Search results for: phosphoric%20acid%20plant
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 68

Search results for: phosphoric%20acid%20plant

68 The Effect of Diluents in the Liquid-Liquid Extraction of Cobalt(II) with Di(2-Ethylhexyl) Phosphoric Acid

Authors: Fatima Ghebghoub

Abstract:

The solvent extraction of cobalt (II) from sulfate medium using di(2-ethylhexy1) phosphoric acid (D2EHPA, HL) at 25°C has been investigated. The influence of the following parameters was studied: the equilibrium pH, the concentration of the extractant and the nature of diluent. The effect of the diluent using polar and non-polar solvents in the extraction of nickel(II) is discussed. The extracted nickel (II species were found to be CoL2 in 1-octanol and methyl isobutyl ketone and CoL2.2HL in toluene, dichloromethane, chloroform, carbon tetrachloride and cyclohexane. The extraction constants are evaluated for the different diluents.

Keywords: liquid-liquid extraction, cobalt(II), di(2-ethylhexyl) phosphoric acid, diluent effect

Procedia PDF Downloads 494
67 Morphology and Mineralogy of Acid Treated Soil

Authors: P. Hari Prasad Reddy, C. H. Rama Vara Prasad, G. Kalyan Kumar

Abstract:

This paper presents the morphological and mineralogical changes occurring in the soil due to immediate and prolonged interaction with different concentrations of phosphoric acid and sulphuric acid. In order to assess the effect of acid contamination, a series of sediment volume, scanning electron microscopy and X-ray diffraction analysis tests were carried out on soil samples were exposed to different concentrations (1N, 4N and 8N) of phosphoric and sulphuric acid. Experimental results show that both acids showed severe morphological and mineralogical changes with synthesis of neogenic formations mainly at higher concentrations (4N and 8N) and at prolonged duration of interaction (28 and 80 days).

Keywords: phosphoric acid, scanning electron microscopy, sulphuric acid, x-ray diffraction analysis

Procedia PDF Downloads 389
66 Carbothermic Reduction of Phosphoric Acid Extracted from Dephosphorization Slags to Produce Yellow Phosphorus

Authors: Ryoko Yoshida, Jyunpei Yoshida, Hua Fang Yu, Yasushi Sasaki, Tetsuya Nagasaka

Abstract:

Phosphorous is an important element for agriculture and industry and is a non-renewable resource. Especially, yellow phosphorus is an essential material in advanced industrial technology, but phosphorus resources were not produced in Japan at all, and all depend on imports. It has been suggested, however, that the remaining accessible reserves of phosphate ore will be depleted within 50 years. Therefore, alternative resources for phosphate ore must be found. In this research, we have developed a process that enables the production of high-purity yellow phosphorus from domestic unused phosphorus resources such as steelmaking slags. The process consists of two parts: (1) the production of crude phosphoric acid from wastes such as steelmaking slag; (2) producing high-purity yellow phosphorus by low-temperature carbothermic reduction of phosphoric acid (H3PO4). The details of the carbothermic reduction of phosphoric acid are presented in this paper. Yellow phosphorus is commercially produced by carbothermic reduction of phosphate ore in an electric arc furnace at more than 1673K. In the newly developed system, gaseous P4O10 evaporated from H3PO4 is successfully reduced to yellow phosphorus by using carbon packed bed at less than 1273K. To meet the depletion of phosphate ore, the proposed process in this study to produce yellow phosphorus by carbothermic reduction of H3PO4 that are extracted from dephosphorization slags will be one of the effective and economical solutions.

Keywords: carbothermic reduction, phosphoric acid, dephosphorization slags, yellow phosphorus

Procedia PDF Downloads 84
65 Exergetic Analysis of Steam Turbine Power Plant Operated in Chemical Industry

Authors: F. Hafdhi, T. Khir, A. Ben Yahia, A. Ben Brahim

Abstract:

An Energetic and exergetic analysis is conducted on a Steam Turbine Power Plant of an existing Phosphoric Acid Factory. The heat recovery systems used in different parts of the plant are also considered in the analysis. Mass, thermal and exergy balances are established on the main compounds of the factory. A numerical code is established using EES software to perform the calculations required for the thermal and exergy plant analysis. The effects of the key operating parameters such as steam pressure and temperature, mass flow rate as well as seawater temperature, on the cycle performances are investigated. A maximum Exergy Loss Rate of about 72% is obtained for the melters, followed by the condensers, heat exchangers and the pumps. The heat exchangers used in the phosphoric acid unit present exergetic efficiencies around 33% while 60% to 72% are obtained for steam turbines and blower. For the explored ranges of HP steam temperature and pressure, the exergy efficiencies of steam turbine generators STGI and STGII increase of about 2.5% and 5.4% respectively. In the same way, optimum HP steam flow rate values, leading to the maximum exergy efficiencies are defined.

Keywords: steam turbine generator, energy efficiency, exergy efficiency, phosphoric acid plant

Procedia PDF Downloads 280
64 Comparing the Gap Formation around Composite Restorations in Three Regions of Tooth Using Optical Coherence Tomography (OCT)

Authors: Rima Zakzouk, Yasushi Shimada, Yuan Zhou, Yasunori Sumi, Junji Tagami

Abstract:

Background and Purpose: Swept source optical coherence tomography (OCT) is an interferometric imaging technique that has been recently used in cariology. In spite of progress made in adhesive dentistry, the composite restoration has been failing due to secondary caries which occur due to environmental factors in oral cavities. Therefore, a precise assessment to effective marginal sealing of restoration is highly required. The aim of this study was evaluating gap formation at composite/cavity walls interface with or without phosphoric acid etching using SS-OCT. Materials and Methods: Round tapered cavities (2×2 mm) were prepared in three locations, mid-coronal, cervical, and root of bovine incisors teeth in two groups (SE and PA Groups). While self-etching adhesive (Clearfil SE Bond) was applied for the both groups, Group PA had been already pretreated with phosphoric acid etching (K-Etchant gel). Subsequently, both groups were restored by Estelite Flow Quick Flowable Composite Resin. Following 5000 thermal cycles, three cross-sectionals were obtained from each cavity using OCT at 1310-nm wavelength at 0°, 60°, 120° degrees. Scanning was repeated after two months to monitor the gap progress. Then the average percentage of gap length was calculated using image analysis software, and the difference of mean between both groups was statistically analyzed by t-test. Subsequently, the results were confirmed by sectioning and observing representative specimens under Confocal Laser Scanning Microscope (CLSM). Results: The results showed that pretreatment with phosphoric acid etching, Group PA, led to significantly bigger gaps in mid-coronal and cervical compared to SE group, while in the root cavity no significant difference was observed between both groups. On the other hand, the gaps formed in root’s cavities were significantly bigger than those in mid-coronal and cervical within the same group. This study investigated the effect of phosphoric acid on gap length progress on the composite restorations. In conclusions, phosphoric acid etching treatment did not reduce the gap formation even in different regions of the tooth. Significance: The cervical region of tooth was more exposing to gap formation than mid-coronal region, especially when we added pre-etching treatment.

Keywords: image analysis, optical coherence tomography, phosphoric acid etching, self-etch adhesives

Procedia PDF Downloads 188
63 Durability Performances of Epoxy Resin/TiO₂ Composited Alkali-Activated Slag/Fly Ash Pastes in Phosphoric Acid Solution

Authors: Jie Ren, Siyao Guo

Abstract:

Laden with phosphates at a low pH value, sewage wastewater aggressive environments constitute a great threat to concrete-based pipes which is made of alkaline cementitious materials such as ordinary Portland cement (OPC). As a promising alternative for OPC-based binders, alkali-activated slag/fly ash (AASF) cementitious binders are generally believed to gain similar or better properties compared to OPC-based counterparts, especially durability. However, there is limited research on the performance of AASF binders in phosphoric acid solution. Moreover, the behavior of AASF binders composited with epoxy resin/TiO₂ when exposed to acidic media has been rarely explored. In this study, the performance of AASF paste with the precursor slag:fly ash (50:50 in mass ratio) enhanced with epoxy resin/TiO₂ composite in phosphoric acid solution (pH = 3.0-4.0) was investigated. The exposure towards acid attack lasted for 90 days. The same AASF mixture without resin/TiO₂ composite was used as a reference. The compressive strength and porous-related properties prior to acidic immersion were tested. The mass variations and degradation depth of the two mixtures of binders were also monitored which is based on phenolphthalein-videomicroscope method. The results show that the binder with epoxy resin/TiO₂ addition gained a higher compressive strength and lower water absorption than the reference. In addition, it also displayed a higher resistance towards acid attack indicated by a less mass loss and less degradation depth compared to the control sample. This improvement can be attributed to a dense microstructure evidenced by the higher compressive strength and related porous structures. It can be concluded that the microstructure can be improved by adding epoxy resin/TiO₂ composite in order to enhance the resistance of AASF binder towards acid attacks.

Keywords: alkali-activated paste, epoxy resin/TiO₂, composites, mechanical properties, phosphoric acid

Procedia PDF Downloads 88
62 Equilibrium and Kinetic Studies of Lead Adsorption on Activated Carbon Derived from Mangrove Propagule Waste by Phosphoric Acid Activation

Authors: Widi Astuti, Rizki Agus Hermawan, Hariono Mukti, Nurul Retno Sugiyono

Abstract:

The removal of lead ion (Pb2+) from aqueous solution by activated carbon with phosphoric acid activation employing mangrove propagule as precursor was investigated in a batch adsorption system. Batch studies were carried out to address various experimental parameters including pH and contact time. The Langmuir and Freundlich models were able to describe the adsorption equilibrium, while the pseudo first order and pseudo second order models were used to describe kinetic process of Pb2+ adsorption. The results show that the adsorption data are seen in accordance with Langmuir isotherm model and pseudo-second order kinetic model.

Keywords: activated carbon, adsorption, equilibrium, kinetic, lead, mangrove propagule

Procedia PDF Downloads 132
61 Agro-Industrial Waste as a Source of Catalyst Production

Authors: Brenda Cecilia Ledesma, Andrea Beltramone

Abstract:

This work deals with the bio-waste valorization approach for catalyst development, the use of products derived from biomass as raw material and the obtaining of biofuels. In this research, activated carbons were synthesized from the orange peel using different synthesis conditions. With the activated carbons obtained with the best structure and texture, PtIr bimetallic catalysts were prepared. Carbon activation was carried out through a chemical process with phosphoric acid as an activating agent, varying the acid concentration, the ratio substrate/activating agent and time of contact between them. The best support was obtained using a carbonization time of 1 h, the temperature of carbonization of 470oC, the phosphoric acid concentration of 50 wt.% and a BET area of 1429 m2/g. Subsequently, the metallic nanoparticles were deposited in the activated carbon to use the solid as a catalytic material for the hydrogenation of HMF to 2,5-DMF. The catalyst presented an excellent performance for biofuels generation.

Keywords: orange peel, bio-waste valorization, platinum, iridium, 5-hydroxymethylfurfural

Procedia PDF Downloads 153
60 A Comparative Study: Influences of Polymerization Temperature on Phosphoric Acid Doped Polybenzimidazole Membranes

Authors: Cagla Gul Guldiken, Levent Akyalcin, Hasan Ferdi Gercel

Abstract:

Fuel cells are electrochemical devices which convert the chemical energy of hydrogen into the electricity. Among the types of fuel cells, polymer electrolyte membrane fuel cells (PEMFCs) are attracting considerable attention as non-polluting power generators with high energy conversion efficiencies in mobile applications. Polymer electrolyte membrane (PEM) is one of the essential components of PEMFCs. Perfluorosulfonic acid based membranes known as Nafion® is widely used as PEMs. Nafion® membranes water dependent proton conductivity which limits the operating temperature below 100ᵒC. At higher temperatures, proton conductivity and mechanical stability of these membranes decrease because of dehydration. Polybenzimidazole (PBI), which has good anhydrous proton conductivity after doped with acids, as well as excellent thermal stability, shows great potential in the application of high temperature PEMFCs. In the present study, PBI polymers were synthesized by solution polycondensation at 190 and 210ᵒC. The synthesized polymers were characterized by FTIR, 1H NMR, and TGA. Phosphoric acid doped PBI membranes were prepared and tested in a PEMFC. The influences of reaction temperature on structural properties of synthesized polymers were investigated. Mechanical properties, acid-doping level, proton conductivity, and fuel cell performances of prepared phosphoric acid doped PBI membranes were evaluated. The maximum power density was found as 32.5 mW/cm² at 120ᵒC.

Keywords: fuel cell, high temperature polymer electrolyte membrane, polybenzimidazole, proton exchange membrane fuel cell

Procedia PDF Downloads 152
59 Estimation of Fouling in a Cross-Flow Heat Exchanger Using Artificial Neural Network Approach

Authors: Rania Jradi, Christophe Marvillet, Mohamed Razak Jeday

Abstract:

One of the most frequently encountered problems in industrial heat exchangers is fouling, which degrades the thermal and hydraulic performances of these types of equipment, leading thus to failure if undetected. And it occurs due to the accumulation of undesired material on the heat transfer surface. So, it is necessary to know about the heat exchanger fouling dynamics to plan mitigation strategies, ensuring a sustainable and safe operation. This paper proposes an Artificial Neural Network (ANN) approach to estimate the fouling resistance in a cross-flow heat exchanger by the collection of the operating data of the phosphoric acid concentration loop. The operating data of 361 was used to validate the proposed model. The ANN attains AARD= 0.048%, MSE= 1.811x10⁻¹¹, RMSE= 4.256x 10⁻⁶ and r²=99.5 % of accuracy which confirms that it is a credible and valuable approach for industrialists and technologists who are faced with the drawbacks of fouling in heat exchangers.

Keywords: cross-flow heat exchanger, fouling, estimation, phosphoric acid concentration loop, artificial neural network approach

Procedia PDF Downloads 165
58 Study of Structural Behavior and Proton Conductivity of Inorganic Gel Paste Electrolyte at Various Phosphorous to Silicon Ratio by Multiscale Modelling

Authors: P. Haldar, P. Ghosh, S. Ghoshdastidar, K. Kargupta

Abstract:

In polymer electrolyte membrane fuel cells (PEMFC), the membrane electrode assembly (MEA) is consisting of two platinum coated carbon electrodes, sandwiched with one proton conducting phosphoric acid doped polymeric membrane. Due to low mechanical stability, flooding and fuel cell crossover, application of phosphoric acid in polymeric membrane is very critical. Phosphorous and silica based 3D inorganic gel gains the attention in the field of supercapacitors, fuel cells and metal hydrate batteries due to its thermally stable highly proton conductive behavior. Also as a large amount of water molecule and phosphoric acid can easily get trapped in Si-O-Si network cavities, it causes a prevention in the leaching out. In this study, we have performed molecular dynamics (MD) simulation and first principle calculations to understand the structural, electronics and electrochemical and morphological behavior of this inorganic gel at various P to Si ratios. We have used dipole-dipole interactions, H bonding, and van der Waals forces to study the main interactions between the molecules. A 'structure property-performance' mapping is initiated to determine optimum P to Si ratio for best proton conductivity. We have performed the MD simulations at various temperature to understand the temperature dependency on proton conductivity. The observed results will propose a model which fits well with experimental data and other literature values. We have also studied the mechanism behind proton conductivity. And finally we have proposed a structure for the gel paste with optimum P to Si ratio.

Keywords: first principle calculation, molecular dynamics simulation, phosphorous and silica based 3D inorganic gel, polymer electrolyte membrane fuel cells, proton conductivity

Procedia PDF Downloads 92
57 Corrosion Inhibition of Brass in Phosphoric Acid Solution by 2-(5-Methyl-2-Nitro-1H-Imidazol-1-Yl) Ethyl Benzoate

Authors: R. Khrifou, M. Galai, R. Touir, M. Ebn Touhami, Y. Ramli

Abstract:

A 2-(5-methyl-2-Nitro-1H-imidazol-1-yl)ethyl benzoate (IMDZ-B) was synthesized and characterized using elemental analyses, NMR, and Fourier transform infrared (FTIR) techniques. Its effect on brass corrosion in 1.0 M H₃PO₄ solution was investigated by using electrochemical measurements coupled with X-ray diffraction analysis (XRD), Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX). The polarization measurements showed that the IMDZ-B acts as a mixed-type inhibitor. Indeed, it is found that the IMDZ-B compound is a very good inhibitor, and its inhibition efficiency increases with concentration to reach a maximum of 99.5 % at 10-³ M. In addition, the obtained electrochemical parameters from impedance indicated that the IMDZ-B molecules act by adsorption on metallic surfaces. This adsorption was found to obey Langmuir’s adsorption isotherm. However, the temperature effect on the performance of IMDZ-B was also studied. It is found that the IMDZ-B takes its performance at high temperatures. In addition, the obtained kinetic and thermodynamic parameters showed that the IMDZ-B molecules act via two adsorption modes, physisorption and chemisorptions, and its process is endothermic and spontaneous. Finally, the XRD and SEM/EDX analyses confirmed the electrochemical obtained results.

Keywords: low concentration, anti-corrosion brass, IMDZ-B product, phosphoric acid solution, electrochemical, SEM\EDAX analysis

Procedia PDF Downloads 15
56 Synthesis of Tricalcium Phosphate Substituted with Magnesium Ions for Bone Regeneration

Authors: Andreia Cucuruz, Cristina Daniela Ghitulica, Georgeta Voicu, Cristina Busuioc

Abstract:

Ceramics based on calcium phosphates have lately increased attention for tissue engineering because they can be used as substitute bones or for bone regeneration since they mimic very well the nanostructure of tough bone tissue, but also because of other advantages such as a very good biocompatibility and osseointegration. This study aims the preparation and characterization of ceramic materials on the basis of TCP (Ca₃(PO₄)₂), within which calcium ions are substituted by magnesium ions (Mg²⁺) in order to improve the regenerative properties of these materials. TCP-Mg material was synthesized by chemical precipitation method using calcium oxide (CaO) and phosphoric acid (H₃PO₄) as precursors. The objective was to obtain powders with different concentrations of Mg in order to analyze the effect of magnesium ions on the physicochemical properties of phosphate ceramics and in vitro degradation in simulated biological fluid (SBF). Ceramic powders were characterized in vitro but also from the compositional and microstructural point of view. TCP_Mg powders were prepared through wet chemical method from calcium oxide (CaO), magnesium oxide nanopowder (MgO < 50 nm particle size (BET) Sigma Aldrich), phosphoric acid (H₃PO₄ - 85 wt.% in H₂O, 99.99% trace metals basis - Sigma Aldrich). In order to determine the quantities of raw materials, calculations were performed to obtain HAp with Ca/P ratio of 1.5.

Keywords: bone regeneration, magnesium substitution, tricalcium phosphate, tissue engineering

Procedia PDF Downloads 311
55 Investigation of Alumina Membrane Coated Titanium Implants on Osseointegration

Authors: Pinar Erturk, Sevde Altuntas, Fatih Buyukserin

Abstract:

In order to obtain an effective integration between an implant and a bone, implant surfaces should have similar properties to bone tissue surfaces. Especially mimicry of the chemical, mechanical and topographic properties of the implant to the bone is crucial for fast and effective osseointegration. Titanium-based biomaterials are more preferred in clinical use, and there are studies of coating these implants with oxide layers that have chemical/nanotopographic properties stimulating cell interactions for enhanced osseointegration. There are low success rates of current implantations, especially in craniofacial implant applications, which are large and vital zones, and the oxide layer coating increases bone-implant integration providing long-lasting implants without requiring revision surgery. Our aim in this study is to examine bone-cell behavior on titanium implants with an aluminum oxide layer (AAO) on effective osseointegration potential in the deformation of large zones with difficult spontaneous healing. In our study, aluminum layer coated titanium surfaces were anodized in sulfuric, phosphoric, and oxalic acid, which are the most common used AAO anodization electrolytes. After morphologic, chemical, and mechanical tests on AAO coated Ti substrates, viability, adhesion, and mineralization of adult bone cells on these substrates were analyzed. Besides with atomic layer deposition (ALD) as a sensitive and conformal technique, these surfaces were coated with pure alumina (5 nm); thus, cell studies were performed on ALD-coated nanoporous oxide layers with suppressed ionic content too. Lastly, in order to investigate the effect of the topography on the cell behavior, flat non-porous alumina layers on silicon wafers formed by ALD were compared with the porous ones. Cell viability ratio was similar between anodized surfaces, but pure alumina coated titanium and anodized surfaces showed a higher viability ratio compared to bare titanium and bare anodized ones. Alumina coated titanium surfaces, which anodized in phosphoric acid, showed significantly different mineralization ratios after 21 days over other bare titanium and titanium surfaces which anodized in other electrolytes. Bare titanium was the second surface that had the highest mineralization ratio. Otherwise, titanium, which is anodized in oxalic acid electrolyte, demonstrated the lowest mineralization. No significant difference was shown between bare titanium and anodized surfaces except AAO titanium surface anodized in phosphoric acid. Currently, osteogenic activities of these cells on the genetic level are investigated by quantitative real-time polymerase chain reaction (qRT-PCR) analysis results of RUNX-2, VEGF, OPG, and osteopontin genes. Also, as a result of the activities of the genes mentioned before, Western Blot will be used for protein detection. Acknowledgment: The project is supported by The Scientific and Technological Research Council of Turkey.

Keywords: alumina, craniofacial implant, MG-63 cell line, osseointegration, oxalic acid, phosphoric acid, sulphuric acid, titanium

Procedia PDF Downloads 95
54 Selective Separation of Amino Acids by Reactive Extraction with Di-(2-Ethylhexyl) Phosphoric Acid

Authors: Alexandra C. Blaga, Dan Caşcaval, Alexandra Tucaliuc, Madalina Poştaru, Anca I. Galaction

Abstract:

Amino acids are valuable chemical products used in in human foods, in animal feed additives and in the pharmaceutical field. Recently, there has been a noticeable rise of amino acids utilization throughout the world to include their use as raw materials in the production of various industrial chemicals: oil gelating agents (amino acid-based surfactants) to recover effluent oil in seas and rivers and poly(amino acids), which are attracting attention for biodegradable plastics manufacture. The amino acids can be obtained by biosynthesis or from protein hydrolysis, but their separation from the obtained mixtures can be challenging. In the last decades there has been a continuous interest in developing processes that will improve the selectivity and yield of downstream processing steps. The liquid-liquid extraction of amino acids (dissociated at any pH-value of the aqueous solutions) is possible only by using the reactive extraction technique, mainly with extractants of organophosphoric acid derivatives, high molecular weight amines and crown-ethers. The purpose of this study was to analyse the separation of nine amino acids of acidic character (l-aspartic acid, l-glutamic acid), basic character (l-histidine, l-lysine, l-arginine) and neutral character (l-glycine, l-tryptophan, l-cysteine, l-alanine) by reactive extraction with di-(2-ethylhexyl)phosphoric acid (D2EHPA) dissolved in butyl acetate. The results showed that the separation yield is controlled by the pH value of the aqueous phase: the reactive extraction of amino acids with D2EHPA is possible only if the amino acids exist in aqueous solution in their cationic forms (pH of aqueous phase below the isoeletric point). The studies for individual amino acids indicated the possibility of selectively separate different groups of amino acids with similar acidic properties as a function of aqueous solution pH-value: the maximum yields are reached for a pH domain of 2–3, then strongly decreasing with the pH increase. Thus, for acidic and neutral amino acids, the extraction becomes impossible at the isolelectric point (pHi) and for basic amino acids at a pH value lower than pHi, as a result of the carboxylic group dissociation. From the results obtained for the separation from the mixture of the nine amino acids, at different pH, it can be observed that all amino acids are extracted with different yields, for a pH domain of 1.5–3. Over this interval, the extract contains only the amino acids with neutral and basic character. For pH 5–6, only the neutral amino acids are extracted and for pH > 6 the extraction becomes impossible. Using this technique, the total separation of the following amino acids groups has been performed: neutral amino acids at pH 5–5.5, basic amino acids and l-cysteine at pH 4–4.5, l-histidine at pH 3–3.5 and acidic amino acids at pH 2–2.5.

Keywords: amino acids, di-(2-ethylhexyl) phosphoric acid, reactive extraction, selective extraction

Procedia PDF Downloads 391
53 Phosphate Bonded Hemp (Cannabis sativa) Fibre Composites

Authors: Stephen O. Amiandamhen, Martina Meinken, Luvuyo Tyhoda

Abstract:

The properties of Hemp (Cannabis sativa) in phosphate bonded composites were investigated in this research. Hemp hurds were collected from the Hemporium institute for research, South Africa. The hurds were air-dried and shredded using a hammer mill. The shives were screened into different particle sizes and were treated separately with 5% solution of acetic anhydride and sodium hydroxide. The binding matrix was prepared using a reactive magnesia, phosphoric acid, class S fly ash and unslaked lime. The treated and untreated hemp fibers were mixed thoroughly in different ratios with the inorganic matrix. Boric acid and excess water were used to retard and control the rate of the reaction and the setting of the binder. The Hemp composite was formed in a rectangular mold and compressed at room temperature at a pressure of 100KPa. After de-molding the composites, they were cured in a conditioning room for 96 h. Physical and mechanical tests were conducted to evaluate the properties of the composites. A central composite design (CCD) was used to determine the best conditions to optimize the performance of the composites. Thereafter, these combinations were applied in the production of the composites, and the properties were evaluated. Scanning electron microscopy (SEM) was used to carry out the advance examination of the behavior of the composites while X-ray diffractometry (XRD) was used to analyze the reaction pathway in the composites. The results revealed that all properties of phosphate bonded Hemp composites exceeded the LD-1 grade classification of particle boards. The proposed product can be used for ceiling, partitioning, wall claddings and underlayment.

Keywords: CCD, fly ash, magnesia, phosphate bonded hemp composites, phosphoric acid, unslaked lime

Procedia PDF Downloads 412
52 Optical Assessment of Marginal Sealing Performance around Restorations Using Swept-Source Optical Coherence Tomography

Authors: Rima Zakzouk, Yasushi Shimada, Yasunori Sumi, Junji Tagami

Abstract:

Background and purpose: The resin composite has become the main material for the restorations of caries in recent years due to aesthetic characteristics, especially with the development of the adhesive techniques. The quality of adhesion to tooth structures is depending on an exchange process between inorganic tooth material and synthetic resin and a micromechanical retention promoted by resin infiltration in partially demineralized dentin. Optical coherence tomography (OCT) is a noninvasive diagnostic method for obtaining cross-sectional images that produce high-resolution of the biological tissue at the micron scale. The aim of this study was to evaluate the gap formation at adhesive/tooth interface of two-step self-etch adhesives that are preceded with or without phosphoric acid pre-etching in different regions of teeth using SS-OCT. Materials and methods: Round tapered cavities (2×2 mm) were prepared in cervical part of bovine incisors teeth and divided into 2 groups (n=10): first group self-etch adhesive (Clearfil SE Bond) was applied for SE group and second group treated with acid etching before applying the self-etch adhesive for PA group. Subsequently, both groups were restored with Estelite Flow Quick Flowable Composite Resin and observed under OCT. Following 5000 thermal cycles, the same section was obtained again for each cavity using OCT at 1310-nm wavelength. Scanning was repeated after two months to monitor the gap progress. Then the gap length was measured using image analysis software, and the statistics analysis were done between both groups using SPSS software. After that, the cavities were sectioned and observed under Confocal Laser Scanning Microscope (CLSM) to confirm the result of OCT. Results: Gaps formed at the bottom of the cavity was longer than the gap formed at the margin and dento-enamel junction in both groups. On the other hand, pre-etching treatment led to damage the DEJ regions creating longer gap. After 2 months the results showed almost progress in the gap length significantly at the bottom regions in both groups. In conclusions, phosphoric acid etching treatment did not reduce the gap lrngth in most regions of the cavity. Significance: The bottom region of tooth was more exposed to gap formation than margin and DEJ regions, The DEJ damaged with phosphoric acid treatment.

Keywords: optical coherence tomography, self-etch adhesives, bottom, dento enamel junction

Procedia PDF Downloads 185
51 Fractionation of Biosynthetic Mixture of Gentamicins by Reactive Extraction

Authors: L. Kloetzer, M. Poştaru, A. I. Galaction, D. Caşcaval

Abstract:

Gentamicin is an aminoglycoside antibiotic industrially obtained by biosynthesis of Micromonospora purpurea or echinospora, the product being a complex mixture of components with very similar structures. Among them, three exhibit the most important biological activity: gentamicins C1, C1a, C2, and C2a. The separation of gentamicin from the fermentation broths at industrial scale is rather difficult and it does not allow the fractionation of the complex mixture of gentamicins in order to increase the therapeutic activity of the product. The aim of our experiments is to analyze the possibility to selectively separate the less active gentamicin, namely gentamicin C1, from the biosynthetic mixture by reactive extraction with di-(2-ethylhexyl) phosphoric acid (D2EHPA) dissolved in dichloromethane, followed selective re-extraction of the most active gentamicins C1a, C2, and C2a. The experiments on the reactive extraction of gentamicins indicated the possibility to separate selectively the gentamicin C1 from the mixture obtained by biosynthesis. The extraction selectivity is positively influenced by increasing the pH-value of an aqueous solution and by using a D2EHPA concentration in organic phase closer to the value needed for an equimolecular ratio between the extractant and this gentamicin. For quantifying the selectivity of separation, the selectivity factor, calculated as the ratio between the degree of reactive extraction of gentamicin C1 and the overall extraction degree of gentamicins were used. The possibility to remove the gentamicin C1 at an extractant concentration of 10 g l-1 and pH = 8 is presented. In these conditions, it was obtained the maximum value of the selectivity factor of 2.14, which corresponds to the modification of the gentamicin C1 concentration from 31.92% in the biosynthetic mixture to 72% in the extract. The re-extraction of gentamicins C1, C1a, C2, and C2a with sulfuric acid from the extract previously obtained by reactive extraction (mixture A – extract obtained by non-selective reactive extraction; mixture B – extract obtained by selective reactive extraction) allows for separating selectively the most active gentamicins C1a, C2, and C2a. For recovering only the active gentamicins C1a, C2, and C2a, the re-extraction must be carried out at very low acid concentrations, far below those corresponding to the stoichiometry of its chemical reactions with these gentamicins. Therefore, the mixture resulted by re-extraction contained 92.6% gentamicins C1a, C2, and C2a. By bringing together the aqueous solutions obtained by reactive extraction and re-extraction, the overall content of the active gentamicins in the final product becomes 89%, their loss reaching 0.3% related to the initial biosynthetic product.

Keywords: di-(2-ethylhexyl) phosphoric acid, gentamicin, reactive extraction, selectivity factor

Procedia PDF Downloads 281
50 Valorization of Argan Residuals for the Treatment of Industrial Effluents

Authors: Salim Ahmed

Abstract:

The aim of this study was to recover a natural residue in the form of activated carbon prepared from Moroccan "argan pits and date pits" plant waste. After preparing the raw material for manufacture, the carbon was carbonised at 300°C and chemically activated with phosphoric acid of purity 85. The various characterisation results (moisture and ash content, specific surface area, pore volume, etc.) showed that the carbons obtained are comparable to those manufactured industrially and could therefore be tested, for example, in water treatment processes and especially for the depollution of effluents used in the agri-food and textile industries.

Keywords: activated carbon, water treatment, adsorption, argan

Procedia PDF Downloads 29
49 Study on Hydrophilicity of Anodic Aluminum Oxide Templates with TiO2-NTs

Authors: Yu-Wei Chang, Hsuan-Yu Ku, Jo-Shan Chiu, Shao-Fu Chang, Chien-Chon Chen

Abstract:

This paper aims to discuss the hydrophilicity about the anodic aluminum oxide (AAO) template with titania nanotubes (NTs). The AAO templates with pore size diameters of 20-250 nm were generated by anodizing 6061 aluminum alloy substrates in acid solution of sulfuric acid (H2SO4), oxalic acid (COOH)2, and phosphoric acid (H3PO4), respectively. TiO2-NTs were grown on AAO templates by the sol-gel deposition process successfully. The water contact angle on AAO/TiO2-NTs surface was lower compared to the water contact angle on AAO surface. So, the characteristic of hydrophilicity was significantly associated with the AAO pore size and what kinds of materials were immersed variables.

Keywords: AAO, nanotube, sol-gel, anodization, hydrophilicity

Procedia PDF Downloads 316
48 Fabrication of SnO₂ Nanotube Arrays for Enhanced Gas Sensing Properties

Authors: Hsyi-En Cheng, Ying-Yi Liou

Abstract:

Metal-oxide semiconductor (MOS) gas sensors are widely used in the gas-detection market due to their high sensitivity, fast response, and simple device structures. However, the high working temperature of MOS gas sensors makes them difficult to integrate with the appliance or consumer goods. One-dimensional (1-D) nanostructures are considered to have the potential to lower their working temperature due to their large surface-to-volume ratio, confined electrical conduction channels, and small feature sizes. Unfortunately, the difficulty of fabricating 1-D nanostructure electrodes has hindered the development of low-temperature MOS gas sensors. In this work, we proposed a method to fabricate nanotube-arrays, and the SnO₂ nanotube-array sensors with different wall thickness were successfully prepared and examined. The fabrication of SnO₂ nanotube arrays incorporates the techniques of barrier-free anodic aluminum oxide (AAO) template and atomic layer deposition (ALD) of SnO₂. First, 1.0 µm Al film was deposited on ITO glass substrate by electron beam evaporation and then anodically oxidized by five wt% phosphoric acid solution at 5°C under a constant voltage of 100 V to form porous aluminum oxide. As the Al film was fully oxidized, a 15 min over anodization and a 30 min post chemical dissolution were used to remove the barrier oxide at the bottom end of pores to generate a barrier-free AAO template. The ALD using reactants of TiCl4 and H₂O was followed to grow a thin layer of SnO₂ on the template to form SnO₂ nanotube arrays. After removing the surface layer of SnO₂ by H₂ plasma and dissolving the template by 5 wt% phosphoric acid solution at 50°C, upright standing SnO₂ nanotube arrays on ITO glass were produced. Finally, Ag top electrode with line width of 5 μm was printed on the nanotube arrays to form SnO₂ nanotube-array sensor. Two SnO₂ nanotube-arrays with wall thickness of 30 and 60 nm were produced in this experiment for the evaluation of gas sensing ability. The flat SnO₂ films with thickness of 30 and 60 nm were also examined for comparison. The results show that the properties of ALD SnO₂ films were related to the deposition temperature. The films grown at 350°C had a low electrical resistivity of 3.6×10-3 Ω-cm and were, therefore, used for the nanotube-array sensors. The carrier concentration and mobility of the SnO₂ films were characterized by Ecopia HMS-3000 Hall-effect measurement system and were 1.1×1020 cm-3 and 16 cm3/V-s, respectively. The electrical resistance of SnO₂ film and nanotube-array sensors in air and in a 5% H₂-95% N₂ mixture gas was monitored by Pico text M3510A 6 1/2 Digits Multimeter. It was found that, at 200 °C, the 30-nm-wall SnO₂ nanotube-array sensor performs the highest responsivity to 5% H₂, followed by the 30-nm SnO₂ film sensor, the 60-nm SnO₂ film sensor, and the 60-nm-wall SnO₂ nanotube-array sensor. However, at temperatures below 100°C, all the samples were insensitive to the 5% H₂ gas. Further investigation on the sensors with thinner SnO₂ is necessary for improving the sensing ability at temperatures below 100 °C.

Keywords: atomic layer deposition, nanotube arrays, gas sensor, tin dioxide

Procedia PDF Downloads 211
47 Nonconventional Method for Separation of Rosmarinic Acid: Synergic Extraction

Authors: Lenuta Kloetzer, Alexandra C. Blaga, Dan Cascaval, Alexandra Tucaliuc, Anca I. Galaction

Abstract:

Rosmarinic acid, an ester of caffeic acid and 3-(3,4-dihydroxyphenyl) lactic acid, is considered a valuable compound for the pharmaceutical and cosmetic industries due to its antimicrobial, antioxidant, antiviral, anti-allergic, and anti-inflammatory effects. It can be obtained by extraction from vegetable or animal materials, by chemical synthesis and biosynthesis. Indifferent of the method used for rosmarinic acid production, the separation and purification process implies high amount of raw materials and laborious stages leading to high cost for and limitations of the separation technology. This study focused on separation of rosmarinic acid by synergic reactive extraction with a mixture of two extractants, one acidic (acid di-(2ethylhexyl) phosphoric acid, D2EHPA) and one with basic character (Amberlite LA-2). The studies were performed in experimental equipment consisting of an extraction column where the phases’ mixing was made by mean of a perforated disk with 45 mm diameter and 20% free section, maintained at the initial contact interface between the aqueous and organic phases. The vibrations had a frequency of 50 s⁻¹ and 5 mm amplitude. The extraction was carried out in two solvents with different dielectric constants (n-heptane and dichloromethane) in which the extractants mixture of varying concentration was dissolved. The pH-value of initial aqueous solution was varied between 1 and 7. The efficiency of the studied extraction systems was quantified by distribution and synergic coefficients. For calculating these parameters, the rosmarinic acid concentration in the initial aqueous solution and in the raffinate have been measured by HPLC. The influences of extractants concentrations and solvent polarity on the efficiency of rosmarinic acid separation by synergic extraction with a mixture of Amberlite LA-2 and D2EHPA have been analyzed. In the reactive extraction system with a constant concentration of Amberlite LA-2 in the organic phase, the increase of D2EHPA concentration leads to decrease of the synergic coefficient. This is because the increase of D2EHPA concentration prevents the formation of amine adducts and, consequently, affects the hydrophobicity of the interfacial complex with rosmarinic acid. For these reasons, the diminution of synergic coefficient is more important for dichloromethane. By maintaining a constant value of D2EHPA concentration and increasing the concentration of Amberlite LA-2, the synergic coefficient could become higher than 1, its highest values being reached for n-heptane. Depending on the solvent polarity and D2EHPA amount in the solvent phase, the synergic effect is observed for Amberlite LA-2 concentrations over 20 g/l dissolved in n-heptane. Thus, by increasing the concentration of D2EHPA from 5 to 40 g/l, the minimum concentration value of Amberlite LA-2 corresponding to synergism increases from 20 to 40 g/l for the solvent with lower polarity, namely, n-heptane, while there is no synergic effect recorded for dichloromethane. By analysing the influences of the main factors (organic phase polarity, extractant concentration in the mixture) on the efficiency of synergic extraction of rosmarinic acid, the most important synergic effect was found to correspond to the extractants mixture containing 5 g/l D2EHPA and 40 g/l Amberlite LA-2 dissolved in n-heptane.

Keywords: Amberlite LA-2, di(2-ethylhexyl) phosphoric acid, rosmarinic acid, synergic effect

Procedia PDF Downloads 254
46 Optimization of Synergism Extraction of Toxic Metals (Lead, Copper) from Chlorides Solutions with Mixture of Cationic and Solvating Extractants

Authors: F. Hassaine-Sadi, S. Chelouaou

Abstract:

In recent years, environmental contamination by toxic metals such as Pb, Cu, Ni, Zn ... has become a worldwide crucial problem, particularly in some areas where the population depends on groundwater for drinking daily consumption. Thus, the sources of metal ions come from the metal manufacturing industry, fertilizers, batteries, paints, pigments and so on. Solvent extraction of metal ions has given an important role in the development of metal purification processes such as the synergistic extraction of some divalent cations metals ( M²⁺), the ions metals from various sources. This work consists of a water purification technique that involves the lead and copper systems: Pb²⁺, H₃O+, Cl⁻ and Cu²⁺, H₃O⁺, Cl⁻ for diluted solutions by a mixture of tri-n-octylphosphine oxide (TOPO) or Tri-n-butylphosphate(TBP) and di (2-ethyl hexyl) phosphoric acid (HDEHP) dissolved in kerosene. The study of the fundamental parameters influencing the extraction synergism: cation exchange/extraction solvent have been examined.

Keywords: synergistic extraction, lead, copper, environment

Procedia PDF Downloads 408
45 Fabrication and Characterization of Cadmium Sulfide Nanowires on Aluminum Oxide Template

Authors: Malik Imran Afzal

Abstract:

Cadmium supplied nanowires have unique electrical and optical properties and applications. To obtain cadmium supplied nanowires with regular and good aspect ratio, they can be synthesized by template synthesis method. Porous anodized aluminum oxide is the most promising template with regular hexagonal shapes. Their aspect ratio can be controlled by controlling the pores’ depth and diameter which greatly depend on anodization voltage and temperature of the electrolyte. In this research, high purity aluminium was used to prepare nanotemplates at 5-6°C in 1M phosphoric acid and cadmium supplied was deposited electrochemically using a co-solution of thiourea, cadmium acetate and ammonium acetate. pH was maintained at 11 in a heat bath at 75°C with the help of aqueous ammonia solution. Both porous anodized alumina and cadmium supplied nanowires were characterized suing SEM. A good quality Nanowires were obtained in bunches with reasonably high aspect ratio.

Keywords: bunches, electrodeposition, hexagonal, thiourea

Procedia PDF Downloads 291
44 A FR Fire-Off with Polysilicic Acid for Pes/Co Blends

Authors: Raziye Atakan, Ebru Celebi, Gulay Ozcan, Neda Soydan, A. Sezai Sarac

Abstract:

In this study, a novel polymeric flame retardant chemical with phosphorous-nitrogen synergism was synthesized by polyvinyl alcohol (PVA), hydrophilic polyester resin (PR), phosphoric acid and dicyandiamide (DCDA). Polyester/Cotton (Pes/Co) blend fabrics were treated via pad-dry-cure process with this synthesized chemical. PVA (PR)-P-DCDA has shown that it is an effective flame retardant on the fabrics. In order to improve durable flame retardancy for cotton part of the blend, polysilicic acid and citric acid monohydrate auxiliaries were added in FR finishing bath at different concentrations. Flammability and characteristic properties of the sample were tested according to relevant ISO standard and procedures. To do so, ISO 6940 vertical flammability test, TGA, DTA, LOI and FTIR analysis have been performed. The obtained results showed that this new finishing formulation is a good char-forming agent for the PES/CO blends and polysilicic acid could be used for cellulosic blends with PVA (PR)-P-DCDA.

Keywords: flame retardancy, flammability, Pes/Co blends, polysilicic acid

Procedia PDF Downloads 373
43 Vitamin B9 Separation by Synergic Pertraction

Authors: Blaga Alexandra Cristina, Kloetzer Lenuta, Bompa Amalia Stela, Galaction Anca Irina, Cascaval Dan

Abstract:

Vitamin B9 is an important member of vitamins B group, being a growth factor, important for making genetic material as DNA and RNA, red blood cells, for building muscle tissues, especially during periods of infancy, adolescence and pregnancy. Its production by biosynthesis is based on the high metabolic potential of mutant Bacillus subtilis, due to a superior biodisponibility compared to that obtained by chemical pathways. Pertraction, defined as the extraction and transport through liquid membranes consists in the transfer of a solute between two aqueous phases of different pH-values, phases that are separated by a solvent layer of various sizes. The pertraction efficiency and selectivity could be significantly enhanced by adding a carrier in the liquid membrane, such as organophosphoric compounds, long chain amines or crown-ethers etc., the separation process being called facilitated pertraction. The aim of the work is to determine the impact of the presence of two extractants/carriers in the bulk liquid membrane, i.e. di(2-ethylhexyl) phosphoric acid (D2EHPA) and lauryltrialkylmetilamine (Amberlite LA2) on the transport kinetics of vitamin B9. The experiments have been carried out using two pertraction equipments for a free liquid membrane or bulk liquid membrane. One pertraction cell consists on a U-shaped glass pipe (used for the dichloromethane membrane) and the second one is an H-shaped glass pipe (used for h-heptane), having 45 mm inner diameter of the total volume of 450 mL, the volume of each compartment being of 150 mL. The aqueous solutions are independently mixed by means of double blade stirrers with 6 mm diameter and 3 mm height, having the rotation speed of 500 rpm. In order to reach high diffusional rates through the solvent layer, the organic phase has been mixed with a similar stirrer, at a similar rotation speed (500 rpm). The area of mass transfer surface, both for extraction and for reextraction, was of 1.59x10-³ m2. The study on facilitated pertraction with the mixture of two carriers, namely D2EHPA and Amberlite LA-2, dissolved in two solvents with different polarities: n-heptane and dichloromethane, indicated the possibility to obtain the synergic effect. The synergism has been analyzed by considering the vitamin initial and final mass flows, as well as the permeability factors through liquid membrane. The synergic effect has been observed at low D2EHPA concentrations and high Amberlite LA-2 concentrations, being more important for the low-polar solvent (n-heptane). The results suggest that the mechanism of synergic pertraction consists on the reaction between the organophosphoric carrier and vitamin B9 at the interface between the feed and membrane phases, while the aminic carrier enhances the hydrophobicity of this compound by solvation. However, the formation of this complex reduced the reextraction rate and, consequently, affects the synergism related to the final mass flows and permeability factor. For describing the influences of carriers concentrations on the synergistic coefficients, some equations have been proposed by taking into account the vitamin mass flows or permeability factors, with an average deviations between 4.85% and 10.73%.

Keywords: pertraction, synergism, vitamin B9, Amberlite LA-2, di(2-ethylhexyl) phosphoric acid

Procedia PDF Downloads 240
42 Comparative Catalytic Activity of Some Ferrites for Phenol Degradation in Aqueous Solutions

Authors: Bayan Alqassem, Israa A. Othman, Mohammed Abu Haija, Fawzi Banat

Abstract:

The treatment of wastewater from highly toxic pollutants is one of the most challenging issues for humanity. In this study, the advanced oxidation process (AOP) was employed to study the catalytic degradation of phenol using different ferrite catalysts which are CoFe₂O₄, CrFe₂O₄, CuFe₂O₄, MgFe₂O₄, MnFe₂O₄, NiFe₂O₄ and ZnFe₂O₄. The ferrite catalysts were prepared via sol-gel and co-precipitation methods. Different ferrite composites were also prepared either by varying the metal ratios or incorporating chemically reduced graphene oxide in the ferrite cluster. The effect of phosphoric acid treatment on the copper ferrite activity. All of the prepared catalysts were characterized using infrared spectroscopy (IR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The ferrites catalytic activities were tested towards phenol degradation using high performance liquid chromatography (HPLC). The experimental results showed that ferrites prepared through sol-gel route were more active than those of the co-precipitation method towards phenol degradation. In both cases, CuFe₂O₄ exhibited the highest degradation of phenol compared to the other ferrites. The photocatalytic properties of the ferrites were also investigated.

Keywords: ferrite catalyst, ferrite composites, phenol degradation, photocatalysis

Procedia PDF Downloads 176
41 Rapid Method for Low Level 90Sr Determination in Seawater by Liquid Extraction Technique

Authors: S. Visetpotjanakit, N. Nakkaew

Abstract:

Determination of low level 90Sr in seawater has been widely developed for the purpose of environmental monitoring and radiological research because 90Sr is one of the most hazardous radionuclides released from atmospheric during the testing of nuclear weapons, waste discharge from the generation nuclear energy and nuclear accident occurring at power plants. A liquid extraction technique using bis-2-etylhexyl-phosphoric acid to separate and purify yttrium followed by Cherenkov counting using a liquid scintillation counter to determine 90Y in secular equilibrium to 90Sr was developed to monitor 90Sr in the Asia Pacific Ocean. The analytical performance was validated for the accuracy, precision, and trueness criteria. Sr-90 determination in seawater using various low concentrations in a range of 0.01 – 1 Bq/L of 30 liters spiked seawater samples and 0.5 liters of IAEA-RML-2015-01 proficiency test sample was performed for statistical evaluation. The results had a relative bias in the range from 3.41% to 12.28%, which is below accepted relative bias of ± 25% and passed the criteria confirming that our analytical approach for determination of low levels of 90Sr in seawater was acceptable. Moreover, the approach is economical, non-laborious and fast.

Keywords: proficiency test, radiation monitoring, seawater, strontium determination

Procedia PDF Downloads 124
40 Effect of Preparation Temperature on Producing Graphene Oxide by Chemical Oxidation Approach

Authors: Rashad Al-Gaashani, Muataz A. Atieh

Abstract:

In this study, the effect of preparation temperature, namely room temperature (RT), 40, 60, and 85°C, on producing of high-quality graphene oxide (GO) has been investigated. GO samples have been prepared by chemical oxidation of graphite via a safe improved chemical technique using a blend of two deferent acids: sulphuric acid (H₂SO₄) and phosphoric acid (H₃PO₄) with volume ratio 4:1, respectively. potassium permanganate (KMnO₄) and hydrogen peroxide (H₂O₂) were applied as oxidizing agents. In this work, sodium nitrate (NaNO₃) was excluded, so the emission of hazardous explosive gases such as NO₂ and N₂O₂ was shunned. Ice and oil baths were used to carefully control the temperature. Several characterization instruments including X-Ray diffraction, transmission electron microscopy, scanning electron microscopy, electron dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and UV-vis spectroscopy were used to study and compare the synthesized samples. The results indicated that GO can be prepared at RT with graphite oxide, and the purity of GO increased with rising of the solvent temperature. Optical properties of GO samples were studied using UV-vis absorption spectra.

Keywords: chemical method, graphite, graphene oxide, optical properties

Procedia PDF Downloads 121
39 Innovative Grafting of Polyvinylpyrrolidone onto Polybenzimidazole Proton Exchange Membranes for Enhanced High-Temperature Fuel Cell Performance

Authors: Zeyu Zhou, Ziyu Zhao, Xiaochen Yang, Ling AI, Heng Zhai, Stuart Holmes

Abstract:

As a promising sustainable alternative to traditional fossil fuels, fuel cell technology is highly favoured due to its enhanced working efficiency and reduced emissions. In the context of high-temperature fuel cells (operating above 100 °C), the most commonly used proton exchange membrane (PEM) is the Polybenzimidazole (PBI) doped phosphoric acid (PA) membrane. Grafting is a promising strategy to advance PA-doped PBI PEM technology. The existing grafting modification on PBI PEMs mainly focuses on grafting phosphate-containing or alkaline groups onto the PBI molecular chains. However, quaternary ammonium-based grafting approaches face a common challenge. To initiate the N-alkylation reaction, deacidifying agents such as NaH, NaOH, KOH, K2CO3, etc., can lead to ionic crosslinking between the quaternary ammonium group and PBI. Polyvinylpyrrolidone (PVP) is another widely used polymer, the N-heterocycle groups within PVP endow it with a significant ability to absorb PA. Recently, PVP has attracted substantial attention in the field of fuel cells due to its reduced environmental impact and impressive fuel cell performance. However, due to the the poor compatibility of PVP in PBI, few research apply PVP in PA-doped PBI PEMs. This work introduces an innovative strategy to graft PVP onto PBI to form a network-like polymer. Due to the absence of quaternary ammonium groups, PVP does not pose issues related to crosslinking with PBI. Moreover, the nitrogen-containing functional groups on PVP provide PBI with a robust phosphoric acid retention ability. The nuclear magnetic resonance (NMR) hydrogen spectrum analysis results indicate the successful completion of the grafting reaction where N-alkylation reactions happen on both sides of the grafting agent 1,4-bis(chloromethyl)benzene. On one side, the reaction takes place with the hydrogen atoms on the imidazole groups of PBI, while on the other side, it reacts with the terminal amino group of PVP. The XPS results provide additional evidence from the perspective of the element. On synthesized PBI-g-PVP surfaces, there is an absence of chlorine (chlorine in grafting agent 1,4-bis(chloromethyl)benzene is substituted) element but a presence of sulfur element (sulfur element in terminal amino PVP appears in PBI), which demonstrates the occurrence of the grafting reaction and PVP is successfully grafted onto PBI. Prepare these modified membranes into MEA. It was found that during the fuel cell operation, all the grafted membranes showed substantial improvement in maximum current density and peak power density compared to unmodified one. For PBI-g-PVP 30, with a grafting degree of 22.4%, the peak power density reaches 1312 mW cm⁻², marking a 59.6% enhancement compared to the pristine PBI membrane. The improvement is caused by the improved PA binding ability of the membrane after grafting. The AST test result shows that the grafting membranes have better long-term durability and performance than unmodified membranes attributed to the presence of added PA binding sites, which can effectively prevent the PA leaching caused by proton migration. In conclusion, the test results indicate that grafting PVP onto PBI is a promising strategy which can effectively improve the fuel cell performance.

Keywords: fuel cell, grafting modification, PA doping ability, PVP

Procedia PDF Downloads 31