Journal of Environmental Management 212 (2018) 278e291

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Journal of Environmental Management

journal homepage: www.elsevier.com/locate/jenvman

Research article

Enhanced alumina recovery from secondary aluminum dross for high

purity nanostructured g-alumina powder production: Kinetic study
Mostafa Mahinroosta, Ali Allahverdi*
Research Laboratory of Inorganic Chemical Process Technologies, School of Chemical Engineering, Iran University of Science and Technology, Narmak 16846-
13114, Tehran, Iran

a r t i c l e i n f o a b s t r a c t

Article history: The numerous ecological problems caused by the accumulation of secondary aluminum dross (SAD) as a
Received 23 October 2017 hazardous waste generated in aluminum castings have necessitated a need for a sustainable recycling
Received in revised form solution. This study proposes a novel and green leaching-based process for recovery of nano-alumina as a
29 January 2018
highly valuable material from SAD. The leaching phase was performed at atmospheric pressure and low
Accepted 2 February 2018
Available online 22 February 2018
temperature. To obtain optimum conditions for the recovery process, the dissolution kinetics and
mechanism of SAD in hydrochloric acid were initially studied under a given liquid-to-solid ratio of 20 ml/
g, various reaction temperatures and times. It was found that the dissolution of SAD in HCl was
Keywords:
Aluminum dross
controlled by layer diffusion with an apparent activation energy of around 10.49 kJ/mol. Alumina in the
Nano alumina form of a high purity nanostructured powder from SAD was then recovered under optimum conditions of
Kinetics 85
C, acid concentration of 5 mol/l, and reaction time of 120 min by the proposed process. Character-
Waste treatment ization of nano-alumina was performed using X-ray diffractometry (XRD), Fourier transform infrared
Nanostructure (FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), energy-dispersive X-ray
spectroscopy (EDAX), and transmission electron microscopy (TEM) techniques. The results revealed that
the as-produced alumina had a nano-crystalline structure, having the crystal size of 15.90 nm and
consisting mainly of gamma phase. The microstructural studies disclosed the aggregations of rounded-
corner shaped particles. Also, wet chemical analysis showed a purity of more than 98% for the produced
alumina.
© 2018 Elsevier Ltd. All rights reserved.

1. Introduction Chemical and mineralogical composition of aluminum dross

depend on raw material and metallurgical process used in pro-
The improper management of various types of solid wastes (e.g. duction (Das et al., 2007). The main phases present in aluminum
industrial, municipal and agricultural) results in serious environ- dross include aluminum metal, Fe2O3, SiO2, Na2O, AlN, Al2O3, NaCl,
mental outcomes such as water toxicity (Melnyk et al., 2014). One MgO$Al2O3, and traces of KCl, cryolite (Na3AlF6), aluminum carbide
way to manage the waste is to recycle or reuse it as the feedstock for (Al4C3), and small amounts of fluoride and chloride compounds. In
production of valuable products (e.g. biodiesel, biofuel, etc.) other studies, however, components such as MgF2, NaAlCl4, KAlCl4,
(Hanifzadeh et al., 2017; Kim et al., 2017). One of the industrial solid MgO, KMgF3, and K2NaAlF6 have also been reported in addition to
wastes with many environmental issues is aluminum dross. It is a the aforementioned chemicals (Dash et al., 2008; Sarker et al.,
solid oxidic compound waste of aluminum smelting process 2015). Aluminum dross can also be generated from treatment of
formed when molten aluminum comes in contact with air in its molten aluminum scraps such as drinking cans with molten salt
outer surface (Dash et al., 2008; Sarker et al., 2015). For every flux (Manfredi et al., 1997). The molten salt flux accumulates on the
1000 kg of molten aluminum, an average of about 15e25 kg of surface of the molten metal resulting in the formation of dross or
aluminum dross is generated (Nai and Ming-Shean, 2013). skim (Adeosun, 2014). There are two types of aluminum dross
including primary dross (also called white dross or wet dross)
(Abdulkadir et al., 2015) and secondary dross (other common
names: black or dry dross) (Adeosun, 2014; Yoo et al., 2011). These
* Corresponding author.
E-mail addresses: m_mahinroosta@chemeng.iust.ac.ir (M. Mahinroosta), ali. two types of dross are different from each other in terms of
allahverdi@iust.ac.ir (A. Allahverdi). aluminum metal content and the amount of soluble salts and oxidic

https://doi.org/10.1016/j.jenvman.2018.02.009
0301-4797/© 2018 Elsevier Ltd. All rights reserved.
 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291 279

compounds (Yoo et al., 2011). Primary dross contains approxi- underground water consequently resulting in serious concerns of
mately 80% of aluminum metal and small amounts of oxidic and water pollution (Meshram and Singh, 2018). In addition, when
salt constituents in the form of clump (Abdulkadir et al., 2015), aluminum dross comes in contact with moisture or water vapor,
whereas secondary dross contains about 5e10% of aluminum metal toxic and flammable gases such as NH3, CH4, PH3, H2, and H2S etc.
and large amounts of oxidic and salt compounds (Adeosun, 2014; may be generated (Das et al., 2007; Murayama et al., 2012). Due to
Nai and Ming-Shean, 2013). Primary dross is generally returned the aforementioned issues, the adoption of an appropriate recy-
to smelter for the purpose of recycling of remaining aluminum cling solution is of particular importance.
metal. At this stage, the salt flux is used to minimize oxidation There are two possible ways to manage secondary dross: py-
(Dash et al., 2008; Nai and Ming-Shean, 2013). Salt flux is mainly rometallurgical and hydrometallurgical processes. The former is
prepared based on an equimolar combination of NaCl-KCl with faced with the problem of high energy consumption and usually
about 10% of fluoride additives such as NaF, cryolite, or KF to requires relatively high temperature treatments and reducing
improve coagulation and therefore the melting process (Ramesh agents (Unlu and Drouet, 2002). Since the latter is a method with
and Yogeshwar, 1997). The oxides present in dross form a long low capital and production costs, together with the high efficiency
continuous network in which aluminum metal has been trapped. and favorable environmental aspects (Havlik, 2008), it can be a
The molten flux smashes this framework, thereby releasing the promising route for the future and an interesting way to recover
metal trapped inside. As a result, coalescence of molten aluminum and process secondary dross. Hydrometallurgical processes can be
droplets is facilitated and eventually, the droplets flow down into performed through alkaline or acidic routes (Tsakiridis et al., 2013).
the aluminum bath. In most cases, salt flux is applied to maximize An accurate understanding of the kinetics of dissolution is required
the recycling of aluminum metal and also to reduce the amount of in order to interpret the complex behavior of leaching process, and
impurities in final aluminum products (Das et al., 2007; Dash et al., to optimize the performance of hydrometallurgical operation (Irena
2008). In some cases, various alloying elements are utilized along et al., 2016). Therefore, the study of dissolution kinetics of sec-
with the salt flux for the production of aluminum alloys. The dross ondary aluminum dross in acid or base can be of great importance,
obtained at this stage is known as secondary dross or alloy dross especially for the purpose of the production of nanostructured
(Dash et al., 2008). alumina powder as a very high valuable material. The dissolution
Disposal of the secondary dross generated in the process of kinetics of aluminum dross in hydrochloric acid and the rate-
aluminum smelting is a global issue and a serious challenge for determining step (RDS) of the dissolution reactions have not been
aluminum manufacturers from the view point of ecological prob- reported in the literature, yet. The first aim of this work is to
lems (Adeosun, 2014; Das et al., 2007). A large portion of the pro- investigate these issues for the first time. As the second aim within
duced secondary dross is discarded in the vicinity of factories that the scope of this study, the preparation of nanostructured alumina
more likely causes the toxic metal ions to enter the surface and powder using a green leaching-based process will be discussed.

2. Materials and methods

2.1. Materials

Secondary aluminum dross (SAD) was supplied from an

aluminum company located in Arak province, Iran. Hydrochloric
acid (37 w/w%), sodium hydroxide (99% purity), and ammonia 25%
were purchased from Merck (Darmstadt, Germany) and used
without any additional purification. Distilled water was used at all
stages of the experiment.

2.2. Experimental procedure

2.2.1. Dissolution experiments

After sampling by quartering and coning method (Brittain,
2002) and before performing any dissolution test, the sample was
dried in an oven at 105
C. This is done to neutralize the effect of the
moisture content of the sample in the dissolution efficiency cal-
culations. For the purpose of dissolution experiments of the SAD in
hydrochloric acid, the experimental setup (shown in Fig. 1)
including a three-neck glass reactor, Graham condenser, water
bath, and magnetic stirrer equipped with a temperature probe (IKA
C-MAG HS7 Digital) was used. After carefully weighing, 5 g of the
SAD was poured into the reactor at the specified temperatures and
atmospheric pressure. Then, 100 ml of HCl with optimum concen-
tration was added to it. The reaction between the SAD and hydro-
chloric acid begins under a certain stirrer speed (500 rpm). After
any dissolution experiment at the given temperature and time, the
suspension was filtered through an ash-less filter paper of What-
man to separate the insoluble residues. After burning the filter
paper inside the crucible, the solid residues were washed several
times with distilled water and then dried at 105
C in an oven.
Finally, after the weight of the crucible was fixed, the amount of
Fig. 1. The experimental setup used for the SAD dissolution tests. solid residues was obtained. For temperatures higher than ambient
280 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291

temperature, to stop or slow down the reaction, the reactor was and production of hazardous materials. Green chemistry includes
immediately placed in a cold water bath. twelve principles covering various concepts of 1) prevention; 2)
One-Factor-At-a Time (OFAT) approach was used for the opti- Atom economy; 3) Less hazardous chemical syntheses; 4)
mization of experiments. This approach involves sequential ex- Designing safer chemicals; 5) Safer solvents and auxiliaries; 6)
periments where one factor is varied at a time and the other ones Design for energy efficiency; 7) Use of renewable feedstock; 8)
are held constant. This process is repeated until an optimal com- Reducing derivatives; 9) Catalysis; 10) Design for degradation; 11)
bination of factors is found which gives the best results. In order to Real-time analysis for pollution prevention; and 12) Inherently
investigate the effect of acid concentration on dissolution efficiency safer chemistry for accident prevention (Anastas and Warner,
of the SAD, experiments were performed using 1, 2, 3, 4, 5, and 1998). Since, in this work, the developed process reuses and re-
6 mol/l HCl at ambient temperature. At this stage the optimum acid duces a hazardous solid waste (prevention), alumina as the final
concentration is selected for subsequent experiments including product is not a toxic substance (Less hazardous chemical synthe-
investigation of the influence of temperature on the dissolution ses), the leaching and precipitating agents have a relatively low
efficiency of the SAD, which are conducted at three temperatures of concentration resulting in less environmental hazards (Safer sol-
20, 55, and 75
C unless otherwise said. vents and auxiliaries), the extraction stage as the heart of the
process is performed at ambient temperature and pressure (Design
for energy efficiency), and the used chemicals and reagents mini-
2.2.2. Alumina production mize the potential for releases, explosion, and fires (Inherently
The sequence of operations for the production of alumina from safer chemistry for accident prevention), the proposed process
the SAD is depicted in Fig. 2. The dissolution stage will be discussed implies to the principles 1, 3, 5, 6, and 12 of the twelve principles of
in detail in sections 3.2e3.6. The chloride solution achieved at the green chemistry, respectively. It is clear that other principles are not
first stage under the optimized dissolution conditions, contains related to the process. Also, the overall process increases recycla-
metal cationic impurities such as Ca2þ, Mg2þ, Fe3þ, etc. Therefore, bility of a hazardous waste implying to sustainable chemistry
to obtain highly pure alumina, it is necessary to remove these im- principles.
purities. For this purpose, initially the pH of the chloride solution
was adjusted to 3e5 to precipitate metal hydroxides. Then,
aluminum hydroxide as an amphoteric material was separated 2.2.3. Measurement methods and complementary techniques
from the other metal hydroxides by adding 3 N NaOH. In this way, Particle size distribution of the SAD was obtained using sieving.
aluminum hydroxide enters into the solution phase in the form of The wire sieves were selected according to ASTM standard E11. To
sodium aluminate and the other metal hydroxides remain as a sol obtain particle size distribution, the nest of sieves was subjected to
which are easily removed by filtration. In the next step, aluminum agitation, which causes the powder sample to distribute between
hydroxide gel appeared by adding dilute hydrochloric acid. After the sieves. Agitation was created using vibration.
that, to remove any soluble ionic contaminants, the produced gel Chemical composition of the SAD sample was analyzed using
was rinsed several times with a mixture of ethanol and deionized ED2000 X-ray fluorescence (XRF) analyzer (Oxford, England) based
water until the pH reaches 7.0e7.5. Finally, to obtain alumina as the on ISO/IEC 17025:2005 standard. For mineralogical study, Philips
targeted product, dehydroxylation of the aluminum hydroxide Expert System X-ray diffractometer was used with CuKa-radiation
dried at 105
C was carried out at 700
C for 2 h. and Ni-filter at 40 kV and 30 mA. The XRD tests were performed at
As an important point, the described recovery process is in the 2q range of 10e80
with a scanning rate of 2
/min, an anti-scatter
framework of green chemistry. Green chemistry is the design of and receiving slit of 1
and 0.01 mm, respectively. Fourier transform
chemical products and processes that decline or eliminate the use infrared (FTIR) spectroscopy was carried out using a SHIMADZU (IR
Spectrophotometer 8400s) FTIR spectrometer in transmittance
mode from 400 to 4000 cm1 using standard KBr technique. All
spectra were obtained with a sensitivity of 4 cm and 64 scans per
spectrum taken. Purity of the as-produced nano alumina was
determined using Zn-EDTA back titration. For this purpose, the
alumina obtained from the proposed process was dissolved in a
mixture of acids. Then, the solution was poured into a conical flask
followed by adding 0.01 mol/l EDTA and buffer solution (pH ¼ 10).
In the next step, the solution was boiled for a few minutes to
accelerate the formation of Al-EDTA complex. Five drops of Erio-
chrome black T indicator was then added and mixed so that the
solution becomes blue in color. Excess of EDTA was titrated with
0.01 mol/l ZnSO4 solution until the color change to wine red as the
endpoint. The volume of the ZnSO4 consumed in titration was used
for the determination of purity. Micrographs of the raw SAD and
dissolution residues were prepared using a TESCAN VEGA II (Czech
Republic) Scanning Electron Microscope device at an accelerating
voltage of 30 kV in the secondary electron (SE) mode of the device.
To make the samples conductive they were coated with a gold layer.
Microstructural study of the as-produced alumina was conducted
using SIGMA VP-500 FESEM microscope (ZEISS) at accelerating
voltage of 15 kV. This microscope was equipped with an EDAX
probe (Oxford Instrument, England) for elemental analysis. TEM
analysis was performed using PHILIPS CEM12 microscope at oper-
ating voltage and vacuum pressure of 120 kV and 106 Pa,
Fig. 2. Suggested flow sheet for the synthesis of alumina from SAD. respectively.
 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291 281

sample. It was found that about 55% of the SAD was smaller than
250 mm, whereas about 90% of the SAD sample was smaller than
2.38 mm.
Table 1 presents physical properties and chemical composition
(determined by X-ray fluorescence technique (XRF)) of the SAD.
The results of chemical analysis show that SAD contains a high
percentage of aluminum oxide.
The mineralogical phases of the SAD were investigated by X-ray
powder diffractometry (XRD). Fig. 4 shows the XRD pattern of the
SAD. According to Fig. 4, the crystalline phases are corundum (a-
Al2O3), quartz (SiO2), graphite, villiaumite (NaF), fluorite (CaF2),
spinel (MgAl2O4), aluminum nitride (AlN), halite (NaCl), dia-
oyudaoite (NaAl11O17) as well as a small amount of aluminum metal
(Al).
NaCl, NaF, and CaF2 originate from the molten salt flux, which is
used during the melting process, in order to protect the aluminum
metal from oxidation in the reactive atmosphere. One more thing
about NaF is that it is also formed as the result of the decomposition
of cryolite (Na3AlF6) which is used as an electrolyte in the melting
Fig. 3. SAD particle size distribution obtained through the standard sieving. process in addition to its role in lowering the melting point of
alumina for the extraction of aluminum metal in aluminum in-
dustry. The corundum (also known as a-alumina) comes from the
Table 1 reaction of the atmospheric oxygen with metallic aluminum
Chemical composition and physical properties of SAD.
molten at high temperatures. Spinel is as a consequence of oxida-
Physical properties tion of magnesium as an alloying element present in the aluminum
Appearance Gray to blackish scrap during remelting.
Bulk density (g/cm3) 0.85 Considering both data given in Table 1 and phases determined
Actual densitya (g/cm3) 2.22 by XRD, it can be deduced that the oxides reported by XRF tech-
Chemical composition (wt.%)
nique are present as real phases as brought in Table 2.
Al2O3 61.74
SiO2 14.96 The other phases were below the XRD detection limit.
CaO 2.56
Fe2O3 4.42
MgO 2.56 3.2. Primary dissolution tests
SO3 0.17
K2O 0.86 The drying curve of the sample is shown in Fig. 5.
Na2O 2.85
As can be seen, the moisture content of the sample is 14 wt/wt %,
TiO2 0.32
MnO 0.30 which is completely removed after 50 min of drying in oven at
CuO 0.11 105
C. After drying, the sample was kept in a desiccator containing
SrO 0.14 silica gel as desiccant for next tests.
a
Obtained according to ASTM standard C188. Fig. 6a illustrates a schema of the dissolution reaction between
HCl and SAD in which oxide materials of the SAD enter into the
3. Results and discussion solution phase and are then separated from the insoluble solids. As
seen in Fig. 6b, the surface of SAD particles is gradually covered by a
3.1. Characterization of the SAD newly generated metal chloride layer, which is so concentrated that
blocks the diffusion of HCl species considerably. Hence, for a solid
Fig. 3 shows the results of the particle size analysis of the SAD SAD particle, the dissolution process can be divided into several

Fig. 4. XRD pattern of secondary aluminum dross.

282 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291

Table 2 usually controlled by the slowest stage, a decisive task should be

Real form(s) of oxide compounds in SAD composition. performed to find the RDS.
Oxide in XRF Real form(s) determined by XRD The reaction of acid with SAD results in the release of a gas from
report mixture. The gas was shown in previous studies to be hydrogen
Al2O3 Mainly as: corundum, spinel, aluminum nitride, and (David and Kopac, 2012) and is produced through reaction (1):
diaoyudaoite
Few as: Al metal and cryolite 2Alþ6HCl/2AlCl3þ3H2[ (1)
SiO2 Quartz
CaO Fluorite
Na2O Villiaumite, halite, diaoyudaoite, and cryolite All the other possible reactions in the dissolution stage are as
MgO Spinel follows:

Al2O3þ6HCl/2AlCl3þ3H2O (2)

Fe2O3þ6HCl/2FeCl3þ3H2O (3)

MgO$Al2O3þ8HCl/2AlCl3þMgCl2þ4H2O (4)

CaF2þ2HCl/CaCl2þ2HF (5)

NaF þ HCl/NaCl þ HF (6)

AlNþ3HCl/AlCl3þNH3 (7)

Na3AlF6þ6HCl/3NaCl þ AlCl3þ6HF (8)

Diaoyudaoite reacts with hydrochloric acid according to the

Fig. 5. Drying curve of SAD sample. following reaction (Shi et al., 2012):

NaAl11O17þ34HCl/NaClþ11AlCl3þ17H2O (9)
stages: 1) diffusion of HCl from solution to the external surface of
SAD particle, known as transitional layer diffusion; 2) diffusion of Fig. 7 depicts SAD particles before and after dissolution in HCl.
HCl through the metal chloride layer to the reaction interface; and As can be seen, amount, color, and the size of SAD particles have
3) chemical reaction at the interface and diffusion of metal cations greatly been changed after dissolution reactions. The chemical
into the bulk solution. Inasmuch as the overall reaction rate is nature and morphological changes of the solid residues will be

Fig. 6. a) Schema of the reaction between HCl and SAD particles, b) dissolution model of a SAD particle in HCl.
 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291 283

Fig. 7. SAD particles before (a) and after (b) dissolution in HCl.

discussed in detail in section 3.8. can be deduced from visual changes of the material (Tiwari et al.,
2015). However, more precise decision-making on choosing the
3.3. Effect of acid concentration temperature and time of the dissolution must be done using
advanced techniques and analyses (as given in section 3.8).
The effect of acid concentration on the dissolution of the SAD Some more dissolution experiments were conducted at 85
C at
was investigated for HCl concentrations of 1, 2, 3, 4, 5, and 6 mol/l at three different times of 15, 60 and 120 min which will be discussed
ambient temperature and the results are depicted in Fig. 8. in section 3.8 using complementary techniques. To investigate
The results show that acid concentration greatly affects the more carefully the effect of temperature on the dissolution effi-
dissolution efficiency of the SAD. The highest dissolution rate was ciency of the SAD in 5 mol/l HCl, experiments were followed at
observed in the first 15 min. After this time, the SAD dissolution three selected temperatures of 20, 55, and 75
C. The results in
increase was less rapid. As the concentration of HCl increases to Fig. 11 show that the temperature plays an important role in the
5 mol/l, the dissolution efficiency of the SAD is accelerated. As dissolution of the SAD in HCl. This can be brought about by the
clearly observed, the further increase of acid concentration to enhancement of Hþ ion activity resulting in a faster dissolution rate
6 mol/l causes the dissolution efficiency to be dropped. The reasons and a higher efficiency. A dissolution efficiency of about 78% can be
for this are more likely related to less acid ionization in water and achieved with enhancement of the temperature to 75
C.
decline of the solubility of saturated AlCl3 (Cui et al., 2013). The
highest dissolution efficiency was attained about 62% using 5 mol/l 3.5. Kinetic models
HCl. So, the acid concentration of 5 mol/l was chosen as the opti-
mum concentration for subsequent experiments.
According to Levenspiel (1999), for non-catalytic reaction of
Fig. 9 shows solution samples removed from the reactor at room
particles with a surrounding gas/liquid fluid, the contracting vol-
temperature, at different dissolution times in 5 mol/l HCl. These
ume, Ginstling-Brounstein-Crank, Jander, and Avrami-Erofeyev ki-
samples have been obtained after filtration of reaction solution
netic models can be considered for dissolution kinetics. The
using Whatman ash-less filter paper.
reaction rate of the heterogeneous system is controlled by the
It can be observed from Fig. 9 that with the enhancement of
diffusion through the liquid film surrounding the solid particles, the
time at a specified dissolution temperature, tendency of the SAD to
diffusion through the product layer or by the chemical reactions at
the reaction with HCl increases accompanied by color change
the surface of the core of the unreacted materials. In this paper, the
which implies the entrance of more constituents into the solution
phase over dissolution time. The appearance of yellow color is due
to the presence of more iron ions in the solution phase due to the
increased dissolution of Fe2O3 in HCl with time (Cui et al., 2015).

3.4. Effect of temperature

Fig. 10 shows solution samples taken from the reactor at

different temperatures, at a prescribed dissolution time. Fig. 10
clarifies that tendency of the SAD to react with HCl increases
with enhancement of the temperature.
The reason for choosing a reaction time of 15 min for visual
observations is to investigate possible changes in SAD dissolution
with increasing temperature in a relatively short time. Time and
temperature are two important parameters in leaching and disso-
lution experiments. The dissolution at a high temperature and in a
short time may lead to a high rate of leaching or dissolution and Fig. 8. Dissolution of SAD as a function of time and acid concentration at ambient
also a relatively good dissolution efficiency, which at first glance temperature.
284 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291

1-(1-a)1/3 ¼ MkcCAt/dr ¼ k1t (10)

which is identified as contracting volume kinetic model, and is

located in category of geometrical contraction models applied for
chemically controlled-processes;

1 þ 2(1-a)-3(1-a)2/3 ¼ 6uMDCAt/dr2 ¼ k2t (11)

which is known as Ginstling-Brounstein-Crank model, and is a

diffusion model used for processes that are controlled through the
diffusion into the layer of porous products;

[1-(1-a)1/3]2 ¼ k3t (12)

which is referred as Jander's model, and is a three-dimensional

diffusion model quite suitable for describing the kinetics of solid-
state reactions with powdered reactants satisfactorily if the ex-
periments are conducted carefully; and

-ln(1-a)¼(k4t)m (13)

which is known as Avrami-Erofeyev model, and is prevalently used

for many solid-state reactions which have been described by
nucleation mechanisms (Khawam and Flanagan, 2006). In the
above-mentioned equations, kc (m/min) is the first order reaction
rate constant; M (kg/mol) is molecular weight of solid reactants; CA
(mol/m3) is the leachant concentration; D (m2/min) is the diffusion
coefficient; d (kg/m3) is bulk density of the particles, r (m) is initial
radius of the particle; a is reacted part at time t; k1 (m/min) and k2
Fig. 9. The color variation of solution phase resulted from SAD dissolution in HCl after (m2/min) are total reaction rate constants and u is stoichiometric
a) 10, b) 15, c) 30, d) 60, e) 90, and f) 120 min at room temperature. (For interpretation
of the references to color in this figure legend, the reader is referred to the Web version
of this article.)

aforementioned kinetic models and activation energy were taken

into consideration to analyze the reaction mechanism of the SAD
dissolution in HCl.
A model is not the real world but merely a human construct to
provide a better understanding of the real world systems. Key
features in common with the development of any model is that:
simplifying assumptions must be made; boundary conditions or
initial conditions must be identified; and the range of applicability
of the model should be understood. In solid-state reactions, a
model can describe a particular reaction type and translate that
mathematically into a rate equation. In general, two types of
models have been proposed for solid-state kinetics including
mechanistic-based and empirically-based models. The
mechanistic-based models typically have a tangible, physical
aspect, in that system components are real, solid and visible. In the
empirically-based models, mathematics facilitates data analysis
with little mechanistic meaning (Crundwell, 2013). Therefore,
different rate expressions are produced from these models. In solid-
state kinetics, mechanistic interpretations usually involve identi-
fying a reasonable reaction model because information about in-
dividual reaction steps is often difficult to obtain. In the systems
containing solid reactants, chemical reactions occur at the interface
of the reactants. Then diffusion through the products must take
place for protraction of the reactions, if this happens the chemical
reactions will progress at the interface of one of or all the reactants.
The mechanism of these stages depends on experimental condi-
tions and properties of solid reactants. Therefore, the overall rate of
the reaction may be controlled by chemical kinetics and/or trans-
Fig. 10. The color variation of solution phase resulted from the SAD dissolution in 5 M
port phenomena. The most important kinetic models which are
HCl after 15 min at a) 20, b) 40, c) 55, d) 65, e) 75, and f) 85
C. (For interpretation of the
prevalently used to study such reactions are as follows (Ahmed references to color in this figure legend, the reader is referred to the Web version of
et al., 2012; Alafara et al., 2009): this article.)
 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291 285

specified temperature.

3.6. Estimating the activation energy

The temperature dependence of the overall reaction rate con-

stant is expressed by the Arrhenius equation:

k ¼ Aexp(-Ea/RT) (14)

in which k is overall reaction constant (m/min); A is coefficient of

frequency (min1); Ea is activation energy (J/mol); R is universal gas
constant (8.314 J/mol.K); and T (K) is the reaction temperature.
Arrhenius equation can be rewritten in logarithmic form:

lnk ¼ lnA-Ea/RT (15)

Fig. 11. Effect of temperature on dissolution efficiency of SAD in 5 M HCl.

By drawing lnk in terms of the reverse reaction temperature, a

line is obtained. The slope of the line involves activation energy.
Fig. 16 shows such a plot for the dissolution reaction of the SAD in
HCl.
According to the line shown in Fig. 16, the slope of the line,
namely -Ea/R is equal to 1262.7 resulting in the activation energy
of 10.49 kJ/mol. An apparent activation energy of about 41 kJ/mol
has been obtained for the aluminum dross dissolution in sec-butyl
alcohol (Yoo et al., 2011). The frequency factor, A, is obtained from
the intercept of the line that is about 0.0449 min1. Finally, the
kinetic equation of the SAD dissolution reaction in HCl is obtained
according to the following equation:

[1-(1-a)1/3]2 ¼ 0.0449exp(-10490/RT)t (16)

Generally, high values of activation energy (>40 kJ/mol) should

Fig. 12. Plots of 1-(1-a)1/3 versus dissolution time of SAD in HCl at three various
temperatures. indicate a chemical reaction controlled process while the low
values of activation energy (<20 kJ/mol) should show a diffusion-
controlled process (Gharabaghi et al., 2013). It is already reported
coefficient. that some diffusion-controlled reactions could also have a high
To determine which of kinetic models (10) to (13) is applicable activation energy and it appears that the rate controlling mecha-
for the mechanism of the SAD dissolution reaction with hydro- nism of heterogeneous dissolution reactions is sometimes pre-
chloric acid, experimental data are plotted based on equations dicted with more efficiency from plots of the kinetics equations
(10)e(13). The results are displayed in Figs. 12e15. rather than from the activation energy value (Chen et al., 2013;
The correlation coefficients of the fitted models in Figs. 12e15 Gbor et al., 2000).
are given in Table 3. According to the data in Table 3, it is clear
that Jander's model fits experimental data better than the other 3.7. Characterization of as-produced nano alumina
models. This means that the reaction rate is controlled through the
internal diffusion to the layer of solid particles in the dissolution 3.7.1. X-ray diffractometry study
process. According to Jander's model presented in equation (12), Fig. 17 shows the XRD pattern of the as-produced nano alumina.
the slopes of the lines indicate the reaction rate constants at a It can be observed that the material exhibits a high crystallinity

Fig. 13. Plots of 1 þ 2(1-a)-3(1-a)2/3 versus dissolution time of SAD in HCl at three Fig. 14. Plots of [1-(1-a)1/3]2 versus dissolution time of SAD in HCl at three various
various temperatures. temperatures.
286 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291

Fig. 16. Plotting Arrhenius equation for experimental data of SAD dissolution in HCl.

highly crystalline having the crystal size of about 15.90 nm esti-

mated using Lorentzian profile in XPowder software (Fig. 18).

3.7.2. Determination of chemical bonds

Fig. 19 illustrates the FTIR spectrum of the as-produced nano
alumina. The band at around 592 cm1 is attributed to symmetric
bending of Al-O-Al (Blonski and Garofalini, 1993). The band
observed at 1140 is due to the existence of cluster of Al3þ and O2
ions on the surface of Al-O vibration. The absorption band at
1655 cm1 is related to the bending vibration of H-O-H bonds in
hydration water. In a study on FTIR spectroscopy of water sorption
on alumina surfaces, it was found that the symmetric and asym-
metric OH stretching vibrations have band centers at 3462 and
3763 cm1 (Al-Abadleh and Grassian, 2003). In a similar finding, it
has been stated that the bands appeared at the two aforementioned
bands are due to the stretching vibration of eOH which is more
likely due to the moisture adsorbed on the surface of the material
(Lee et al., 2013).

Fig. 15. Plots of Avrami-Erofeyev equation versus dissolution time of SAD in HCl at 3.7.3. Chemical composition
three various temperatures for (a) m ¼ 1, (b) m ¼ 2, and (c) m ¼ 3. Based on Zn-EDTA back titration method which has been
described in section 2.2.3, the purity of the as-produced nano
alumina was found to be around 98.52%. The alumina with a purity
with characteristic peaks of g-, k-, and q-phases. The standard cards
of more than 90% has commercial applications (Salahudeen et al.,
of ICDD-29-1486, ICDD-29-0063, and ICDD-10-0425 were used for
2015). Since, the as-produced alumina in this work satisfies the
identification of g-phase of alumina (Chauruka et al., 2015). The q-
minimum purity, it can be potentially used for commercial appli-
phase was determined according to the standard cards of ICDD-35-
cations such as preparation of catalyst, catalyst support, adsorbent,
0121, ICDD-11-0517, and ICDD-23-1009. The kappa phase was
etc.
recognized using ICDD-04-0878 standard card (Santos et al., 2000).
The XRD pattern shows that the as-produced nano alumina is

Table 3
Correlation coefficients of the fitted models on the experimental data.

Model Dissolution temperature

T ¼ 20
C T ¼ 55
C T ¼ 75
C
2 2
Contracting volume model R ¼ 0.8586 R ¼ 0.8239 R2 ¼ 0.8247
Ginstling-Brounstein-Crank R2 ¼ 0.9686 R2 ¼ 0.9162 R2 ¼ 0.9026
model
Jander's model R2 ¼ 0.9791 R2 ¼ 0.9427 R2 ¼ 0.9301
Avrami-Erofeyev model m¼1 R2 ¼ 0.8988 R2 ¼ 0.8686 R2 ¼ 0.8690
m¼2 R2 ¼ 0.7962 R2 ¼ 0.7840 R2 ¼ 0.7964
m¼3 R2 ¼ 0.7556 R2 ¼ 0.7529 R2 ¼ 0.93
Fig. 17. XRD pattern of the as-synthesized nano alumina from SAD.
 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291 287

various temperatures determined by XRD are presented in Fig. 22.

As can be obviously seen from Fig. 22, at room temperature and
in a short time, much of the corundum remains undissolved. It was
realized that with enhancement of dissolution temperature in the
same time period, the intensities of corundum, spinel, and dia-
oyudaoite crystalline phases existed in the residues experienced a
decreasing trend. At 85
C, with increasing time up to 120 min,
almost the entire corundum phase has been dissolved in acid,
which is very desirable for recovery of alumina. In contrast, with
increasing temperature, graphite and quartz remain as dominant
crystalline phases.
To quantify the qualitative XRD data for the purpose of better
comparison, the Rietveld fitting analysis was employed. Fig. 23 il-
lustrates the Rietveld fits and corresponding difference patterns.
The Rietveld fitting analysis was performed using crystallographic
information files (CIFs) of corundum, quartz, diaoyudaoite,
graphite, and spinel. Any unanalyzed pattern will appear as a re-
sidual or difference pattern. A difference pattern closer to a flat
pattern shows a good fitness. The instrumental and modelled
Rietveld data show relatively good agreement, observed in the
difference patterns and relatively low fitting parameters of
weighted profile R-factor (Rwp) and good of fitness (GOF) obtained
for all residue samples. Table 4 presents the summary of quanti-
tative phase analysis results for the XRD patterns obtained by
Rietveld refinement method.
According to data shown in Table 4, the residue 1 consists of
Fig. 18. Lorentzian profile for crystal size estimation.
predominantly corundum (46.1%) which has not been dissolved in
5 mol/l HCl during 15 min at ambient temperature. The corundum,
3.7.4. Microstructural study diaoyudaoite, and spinel phases were successfully dissolved in HCl
Fig. 20 depicts the FESEM micrograph of the as-produced nano with enhancement of dissolution time and temperature. In the case
alumina. It can be observed that the material has a rounded-corner of diaoyudaoite, its weight percentage was eventually reduced
shape, consisting of dense agglomerations of nano-crystallites with from 11.4% to 1.9% with increasing temperature and time. Such an
rough surface. A lot of tiny grains have been attached on large ones overall trend exists for spinel, as its weight percentage declined
and they are floccule in shape and non-uniformly distributed. from 12.7% to 1.6%. Since corundum, spinel, and diaoyudaoite
Elemental analysis by EDAX technique revealed a major chemistry contain aluminum in their chemical compositions, such an
of 52.1 wt% of Al and 45.5 wt% of O confirming the presence of improved dissolution behavior is desirable for the synthesis of
aluminum oxide. Also, the presence of Fe shows a little bit of im- alumina. The other two phases, namely graphite and quartz remain
purity. The values of s (0.9 wt% for both Al and O, and 0.7 wt% for undissolved and become predominant phases with over dissolution
Fe) show the errors in the weight fractions corroborating excellent time and temperature.
elemental analyses. The scanning electron microscopy (SEM) was applied to inves-
Fig. 21 displays the TEM image of the as-produced nano alumina tigate the change of morphology of the SAD before and after acid
at a magnification of 13 kX. It is clear that the as-prepared alumina dissolution process at various reaction times. Fig. 24 shows the SEM
comprises of a large quantity of relatively regular shaped particles images of the SAD before and after dissolution times of 15, 60, and
appeared as a lumpy structure. Although the details of the shape 120 min at temperature of 85
C.
are not obvious in this image. It can be seen that the raw SAD exhibits a relatively compact
structure comprised of strongly clumped particles (Fig. 24a), while
residues present a loose structure with flake-like particles (Fig. 24c
3.8. Characterization of dissolution residues and d). From SEM micrographs, superficial changes of SAD particles
are clear after being dissolved in HCl at temperature of 85
C at
Mineralogical analyses of the SAD dissolution residues at different times. Another obvious fact deduced from SEM micro-
graphs is that more destruction of morphology of the SAD particles
has occurred over dissolution time.

3.9. Comparison with alternatives

Alumina is commonly recovered from industrial solid wastes

based on pyro- and hydro-metallurgical processes. The pyro-
metallurgical processes are energy-intensive and need reductants.
The hydro-metallurgical extraction processes require a lower en-
ergy consumption and in this respect, they have an advantage over
pyrometallurgical-based processes. But among the hydrometallur-
gical processes, those are interesting that use less hazardous
chemicals and are closer to the zero waste concept. The proposed
recovery process in this study is a novel hydrometallurgical-based
Fig. 19. FTIR spectrum of the as-synthesized nano alumina from SAD. process which is performed at low temperature and atmospheric
288 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291

Fig. 22. XRD patterns of dissolution residues of SAD at various dissolution times and
temperatures: (1) 20
C, t ¼ 15 min (2) 55
C, t ¼ 15 min (3) 65
C, t ¼ 15 min (4) 75
C,
t ¼ 15 min (5) 85
C, t ¼ 15 min (6) 85
C, t ¼ 60 min (7) 85
C, t ¼ 120 min.

pressure. The processes reported to recover alumina from SAD

suffer from several problems, including the use of highly concen-
trated acid (Amer, 2002; Beaulieu et al., 2008), high energy con-
sumption (Sulaiman and Muslim, 2008) and toxic drainage (How
et al., 2017). The present work despite the kinetic study for the
first time and enriching existing knowledge, proposes an eco-
friendly recovery process, largely satisfying the zero-waste concept.

4. Conclusions and future perspective

The purpose of this study was to develop a green acid leaching-

based process for the production of nanostructured alumina pow-
der from hazardous secondary aluminum dross. To do this, the
Fig. 20. FESEM image of the as-produced nano alumina and respective elemental
dissolution kinetics of the dross in acid solution was firstly inves-
analysis. tigated and then, under optimal dissolution conditions, a process
for enhanced recovery of alumina in the form of a high purity
nanostructured powder was developed. Investigating the effect of
acid concentration, leaching temperature and time showed that the
dissolution efficiency initially increased with enhancement of acid
concentration followed by a reverse trend with further increase of
acid concentration. It was determined that despite the high disso-
lution temperature and time, there is still a few amounts of insol-
uble residual constituents. This makes the exigency to improve the
dissolution efficiency by changing other conditions such as particle
size. The dissolution process can be controlled by layer diffusion.
The activation energy was found to be 10.49 kJ/mol. The changes
occurred due to the dissolution of dross in acid were confirmed by
some complementary analyses including XRD, Rietveld fitting, and
scanning electron microscopy. These results are essential in reali-
zation of the dissolution process of secondary aluminum dross as a
potential raw material for recovery of alumina. In the second phase
of the work, based on the proposed process, alumina with a purity
of more than 98% was obtained which had a nano-crystalline
structure, consisting mainly of gamma-phase. Morphological
studies by FESEM and TEM revealed the dense agglomerations of
alumina particles. Because the overall recovery process increases
the reusability of the hazardous waste, produces a non-toxic
product (alumina), uses less hazardous reagents, and causes less
pollution release, it can be considered as an environmentally-
friendly process. Also, the residue at the end of the process can
be potentially applied as filler/aggregate in construction and
Fig. 21. TEM image of the as-produced nano alumina (magnification: 13kX). building materials. The developed process has economic justifica-
tion due to the use of inexpensive and accessible feedstock, low
energy consumption and simplicity. However, to prove this, a
M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291 289

Fig. 23. Rietveld plots and their corresponding difference patterns.

290 M. Mahinroosta, A. Allahverdi / Journal of Environmental Management 212 (2018) 278e291

Table 4
Summary of Rietveld analysis results for the seven residue samples.

Phase name Chemical formula Weight percent of crystalline phase

Residue 1 Residue 2 Residue 3 Residue 4 Residue 5 Residue 6 Residue 7

Corundum a-Al2O3 46.1% 15.4% 13.8% 9.9% 5.0% 4.5% 3.4%

Diaoyudaoite NaAl11O17 11.4% 17.2% 16.5% 10.3% 12.3% 2.9% 1.9%
Graphite C 13.9% 20.9% 24.5% 30.8% 28.1 29.8% 30.2%
Spinel MgAl2O4 12.7% 14.5% 10.6% 8.3% 4.7% 2.6% 1.6%
Quartz SiO2 15.9% 32.0% 34.6% 40.7% 49.9% 60.2% 62.9%
Rwp (%) e 6.53 9.64 9.83 5.46 5.37 4.87 8.93
GOF e 4.98 5.18 5.37 4.51 3.47 2.24 4.93

Fig. 24. SEM images of the SAD before (a) and after dissolution in HCl at 85
C for 15 (b), 60 (c), and 120 (d) min.

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