Abstract: Recovery of pure copper and silver from end-of-life photovoltaic (PV) panels was investigated in this paper using an effective hybrid pyro-hydrometallurgical process. In the first step of waste treatment, solar panel waste was first dismantled to obtain a PV sheet to be cut and calcined at 500 °C, to separate out PV ribbon from glass cullet, ash, and volatile while the silicon wafer containing silver finger was collected for recovery. In the second step of metal recovery, copper recovery from PV ribbon was via 1-3 M HCl leaching with SnCl₂ and H₂O₂ additions in order to remove the tin-lead coating on the ribbon. The leached copper band was cleaned and subsequently melted as an anode for the next step of electrorefining. Stainless steel was set as the cathode with CuSO₄ as an electrolyte, and at a potential of 0.2 V, high purity copper of 99.93% was obtained at 96.11% recovery after 24 hours. For silver recovery, the silicon wafer containing silver finger was leached using HNO₃ at 1-4 M in an ultrasonic bath. In the next step of precipitation, silver chloride was then obtained and subsequently reduced by sucrose and NaOH to give silver powder prior to oxy-acetylene melting to finally obtain pure silver metal. The integrated recycling process is considered to be economical, providing effective recovery of high purity metals such as copper and silver while other materials such as aluminum, copper wire, glass cullet can also be recovered to be reused commercially. Compounds such as PbCl₂ and SnO₂ obtained can also be recovered to enter the market.
Abstract: Neodymium-iron-boron (NdFeB) magnets classified as high-power magnets are widely used in various applications such as automotive, electrical and medical devices. Because significant amounts of rare earth metals will be subjected to shortages in the future, therefore domestic NdFeB magnet waste recycling should therefore be developed in order to reduce social and environmental impacts towards a circular economy. Each type of wastes has different characteristics and compositions. As a result, these directly affect recycling efficiency as well as types and purity of the recyclable products. This research, therefore, focused on the recycling of manufacturing NdFeB magnet waste obtained from the sintering stage of magnet production and the waste contained 23.6% Nd, 60.3% Fe and 0.261% B in order to recover high purity neodymium oxide (Nd2O3) using hybrid metallurgical process via oxidative roasting and selective leaching techniques. The sintered NdFeB waste was first ground to under 70 mesh prior to oxidative roasting at 550–800 oC to enable selective leaching of neodymium in the subsequent leaching step using H2SO4 at 2.5 M over 24 h. The leachate was then subjected to drying and roasting at 700–800 oC prior to precipitation by oxalic acid and calcination to obtain Nd2O3 as the recycling product. According to XRD analyses, it was found that increasing oxidative roasting temperature led to an increasing amount of hematite (Fe2O3) as the main composition with a smaller amount of magnetite (Fe3O4) found. Peaks of Nd2O3 were also observed in a lesser amount. Furthermore, neodymium iron oxide (NdFeO3) was present and its XRD peaks were pronounced at higher oxidative roasting temperatures. When proceeded to acid leaching and drying, iron sulfate and neodymium sulfate were mainly obtained. After the roasting step prior to water leaching, iron sulfate was converted to form Fe2O3 as the main compound, while neodymium sulfate remained in the ingredient. However, a small amount of Fe3O4 was still detected by XRD. The higher roasting temperature at 800 oC resulted in a greater Fe2O3 to Nd2(SO4)3 ratio, indicating a more effective roasting temperature. Iron oxides were subsequently water leached and filtered out while the solution contained mainly neodymium sulfate. Therefore, low oxidative roasting temperature not exceeding 600 oC followed by acid leaching and roasting at 800 oC gave the optimum condition for further steps of precipitation and calcination to finally achieve Nd2O3.
Abstract: The transition to a more sustainable economy is directed by a reduction in the consumption of raw materials in equivalent production. The recovery of byproducts and especially the dredged sediment as mineral addition in cements matrix represents an alternative to reduce raw material consumption and construction sector’s carbon footprint. However, the efficient use of sediment requires adequate and optimal treatment. Several processing techniques have so far been applied in order to improve some physicochemical properties. The heat treatment by calcination was effective in removing the organic fraction and activates the pozzolanic properties. In this article, the effect of the optimized heat treatment of marine sediments in the physico-mechanical and environmental properties of mortars are shown. A finding is that the optimal substitution of a portion of cement by treated sediments by calcination at 750 °C helps to maintain or improve the mechanical properties of the cement matrix in comparison with a standard reference mortar. The use of calcined sediment enhances mortar behavior in terms of mechanical strength and durability. From an environmental point of view and life cycle, mortars formulated containing treated sediments are considered inert with respect to the inert waste storage facilities reference (ISDI-France).
Abstract: Tricalcium phosphate (β-Ca3(PO4)2, β-TCP) powders were synthesized using wet polymeric precipitation method for the first time to our best knowledge. The results of X-ray diffraction analysis showed the formation of almost single a Ca-deficient hydroxyapatite (CDHA) phase of a poor crystallinity already at room temperature. With continuously increasing the calcination temperature up to 800 °C, the crystalline β-TCP was obtained as the main phase. It was demonstrated that infrared spectroscopy is very effective method to characterize the formation of β-TCP. The SEM results showed that β-TCP solids were homogeneous having a small particle size distribution. The β-TCP powders consisted of spherical particles varying in size from 100 to 300 nm. Fabricated β-TCP specimens were placed to the bones of the rats and maintained for 1-2 months.
Abstract: Calcined kaolinite clay (CKC) is a pozzolanic material that is current drawing research attention. This work investigates the conditions for the best performance of a CKC from a kaolinite clay source in Ajebo, Abeokuta (southwest Nigeria) known for its commercial availability. Samples from this source were subjected to X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). XRD shows that kaolinite is the main mineral in the clay source. This mineral is responsible for the pozzolanic behavior of CKC. DSC indicates that the transformation from the clay to CKC occurred between 550 and 750 oC. Using this temperature range, clay samples were milled and different CKC samples were produced in an electric muffle furnace using temperatures of 550, 600, 650, 700, 750 and 800 oC respectively for 1 hour each. This was also repeated for 2 hours. The degree of de-hydroxylation (dtg) and strength activity index (SAI) were also determined for each of the CKC samples. The dtg and SAI tests were repeated two more times for each sample and averages were taken. Results showed that peak dtg occurred at 750 oC for 1 hour calcining combination (94.27%) whereas marginal differences were recorded at some lower temperatures (90.97% for 650 oC for 2 hours; 91.05% for 700 oC for 1 hour and 92.77% for 700 oC for 2 hours). Optimum SAI was reported at 700 oC for 1 hour (99.05%). Rating SAI as a better parameter than dtg, 700 oC for 1 hour combination was adopted as the best calcining condition. The paper recommends the adoption of this clay source for pozzolan production by adopting the calcining conditions established in this work.
Abstract: Solar-light activated titanium dioxide photocatalysts were prepared by hydrolysis of titanium (IV) isopropoxide with thiourea, followed by calcinations at 450 °C. The experiments demonstrated that methyl orange in aqueous solutions were successfully degraded under solar light using doped TiO2. The photocatalytic oxidation of a mono azo methyl-orange dye has been investigated in multi ion doped TiO2 and solar light. Solutions were irradiated by solar-light until high removal was achieved. It was found that there was no degradation of methyl orange in the dark and in the absence of TiO2. Varieties of laboratory prepared TiO2 catalysts both un-doped and doped using titanium (IV) isopropoxide and thiourea as a dopant were tested in order to compare their photoreactivity. As a result, it was found that the efficiency of the process strongly depends on the working conditions. The highest degradation rate of methyl orange was obtained at optimum dosage using commercially produced TiO2. Our work focused on laboratory synthesized catalyst and the maximum methyl orange removal was achieved at 81% with catalyst loading of 0.04 g/L, initial pH of 3 and methyl orange concentration of 0.005 g/L using multi-ion doped catalyst. The kinetics of photocatalytic methyl orange dye stuff degradation was found to follow a pseudo-first-order rate law. The presence of the multi-ion dopant (thiourea) enhanced the photoefficiency of the titanium dioxide catalyst.
Abstract: The layered structure LiNi1/3Co1/3Mn1/3-xAlxO2 (x = 0 ~
0.04) series cathode materials were synthesized by a carbonate
co-precipitation method, followed by a high temperature calcination
process. The influence of Al substitution on the microstructure and
electrochemical performances of the prepared materials was
investigated by X-Ray diffraction (XRD), scanning electron
microscopy (SEM), and galvanostatic charge/discharge test. The
results show that the LiNi1/3Co1/3Mn1/3-xAlxO2 has a well-ordered
hexagonal α-NaFeO2 structure. Although the discharge capacity of
Al-doped samples decreases as x increases,
LiNi1/3Co1/3Mn1/3-0.02Al0.02O2 exhibits superior capacity retention at
high voltage (4.6 V). Therefore, LiNi1/3Co1/3Mn1/3-0.02Al0.02O2 is a
promising material for “green” vehicles.
Abstract: The conventional ceramic route was utilized to
prepare a hard magnetic powder (M-type strontium ferrite,
SrFe12O19). The stoichiometric mixture of iron oxide and strontium
carbonate were calcined at 1000oC and then fired at various
temperatures. The influence of various reaction parameters such as
mixing ratio, calcination temperature, firing temperature and firing
time on the magnetic behaviors of the synthesized magnetic powder
were investigated. The magnetic properties including Coercivity
(Hc), Magnetic saturation (Ms), and Magnetic remnance (Mr) were
measured by vibrating sample magnetometer. Morphologically the
produced magnetic powder has a dense hexagonal grain shape
structure.
Abstract: The aim of this study was to investigate the
photocatalytic activity of polycrystalline phases of bismuth tungstate
of formula Bi2WO6. Polycrystalline samples were elaborated using a
coprecipitation technique followed by a calcination process at
different temperatures (300, 400, 600 and 900°C). The obtained
polycrystalline phases have been characterized by X-ray diffraction
(XRD), scanning electron microscopy (SEM), and transmission
electron microscopy (TEM). Crystal cell parameters and cell volume
depend on elaboration temperature. High-resolution electron
microscopy images and image simulations, associated with X-ray
diffraction data, allowed confirming the lattices and space groups
Pca21. The photocatalytic activity of the as-prepared samples was
studied by irradiating aqueous solutions of Rhodamine B, associated
with Bi2WO6 additives having variable crystallite sizes. The
photocatalytic activity of such bismuth tungstates increased as the
crystallite sizes decreased. The high specific area of the
photocatalytic particles obtained at 300°C seems to condition the
degradation kinetics of RhB.
Abstract: The synthesis of CuFe2O4 spinel powders by an
optimized combustion-like process followed by calcination is
described herein. The samples were characterized using X-ray
diffraction (XRD), differential thermal analysis (TG/DTA), scanning
electron microscopy (SEM), dilatometry and 4-probe DC methods.
Different glycine to nitrate (G/N) ratios of 1 (fuel-deficient), 1.48
(stoichiometric) and 2 (fuel-rich) were employed. Calcining the asprepared
powders at 800 and 1000°C for 5 hours showed that the G/N
ratio of 2 results in the formation of the desired copper spinel single
phase at both calcination temperatures. For G/N=1, formation of
CuFe2O4 takes place in three steps. First, iron and copper nitrates
decompose to iron oxide and pure copper. Then, copper transforms to
copper oxide and finally, copper and iron oxides react with each other
to form a copper ferrite spinel phase. The electrical conductivity and
the coefficient of thermal expansion of the sintered pelletized
samples were 2 S.cm-1 (800°C) and 11×10-6 °C-1 (25-800°C),
respectively.
Abstract: Although, lanthanum carbonate has not been approved
by the FDA for treatment of hyperphosphatemia, we prospectively
evaluated the efficacy of the combination of Calcium hydroxyapatite
(CHAp) and Lanthanum Carbonate (LaC) for the treatment of
hyperphosphatemia on mice. CHAp was prepared by co-precipitation
method using Ca(OH)2, H3PO4, NH4OH with calcination at 1200ºC.
Lanthanum carbonate was prepared by chemical method using
NaHCO3 and LaCl3 at low pH environment, below 4.0. The
structures were characterized by FTIR spectra and SEM -EDX
analysis. The study group included 16 subjects-mice divided into four
groups according to the administered substance: lanthanum carbonate
(group A), CHAp (group B), lanthanum carbonate + CHAp (group C)
and salt water (group D). The results indicate a phosphate decrease
when subjects (mice) were treated with CHAp and lanthanum
carbonate (0.5% CMC), in a single dose of 1500 mg/kg. Serum
phosphate concentration decreased [(from 4.5 ± 0.8 mg/dL) to
4.05 ± 0.2 mg/dL), P < 0.01] in group A and in group C (to 3.6
± 0.2 mg/dL) at 12 hours from the administration. The combination
of CHAp and lanthanum carbonate is a suitable regimen for
hyperphosphatemia treatment because it avoids both the
hypercalcemia of CaCO3 and the adverse effects of CHAp.
Abstract: Nanofibers of PVA /nickel nitrate/silica/alumina
izopropoxide/boric acid composite were prepared by using sol-gel
processing and electrospinning technique. By high temperature
calcinations of the above precursor fibers, nanofibers of
NiO/Al2O3/B2O3/SiO2 composite with diameters about 500 nm
could be successfully obtained. The fibers were characterized by
XRD and SEM analyses.
Abstract: The development of active and stable catalysts
without noble metals for low temperature oxidation of exhaust gases
remains a significant challenge. The purpose of this study is to
determine the influence of the preparation method on the catalytic
activity of the supported copper-manganese mixed oxides in terms of
VOCs oxidation. The catalysts were prepared by impregnation of γ-
Al2O3 with copper and manganese nitrates and acetates and the
possibilities for CO, CH3OH and dimethyl ether (DME) oxidation
were evaluated using continuous flow equipment with a four-channel
isothermal stainless steel reactor. Effect of the support, Cu/Mn mole
ratio, heat treatment of the precursor and active component loading
were investigated. Highly active alumina supported Cu-Mn catalysts
for CO and VOCs oxidation were synthesized. The effect of
preparation conditions on the activity behavior of the catalysts was
discussed.
The synergetic interaction between copper and manganese species
increases the activity for complete oxidation over mixed catalysts.
Type of support, calcination temperature and active component
loading along with catalyst composition are important factors,
determining catalytic activity. Cu/Mn molar ratio of 1:5, heat
treatment at 450oC and 20 % active component loading are the best
compromise for production of active catalyst for simultaneous
combustion of CO, CH3OH and DME.
Abstract: Magnetic powder of Sr-ferrite was prepared by
conventional and sol-gel auto-combustion methods. In conventional
method, strontium carbonate and ferric oxide powders were mixed
together and then mixture was calcined. In sol-gel auto-combustion
method, a solution containing strontium nitrate, ferric nitrate and
citric acid was heated until the combustion took place automatically;
then, as-burnt powder was calcined. Thermal behavior, phase
identification, morphology and magnetic properties of powders
obtained by these two methods were compared by DTA, XRD, SEM
and VSM techniques. According to the results of DTA analysis,
formation temperature of Sr-ferrite obtained by conventional and solgel
auto-combustion methods were 1300°C and 1000°C, respectively.
XRD results confirmed the formation of pure Sr-ferrite at the
mentioned temperatures. Plate and hexagonal-shape particles of Srferrite
were observed using SEM. The Sr-ferrite powder obtained by
sol-gel auto-combustion method had saturation magnetization of
66.03 emu/g and coercivity of 5731 Oe in comparison with values of
58.20 emu/g and 4378 Oe obtained by conventional method.
Abstract: In this paper, strontium ferrite (SrO.6Fe2O3) was
synthesized by the sol-gel auto-combustion process. The thermal
behavior of powder obtained from self-propagating combustion of
initial gel was evaluated by simultaneous differential thermal analysis
(DTA) and thermo gravimetric (TG), from room temperature to
1200°C. The as-burnt powder was calcined at various temperatures
from 700-900°C to achieve the single-phase Sr-ferrite. Phase
composition, morphology and magnetic properties were investigated
using X-ray diffraction (XRD), transmission electron microscopy
(TEM) and vibrating sample magnetometry (VSM) techniques.
Results showed that the single-phase and nano-sized hexagonal
strontium ferrite particles were formed at calcination temperature of
800°C with crystallite size of 27 nm and coercivity of 6238 Oe.
Abstract: Strontium hexaferrite (SrFe12O19; Sr-ferrite) is one of
the well-known materials for permanent magnets. In this study, Mtype
strontium ferrite was prepared by following the conventional
ceramic method from steelmaking by-product. Initial materials;
SrCO3 and by-product, were mixed together in the composition of
SrFe12O19 in different Sr/Fe ratios. The mixtures of these raw
materials were dry-milled for 6h. The blended powder was presintered
(i.e. calcination) at 1000°C for different times periods, then
cooled down to room temperature. These pre-sintered samples were
re-milled in a dry atmosphere for 1h and then fired at different
temperatures in atmospheric conditions, and cooled down to room
temperature. The produced magnetic powder has a dense hexagonal
grain shape structure. The calculated energy product values for the
produced samples ranged from 0.3 to 2.4 MGOe.
Abstract: In this study, fish bone waste was used as a new
catalyst for biodiesel production. Instead of discarding the fish bone
waste, it will be utilized as a source for catalyst that can provide
significant benefit to the environment. Also, it can be substitute as a
calcium oxide source instead of using eggshell, crab shell and snail
shell. The XRD and SEM analysis proved that calcined fish bone
contains calcium oxide, calcium phosphate and hydroxyapatite. The
catalyst was characterized using Scanning Electron Microscope
(SEM) and X-ray Diffraction (XRD).
Abstract: Calcium oxide (CaO) as carbon dioxide (CO2)
adsorbent at the elevated temperature has been very well-received
thus far. The CaO can be synthesized from natural calcium carbonate
(CaCO3) sources through the reversible calcination-carbonation
process. In the study, cockle shell has been selected as CaO
precursors. The objectives of the study are to investigate the
performance of calcination and carbonation with respect to different
temperature, heating rate, particle size and the duration time. Overall,
better performance is shown at the calcination temperature of 850oC
for 40 minutes, heating rate of 20oC/min, particle size of < 0.125mm
and the carbonation temperature is at 650oC. The synthesized
materials have been characterized by nitrogen physisorption and
surface morphology analysis. The effectiveness of the synthesized
cockle shell in capturing CO2 (0.72 kg CO2/kg adsorbent) which is
comparable to the commercialized adsorbent (0.60 kg CO2/kg
adsorbent) makes them as the most promising materials for CO2
capture.
Abstract: The production of biodiesel from crude palm oil with
a homogeneous base catalyst is unlikely owing to considerable
formation of soap. Free fatty acids (FFA) in crude palm oil need to
be reduced, e.g. by esterification. This study investigated the activity
of sulfated zirconia calcined at various temperatures for esterification
of FFA in crude palm oil to biodiesel. It was found that under a
proper reaction condition, sulfated zirconia well catalyzes
esterification. FFA content can be reduced to an acceptable value for
typical biodiesel production with a homogeneous base catalyst.
Crystallinity and sulfate attachment of sulfated zirconia depend on
calcination temperature during the catalyst preparation. Too low
temperature of calcination gives amorphous sulfated zirconia which
has low activity for esterification of FFA. In contrast, very high
temperature of calcination removes sulfate group, consequently,
conversion of FFA is reduced. The appropriate temperature range of
calcination is 550-650 oC.
Abstract: In this study, ZnO nano rods and ZnO ultrafine particles were synthesized by Gel-casting method. The synthesized ZnO powder has a hexagonal zincite structure. The ZnO aggregates with rod-like morphology are typically 1.4 μm in length and 120 nm in diameter, which consist of many small nanocrystals with diameters of 10 nm. Longer wires connected by many hexahedral ZnO nanocrystals were obtained after calcinations at the temperature over 600° C.The crystalline structures and morphologies of the powder have been characterized by X-ray diffraction(XRD) and Scaning electron microscopy (SEM).The result shows that the different preparation conditions such as concentration H2O, calcinations time and calcinations temperature have a lot of influences upon the properties of nano ZnO powders, an increase in the temperature of the calcinations results in an increase of the grain size and also the increase of the calcinations time in high temperature makes the size of the grains bigger. The existences of extra watter prevent nano grains from improving like rod morphology. We have obtained the smallest grain size of ZnO powder by controlling the process conditions. Finally In a suitable condition, a novel nanostructure, namely bi-rod-like ZnO nano rods was found which is different from known ZnO nanostructures.