PVA)] reinforced with cellulose nanocrystals (CNC) using the solution casting method. The CNC were extracted at a nanometric scale from lignocellulosic fibers via sulfuric acid hydrolysis and then characterized using X-ray diffraction (XRD), thermogravimetric analysis (TGA), confocal microscopy, infrared spectroscopy (IR), atomic force and transmission electron microscopies (AFM and TEM) techniques. The as extracted CNC were used as a reinforcing phase to produce a variety of bio-composite films at different CNC loading (0.5-10 wt %) with specific properties. The rheological properties of film-forming solutions (FFS) of bio-composites were studied, and their relation to the casting process was evaluated. Then, the structural, optical transparency, water vapor permeability, thermal stability and mechanical properties of all prepared bio-composite films were evaluated and studied in this report. The high performances of these bio-composite films are expected to have potential in biomaterials or packaging applications.

Keywords: biopolymer composites, cellulose nanocrystals, food packaging, lignocellulosic fibers

Procedia PDF Downloads 214