Received: 16 July 2020 Revised: 22 January 2021 Accepted: 24 January 2021

DOI: 10.1002/apj.2623

RESEARCH ARTICLE

Aluminum–iron separation in high-acid leaching solution

and high-purity alumina preparation

Hairong Shen | Likun Gao | Fangtong Ma | Bing Rao | Peng Jiang |

Guangyan Gao | Kebo Peng

Faculty of Land Resource Engineering,

Kunming University of Science and
Technology, Kunming, China
Correspondence
Likun Gao, Faculty of Land Resource
Engineering, Kunming University of
Science and Technology, 68 Wenchang,
Road, 121 Str., Kunming, Yunnan 650093,
China.
Email: 20030032@kust.edu.cn
Abstract
The demand for bauxite has increased sharply due to the fast development of
alumina industry, so new technology must be developed to take full advantage
of nontraditional bauxite resources to realize a continuous supply of bauxite.
In this experiment, anatase sulfuric acid leaching liquor is taken as the
research object to conduct aluminum–iron separation and high-purity alumina
preparation. The leaching solution contains 34.20 g/L of Al2O3, 25.30 g/L of
TFe, 7.96 g/L of TiO2, 12.74 mg/L of Sc2O3, and 288.72 g/L of H2SO4. When

Funding information
National Natural Science Foundation of
China, Grant/Award Numbers: No.
51764023 and No. 51464030, 51464030,
51764023
the temperature is low, aluminum and iron condensation, which are not con-
ducive to the separation and recovery of various elements, may occur easily. In
this study, the ammonium aluminum sulfate crystallization–recrystallization
and ion exchange–calcination method is adopted to effectively separate alumi-
num and iron in a strong acid solution comprising high concentrations of alu-
minum and iron without consuming high residual acid in the leaching liquor.
Consequently, successful production of high-added-value product 4N (99.99%)
level γ-Al2O3 with ammonium aluminum sulfate is obtained through separa-
tion as the raw material. The product has a specific surface area of 7.845 m2/g
with a nearly spherical shape and being evenly distributed. Therefore, it real-
izes high-value aluminum utilization from nontraditional bauxite.

KEYWORDS
aluminum–iron separation, ammonium aluminum sulfate, high-purity alumina, purify

1 | INTRODUCTION industry to produce alumina from high-quality bauxite;

Alumina is a significant metal oxide and is widely applied
in electrolytic aluminum, ceramics, medicine, electronics,
mechanics, and other sectors.1,2 With the rapid develop-
ment of the alumina industry, China's bauxite resources
face a severe supply situation.3 Therefore, it is of great
significance to explore and study some nontraditional
bauxite resources. The methods to extract alumina from
bauxite or other alumina ores comprise the alkaline and
acid processes. Currently, the alkaline process is used in
this method uses sodium hydroxide or sodium carbonate
to treat the aluminum ore, thus converting the alumina
in the ore to sodium aluminate solution, while iron, tita-
nium, and other impurities, as well as the majority of the
silicon content, are converted to insoluble compounds in
the dissolution process.4 However, for low-grade bauxite,
silicon enters into solution in the dissolution process
because of the reaction of alkali with silica. Therefore,
alkaline process is not applicable for the simultaneous
extraction and separation of aluminum and silicon.5

Asia-Pac J Chem Eng. 2021;e2623. wileyonlinelibrary.com/journal/apj © 2021 Curtin University and John Wiley & Sons, Ltd. 1 of 16
https://doi.org/10.1002/apj.2623
2 of 16
Compared to the alkaline process, the acid process pos-
sesses better thermodynamic driving force and able to
treat low-grade aluminum-containing minerals,6 owing
to its low energy consumption, few residues, extra-low
silicon content in the leaching liquor, and comprehensive
utilization of various valuable elements. Alumina is pro-
duced by the acid process using nitric acid, sulfuric acid,
hydrochloric acid, and other inorganic acids to treat
aluminum-bearing minerals to obtain an acidic aqueous
solution of the corresponding aluminum salt,7–10 and the
aluminum salt, hydrate crystal (through evaporation
crystallization), or alkali aluminum salt (hydrolyzation
crystallization) is then separated from the solution, or it
can undergo alkali neutralization to precipitate alumi-
num hydroxide. Finally, the aluminum hydroxide,
hydrates of various aluminum salts, or alkali aluminum
salt can be roasted to produce alumina products. The
study by Wang et al.11 from Beijing General Research
Institute of Mining and Metallurgy on the leaching test of
bauxite with a low alumina–silica ratio shows that when
the liquid/solid ratio is 3:1, the reaction time is 300 min
and sulfuric acid leaching is adopted; the leaching rates
of alumina and iron reach 93% and 88.94%, respectively.
Wu et al.9 adopted 50% sulfuric acid to lixiviate coal fly
ash, and the leaching rate of alumina reached up to
82.4% under pressure conditions at a temperature of
180
C for 4 h. Zhao et al.12 conducted some research for
the acid leaching of low-grade gibbsite. Their results
showed that the aluminum and iron leaching rates were
over 95% and the filter residue was mainly silica. Das
et al.13 reported alumina recovery from waste aluminum
dross by the method of H2SO4 leaching. However, the
main barrier for acid leaching is complicated acid recov-
ery and the difficulty in removing iron from aluminum
salt solution.14,15 Some countries that lack bauxite
resources have been researching methods to treat non-
bauxite raw materials to produce alumina with the acid
process, so some progress has been made in the study of
alumina production with the acid process in recent years.
Titanium minerals are widely distributed in the litho-
sphere and mainly include ilmenite, rutile, anatase,
perovskite, and sphene. Among them, as a Ti-bearing
independent mineral with industrial value, anatase has
high titanium dioxide content (95 wt% TiO2) with triva-
lent aluminum and iron as common impurity elements
with up to 0.55 wt% Al2O3 and 1.6 wt% Fe2O3 reported.16
The sulfuric acid leaching process is the most effective
way to treat low-grade titanium resources.17–19 Al, Fe, K,
Ca, Mg, and other elements dissolve out together with Ti
in the leaching process, so alumina and various elements
can be separated and extracted in the follow-up purifica-
tion process of the leaching solution. The study by
Agatzini-Leonardou et al. on the leaching test of anatase
SHEN ET AL.
with dilute sulfuric acid shows that the dissolution of tita-
nium is significantly affected by temperature and acid
normality, and the recovery efficiency of titanium is low
under the diluted sulfuric acid condition.20 To improve
the reactivity of the ore and the extraction efficiency of
aluminum, the leaching rate of aluminum by direct acid
leaching can be boosted by improving the reaction tem-
perature.21 Recently, our research group invented a new
way to extract alumina from the anatase of Qinglong,
Guizhou, where the raw ore contents are 5.3% TiO2,
84.7 g/t Sc2O3, 22.18% Al2O3, 16.85% TFe, and 35.75%
SiO2, which adopted the atmospheric leaching process of
sulfuric acid to raise the leaching temperature by virtue
of the high boiling point of sulfuric acid and realized the
high-efficiency leaching of anatase with the appropriate
two-stage countercurrent leaching process. The leaching
conditions for stage one are an ore-grinding fineness of
−0.074 mm, content of 82.6%, initial sulfuric acid concen-
tration of 5.5 mol/L, leaching liquid/solid ratio of 3 ml/g,
stirring speed of 400 r/min, leaching temperature of
100
C, and leaching time of 90 min. The leaching condi-
tions for stage two are an initial sulfuric acid concentra-
tion of 11.0 mol/L, leaching liquid/solid ratio of 4 ml/g,
stirring speed of 400 r/min, leaching temperature of
150
C, and leaching time of 60 min. Then, a leaching
solution containing 34.20 g/L Al2O3, 25.30 g/L TFe,
7.96 g/L TiO2, 12.74 mg/L Sc2O3, and 288.72 g/L H2SO4 is
obtained, while the leaching efficiencies of aluminum,
iron, titanium, and scandium are 99.73%, 99.80%, 97.27%,
and 97.20%, respectively. However, the leaching liquor, a
strong acid solution, contains high concentrations of alu-
minum and iron, which are likely to cause the formation
of aggregates and agglomerations at low temperatures,
thus making the purification and enrichment of the
leaching liquor more difficult.
There are three main methods to separate aluminum
and iron in a leaching liquor: the extraction method, pre-
cipitation method (organic and inorganic), and crystalli-
zation method. In the extraction method, an appropriate
extractant is used to selectively extract iron from the
leaching liquor and transfer it to the organic phase, and
then back extraction and a series of processes are adopted
to obtain a ferrous substance, thus realizing the prelimi-
nary separation of aluminum and iron.22,23 In the inor-
ganic precipitation method,24 additives including MnO2,
KMnO4, K3[Fe (CN)6], or K4Fe(CN)63H2O can be added
to reach the ideal effect. In the organic complexation pre-
cipitation method, a selective reaction between the
organic reagent and iron is used to produce an insoluble
ferric ion complex precipitation, thus achieving the goal
of iron removal through filtration. In the crystallization
method, varying solubility of different materials in the
same solvent is used to reach the goal of purification. The
SHEN ET AL.
crystallization method can be classified into the alumi-
num chloride crystallization method, aluminum sulfate
crystallization method, and ammonium aluminum sul-
fate crystallization method. When the solution contains
large quantities of Na2SO4, K2SO4, and other materials
with low solubility, directly using the concentration crys-
tallization method can easily cause the aluminum sulfate
crystal to mingle with many impurities. Compared to alu-
minum sulfate and other sulfates, ammonium aluminum
sulfate has lower solubility, so it can be used to separate
and extract aluminum with the ammonium aluminum
sulfate crystallization method. Zhao et al.25 adopted the
ammonium aluminum sulfate crystallization method to
separate and extract aluminum from the leaching solu-
tion of coal fly ash sulfuric acid. In this method, when
the ammonium–aluminum ratio is 1.0–1.5 and the crys-
tallization temperature is 15
C, the crystallization ratio of
aluminum can reach 74%, and the purity of NH4Al
(SO4)212H2O exceeds 90%.
Ammonium aluminum sulfate is the raw material for
preparing high-purity reactive alumina and is generally
synthesized through cooling crystallization.26 Nyvlt and
Hostomská27 produced ammonium aluminum sulfate
dodecahydrate crystal by utilizing crystallization com-
plexation through regulation of the percentage of Al3+
and NH4+ in sulfuric acid leaching liquor; Wan et al.28
realized the recovery and utilization of aluminum after
obtaining ammonium aluminum sulfate dodecahydrate
crystal by adding (NH4)2SO4 to the acidic waste liquor
containing Al3+. Currently, the main method to produce
high-purity alumina with ammonium aluminum sulfate
as the raw material both at home and abroad is the pyrol-
ysis method,29–32 which has the advantages of low raw
material cost and a reusable mother liquor. Park et al.
prepared high-purity ammonium aluminum sulfate
through the reaction of ammonium aluminum sulfate
derived from coal fly ash and fine α-Al2O3 with a particle
size of 0.1–0.5 μm obtained by calcining ammonium alu-
minum sulfate.33 Tanev et al.34 adopted different heating
methods to study the pyrolysis process of ammonium alu-
minum sulfate and thought that a lower calcination tem-
perature when the γ-Al2O3 phase had not yet totally
formed could increase the specific surface area of the
product.
Based on the above analysis, in this experiment, the
anatase sulfuric acid leaching solution is taken as the
research object, and the ammonium aluminum sulfate
crystallization method is adopted to separate and extract
aluminum from the leaching liquor without consuming
the high residual acid in the leaching liquor, and the
waste acid can be concentrated for cycle use. For the
ammonium aluminum sulfate obtained after iron and
aluminum separation, the combined process of
3 of 16
recrystallization (preliminary purification) and ion
exchange (in-depth purification) is adopted to remove the
iron in the ammonium aluminum sulfate, thus obtaining
high-purity ammonium aluminum sulfate products.
Finally, the obtained high-purity ammonium aluminum
sulfate was calcined using the pyrolysis method to pro-
duce alumina. The acquired alumina products were then
characterized by thermogravimetric analysis and differ-
ential scanning calorimetry (TGA-DSC), X-ray diffraction
(XRD), scanning electron microscopy (SEM), and
Brunauer–Emmett–Teller (BET) analysis to investigate
the effects of calcination temperature on the phase, mor-
phology, and specific surface area of alumina. The sepa-
ration of aluminum and iron in the sulfuric acid leaching
solution of anatase and the process flow of a high-purity
alumina preparation is shown in Figure 1.
2 | MATERIALS AND METHODS
2.1 | Materials
The main anatase ore components and contents are 5.3%
TiO2, 84.7 g/t Sc2O3, 22.18% Al2O3, 16.85% TFe, and
35.75% SiO2, and the main mineral composition in the
raw ore includes kaolinite, sericite, quartz, anatase, and
limonite, which account for approximately 95.60% of the
total ore. These minerals are difficult to treat because
they are weathered and altered minerals with fine crystal
sizes, mostly less than 10 μm, making monomer dissocia-
tion difficult to achieve. The results of the chemical mul-
tielement analysis of anatase are shown in Table 1.
The anatase leaching test research shows that the
two-stage countercurrent leaching process can obtain a
leaching solution containing 34.20 g/L Al2O3, 25.30 g/L
TFe, 7.96 g/L TiO2, 12.74 mg/L Sc2O3, and 288.72 g/L
H2SO4, where the leaching rates of scandium, titanium,
iron, and aluminum reached 97.20%, 97.27%, 99.80%, and
99.73%, respectively. The main components of anatase
sulfuric acid leaching solution are shown in Table 2.
2.2 | Methods
2.2.1 | Separation experiment of iron
and aluminum in anatase acid leaching
solution
The iron and aluminum separation test in the anatase
sulfuric acid leaching solution was carried out in a
cooling crystallizer. An appropriate amount of acid
leaching solution was placed in a reaction vessel and
heated to a suitable temperature, and then ammonium
4 of 16
sulfate was added to the acid leaching solution to provide
the required NH4+ for the ammonium aluminum reac-
tion, heated for a period of time to dissolve the ammo-
nium sulfate and fully react with the acid leaching
solution, and placed in the cooling crystallizer. The tem-
perature, chemical reaction time, stirring speed, and
other conditions were controlled. After the crystallization
process was completed, the ammonium aluminum sul-
fate crystal and the crystallization tail liquid are sepa-
rated, the volume of the crystallization tail liquid was
measured by measuring cylinder, the content of iron and
aluminum in the crystalline tail liquid were determined
by inductively coupled plasma spectrometer (ICPS-
1000II, Shimadu, Japan), and the purity of alumina was
SHEN ET AL.
F I G U R E 1 The separation of
aluminum and iron in the sulfuric acid
leaching solution of anatase and the process
flow of high-purity alumina preparation
measured using ICP (shimadzu ICPE-8100). All of the
chemical reagents used in this study were of analytical
grade. The calculation formula of iron inclusion rate is as
follows:
α = ð1 −v2 a2 =v1 a1 Þ × 100%: ð1Þ
The formula for calculating the crystallization rate of
aluminum is as follows:
β = ð1 −v2 b2 =v1 b1 Þ × 100%: ð2Þ
In the above formula, α represents the inclusion ratio
of iron, β represents the crystallization ratio of
SHEN ET AL. 5 of 16

TABLE 1 Chemical analysis of anatase crystallizer, and the temperature, chemical reaction time,
stirring speed, and other conditions were controlled.
Element Content(%)
−6
After the crystallization process was completed, solid–
Sc (10 ) 84.7
liquid separation was used to obtain the aluminum
TiO2 5.3 ammonium sulfate crystals and crystallization tail
Fe 16.85 liquid. The volume of the crystallization tail liquid was
Al2O3 22.18 measured, and the iron and aluminum contents in
SiO2 35.75 the crystalline tail liquid were tested to calculate the
iron-removal rate and aluminum crystallization rate. The
K 2O 1.04
iron-removal rate is calculated as
P 0.1
MgO 0.76
γ = ð1 −v4 a4 =v3 a3 Þ × 100%: ð3Þ
CaO 0.064
S 0.02
Na2O <0.1 The formula for calculating the crystallization rate of
As(10 ) −6
22.3 aluminum is
Total rare earth 0.04
δ = ðv4 b4 =v3 b3 Þ × 100%: ð4Þ

In the above formulas, γ represents the iron-

T A B L E 2 Chemical composition of anatase sulphuric acid
leachate (g/L)
Element Content
Al2O3 34.20
TFe 25.30
TiO2 7.96
Sc2O3 12.74
H2SO4 288.72
Note: The unit of Sc2O3 is mg/L.
aluminum, v1 represents the volume of the acid leaching
solution before crystallization, v2 represents the volume
of the crystallization tail solution, a1 represents the iron
concentration in the acid leaching solution before crystal-
lization (calculated as TFe), a2 represents the concentra-
tion of iron in the crystallization tail (calculated as TFe),
b1 represents the concentration of aluminum in the acid
leaching solution before crystallization (calculated as
Al2O3), and b2 represents the concentration of aluminum
in the crystallization tail (calculated as Al2O3).
2.2.2 | Experiment on removing iron
from ammonium aluminum sulfate by
recrystallization
The crude aluminum ammonium sulfate product was
added to deionized water to dissolve with heating, and
the volume of the solution was measured. The aluminum
ammonium sulfate solution was placed in a cooling
removal rate, δ represents the crystallization rate of
aluminum, v3 represents the volume of the aluminum
ammonium sulfate solution before crystallization, v4
represents the volume of the crystallization tail liquid,
a3 represents the iron concentration in the aluminum
ammonium sulfate solution before crystallization (cal-
culated as TFe), a4 represents the concentration of iron
in the crystallization tail (calculated as TFe), b3 repre-
sents the concentration of aluminum in the aluminum
ammonium sulfate solution before crystallization (cal-
culated as Al2O3), and b4 represents the concentration
of aluminum in the crystallization tail (calculated as
Al2O3).
2.2.3 | Experiment of removing iron
from ammonium aluminum sulfate by ion
exchange method
Fill the ion exchange resin into the resin column and
pretreat it, and then the aluminum ammonium sulfate
obtained by the preliminary iron removal by the recrys-
tallization method is added to deionized water and
heated to dissolve. Measure the volume of the resulting
solution, and add it to the resin column to remove iron
by ion exchange adsorption. Control the concentration,
flow rate, temperature, and other conditions of alumi-
num ammonium sulfate solution, measure the volume
and iron and aluminum ions concentration of the solu-
tion after the resin adsorption iron, and calculate the
iron-removal rate and aluminum loss rate. The formula
for calculating the iron-removal rate is
6 of 16
ε = ð1 −v6 a6 =v5 a5 Þ × 100%: ð5Þ
The formula for calculating the loss rate of aluminum
is
ζ = ð1 − v6 b6 =v5 b5 Þ × 100%: ð6Þ
In the above formulas, ε represents the iron-removal
rate, ζ represents the loss rate of aluminum, v5 represents
the volume of ammonium aluminum sulfate solution
before iron removal by resin adsorption, v6 represents the
volume of ammonium aluminum sulfate solution after
iron removal by resin adsorption, a5 represents the iron
concentration in ammonium aluminum sulfate solution
before iron adsorption by resin (calculated as TFe), a6
represents the iron concentration in ammonium alumi-
num sulfate solution after iron adsorption by resin (calcu-
lated as TFe), b5 represents the aluminum concentration
in ammonium aluminum sulfate solution before iron
adsorption by resin (calculated as Al2O3), and b6 repre-
sents the aluminum concentration in ammonium alumi-
num sulfate solution after iron adsorption by resin
(calculated as Al2O3).
2.2.4 | Preparation of high-purity
alumina by pyrolysis of aluminum
ammonium sulfate
The thermal decomposition process of ammonium alu-
minum sulfate was analyzed by the MELER/1600H
synchronous thermal analyzer of METTLER TOLEDO,
Switzerland. The protective gas was nitrogen, the
heating rate was 10 K/min, the heating range was
25–1,100
C, and the sample volume was 18.91 mg. A
TGA-DSC curve was drawn of the aluminum ammo-
nium sulfate, and the entire thermal decomposition
process of aluminum ammonium sulfate was analyzed
thoroughly.
The YFX5/16Q-YC resistance furnace of Shanghai
Yifeng Electric Furnace Co., Ltd. was used to conduct
roasting tests on aluminum ammonium sulfate at differ-
ent temperatures to observe the appearance of the
roasted product. The conversion of the crystalline form of
the calcined product was analyzed by the D/MAX-2200
X-ray diffractometer of Rigaku Corporation, and the
Uadrasorb-evo automatic specific surface and pore size
distribution analyzer of the US Kangta Company was
used to measure and analyze the specific surface area of
the calcined product and detect the purity of the alumina
obtained by pyrolysis of aluminum ammonium sulfate
and other related parameters.
SHEN ET AL.
3 | RESULTS A ND DISCUSSION
3.1 | Separation of iron and aluminum
in acid leaching solution by ammonium
aluminum sulfate crystallization
3.1.1 | Effect of Al3+ initial
concentration on separation of iron and
aluminum
The initial concentration of acid leaching solution Al3+ is
an important factor affecting the separation of iron and
aluminum. The higher the initial concentration of Al3+,
the easier it is for aluminum ammonium sulfate to reach
supersaturation in solution. Supersaturation promotes
the nucleation and crystallization rates of crystals, but
the increase in growth rate under high supersaturation
promotes impurity incorporation, either at defects or
within liquid inclusions.35 Under the conditions of a
NH4+/Al3+ molar ratio of 1.2, temperature of 25
C,
chemical reaction time of 30 min, and stirring speed of
300 r/min, the effect of initial Al3+ concentration on the
separation efficiency of iron and aluminum is shown in
Figure 2. The inclusion rate of iron in aluminum ammo-
nium sulfate increases with the initial concentration of
Al3+. When the initial concentration of Al3+ increases
from 0.48 to 0.68 mol/L, the iron inclusion rate increases
from 6.36% to 13.79%. When the initial concentration of
Al3+ was increased to 0.88 mol/L, the iron inclusion rate
increased rapidly to 24.45%. The crystallization rate of
aluminum gradually increases with the increase in the
initial concentration of Al3+. When the initial concentra-
tion of Al3+ increases from 0.48 to 0.68 mol/L, the crystal-
lization rate of aluminum increases sharply from 60.70%
to 82.77%. If the initial concentration of Al3+ continues to
F I G U R E 2 Effect of Al3+ initial concentration on iron
inclusion rate and aluminum crystallization rate
SHEN ET AL.
increase, the crystallization rate of aluminum increases
slowly. Considering the inclusion rate of iron in alumi-
num ammonium sulfate and the crystallization rate of
aluminum, the initial concentration of Al3+ was deter-
mined to be 0.68 mol/L.
3.1.2 | Effect of NH4+/Al3+ molar ratio
on separation of iron and aluminum
The crystallization principle of ammonium aluminum
sulfate is
Al2 ðSO4 Þ3 + ðNH4 Þ2 SO4 + 24H2 O
! 2NH4 AlðSO4 Þ2  12H2 O:
The above equation shows that the NH4+/Al3+ molar
ratio is an important factor affecting the crystallization
rate of aluminum. Under the conditions of an initial Al3+
concentration of 0.68 mol/L, temperature of 25
C,
chemical reaction time of 30 min, and stirring speed of
300 r/min, the effect of NH4+/Al3+ molar ratio on the
separation efficiency of iron and aluminum is shown in
Figure 3. When the NH4+/Al3+ molar ratio is increased
from 1.0 to 1.2, the iron inclusion rate in aluminum
ammonium sulfate increases from 7.25% to 13.79%. As
the NH4+/Al3+ molar ratio continues to increase, the iron
inclusion rate does not change much but tends to
increase first and then decrease. When the NH4+/Al3+
molar ratio increases from 1.0 to 1.2, the crystallization
rate of aluminum increases rapidly from 71.16% to
82.77%. As the NH4+/Al3+ molar ratio continues to
increase, the crystallization rate of aluminum grows very
slowly, and the excessive molar ratio of NH4+/Al3+ leads
to an increase in the amount of ammonium sulfate. The
F I G U R E 3 Effect of NH4+/Al3+ molar ratio on iron inclusion
rate and aluminum crystallization rate
7 of 16
remaining NH4+ in the solution reacts with other ions
(Fe3+, Fe2+, Ca2+, Mg2+, and Na+) to form the
corresponding double salt and is incorporated into the
aluminum ammonium sulfate crystals, resulting in a
decrease in the purity of the aluminum ammonium sul-
fate crystals. By comprehensively considering the iron
inclusion rate in ammonium aluminum sulfate, the crys-
tallization rate of aluminum and the remaining amount
of ammonium sulfate, the NH4+/Al3+ molar ratio of 1.2
was determined.
3.1.3 | Effect of temperature on the
separation of iron and aluminum
ð7Þ
The solubility of ammonium aluminum sulfate in water
is closely related to the temperature.36 It can be seen from
Figure 4 that as the temperature decreases, the solubility
of aluminum ammonium sulfate gradually decreases,
and the lower the temperature, the higher the crystallin-
ity of aluminum ammonium sulfate. Under the condi-
tions of an initial Al3+ concentration of 0.68 mol/L,
NH4+/Al3+ molar ratio of 1.2, chemical reaction time of
30 min, and stirring speed of 300 r/min, the effect of tem-
perature on the separation efficiency of iron and alumi-
num is shown in Figure 5, and the temperature has a
strong influence on the purity of aluminum ammonium
sulfate crystals. The iron inclusion rate in ammonium
aluminum sulfate increases with decreasing temperature.
When the temperature decreases from 25
C to 15
C, the
iron inclusion rate increases rapidly from 13.79% to
22.71%. The crystallization rate of aluminum also
increases with the decrease in temperature. When the
temperature drops from 35
C to 15
C, the crystallization
rate of aluminum increases rapidly from 60% to 91.86%.
FIGURE 4 Solubility curve of aluminum ammonium sulfate in
water
8 of 16 SHEN ET AL.

3.1.5 | Effect of stirring speed on the

separation of iron and aluminum

Due to the many conflicting factors affecting crystalliza-

F I G U R E 5 Effect of temperature on the iron inclusion rate
and aluminum crystallization rate
By comprehensively considering the iron inclusion rate
in aluminum ammonium sulfate, the crystallization rate
of aluminum and the cooling cost, the crystallization
temperature was determined to be 25
C.
tion, the effect of stirring speed on crystallization is quite
complex.37 The stirring process makes the concentration
and temperature of the entire solution system more bal-
anced, so the particle size and quality of the aluminum
ammonium sulfate crystals obtained are also more uni-
form and stable. Under the conditions of an initial Al3+
concentration of 0.68 mol/L, NH4+/Al3+ molar ratio of 1.2,
temperature of 25
C, and chemical reaction time of
30 min, the effect of stirring speed on the separation effi-
ciency of iron and aluminum is shown in Figure 7. The
iron inclusion rate decreases with the increase in the stir-
ring speed, and the downward trend is slowed down.
When the stirring speed is 300 r/min, the iron inclusion
rate is 13.79%. This is because when the stirring speed is
fast, the diffusion process has greater control of the crystal

3.1.4 | Effect of chemical reaction time

on the separation of iron and aluminum

The chemical reaction time has a certain effect on the

properties of the aluminum ammonium sulfate crystals
and the crystallization rate of other components in the
solution. If the reaction time is too short, the crystals in
the solution are not yet stable and the particle size is small,
which easily leads to a low crystallization rate; an appro-
priate extension of time can promote more complete crys-
tallization. Under the conditions of an initial Al3+
concentration of 0.68 mol/L, NH4+/Al3+ molar ratio of 1.2, F I G U R E 6 Effect of time on iron inclusion rate and aluminum
temperature of 25
C, and stirring speed of 300 r/min, the crystallization rate
effect of chemical reaction time on the separation effi-
ciency of iron and aluminum is shown in Figure 6. It can
be seen from the figure that the crystallization of alumi-
num ammonium sulfate is rapid; when the temperature
reaches 25
C, the crystallization process of aluminum has
been basically completed, and as the reaction time con-
tinues to be extended, the crystallization rate of aluminum
remains basically unchanged and is maintained at approx-
imately 83.00%. The chemical reaction time ranged from
0 to 40 min, and the iron inclusion rate in the solution
increased first and then decreased with the extension of
the reaction time. When the reaction time was 30 min, the
iron inclusion rate was 13.79%. By comprehensively con-
sidering the iron inclusion rate in ammonium sulfate, the
crystallization rate of aluminum, and the stability of alu-
minum ammonium sulfate crystals, the chemical reaction F I G U R E 7 Effect of stirring speed on iron inclusion rate and
time was determined to be 30 min. aluminum crystallization rate
SHEN ET AL.
growth rate. Because the concentration of impure iron in
the solution is significantly lower than that of aluminum,
the diffusion stimulus is weaker, making it difficult for
iron to be incorporated into the crystal.38 The crystalliza-
tion rate of aluminum increases first and then decreases
with the increase in the stirring speed. When the stirring
speed is 300 r/min, the crystallization rate reaches the
maximum value of 82.77%. This is because a stirring speed
that is too high causes the generation of a certain amount
of crystal debris, the dissolution of which results in a slight
decrease in the aluminum crystallization ratio. By compre-
hensively considering the iron inclusion rate and alumi-
num crystallization rate in ammonium aluminum sulfate,
the stirring speed is determined to be 300 r/min.
The above experimental research shows that under the
conditions of initial Al3+ concentration of 0.68 mol/L,
NH4+/Al3+ molar ratio of 1.2, temperature of 25
C,
chemical reaction time of 30 min, and stirring speed of
300 r/min, the content of iron in the crystallization
tail liquid (calculated as TFe) is 29.57 g/L, the aluminum
content (calculated as Al2O3) is 7.90 g/L, in the
resulting crude ammonium aluminum sulfate product
(water-containing), the iron content (calculated as TFe)
is 1.323%, and the aluminum content (calculated as Al2O3)
is 10.80%.
3.2 | Experimental study on the deep
iron removal of ammonium aluminum
sulfate
There are various methods for removing iron from
ammonium aluminum sulfate, such as the potassium
permanganate method, organic complexation method,
and extraction method, but these processes all require
the addition of other substances to the ammonium alumi-
num sulfate solution, which can easily introduce other
impurity ions. Both the recrystallization method and the
ion exchange method effectively avoid the contamination
of impurity ions. According to the characteristics of the
two processes, it is proposed to use a combination of
recrystallization preliminary purification and ion
exchange deep purification to remove iron from ammo-
nium aluminum sulfate.
3.2.1 | Recrystallization method to
remove iron from ammonium aluminum
sulfate
Effect of liquid/solid ratio on iron-removal rate and
aluminum crystallization rate
The liquid/solid ratio is the ratio of the volume of pure
water required to dissolve ammonium aluminum sulfate
9 of 16
and the mass of ammonium aluminum sulfate. The effect
of the liquid/solid ratio on the purification effect of
ammonium aluminum sulfate under the conditions of a
temperature of 25
C, chemical reaction time of 30 min,
and stirring speed of 400 r/min is shown in Figure 8. The
iron-removal rate gradually increases with the increase in
the liquid/solid ratio. When the liquid/solid ratio
increases from 1.0 to 1.4 ml/g, the iron-removal rate
increases rapidly from 90.76% to 94.97%, continue to
increase the liquid/solid ratio and the iron-removal rate
did not change much. The crystallization rate of alumi-
num continuously decreases with the increase in the liq-
uid/solid ratio. When the liquid/solid ratio is 1.0 ml/g,
the crystallization rate of aluminum is as high as 87.77%;
at this time, the high content of ammonium aluminum
sulfate crystals increases the solution viscosity and the
fluidity decreases; when the liquid/solid ratio is increased
to 1.4 ml/g, the crystallization rate of aluminum is
83.28%, and when the liquid/solid ratio is further
increased to 1.8 ml/g, the crystallization rate of alumi-
num is reduced to 72.45%. By comprehensively consider-
ing the iron-removal rate, the aluminum crystallization
rate and the fluidity of the solution, the liquid/solid ratio
is determined to be 1.4 ml/g.
Effect of stirring speed on iron-removal rate and
aluminum crystallization rate
During the recrystallization process, proper stirring speed
can increase the migration rate of ions in the solution
and form a relatively uniform stagnation layer on the
crystal surface, thereby promoting the adsorption of ions
on the crystal surface and promoting the growth of the
crystal.39 Under the conditions of a liquid/solid ratio of
1.4 ml/g, a temperature of 25
C, and a chemical reaction
time of 30 min, the effect of the stirring speed on the
F I G U R E 8 Effect of liquid/solid ratio on iron-removal rate and
aluminum crystallization rate
10 of 16
purification effect of ammonium aluminum sulfate is
shown in Figure 9. The stirring speed has a greater influ-
ence on the iron-removal rate. With the increase in the
stirring speed, the iron-removal rate shows an upward
trend. When the stirring speed is increased from 100 to
300 r/min, the iron-removal rate increases slowly; when
the stirring speed is increased to at 400 r/min, the iron-
removal rate increases rapidly to 94.97%; continue to
increase the stirring speed, the iron-removal rate
increases slowly, and a certain amount of crystal debris is
generated due to the excessive speed. The dissolution of
this debris causes the aluminum crystallization rate to
decrease slightly. The effect of stirring speed on the
crystallization rate of aluminum is not obvious. With
the increase in stirring speed, the crystallization rate
of aluminum fluctuates slightly. By comprehensively
considering the iron-removal rate and the crystallization
rate of aluminum, the stirring speed is determined to be
400 r/min.
According to the above experimental research, under
the conditions of a liquid/solid ratio of 1.4 ml/g, a tem-
perature of 25
C, a chemical reaction time of 30 min, and
a stirring speed of 400 r/min, the iron-removal rate
reached 94.97%, and the crystallization rate of aluminum
was 83.28%. The aluminum content (calculated as Al2O3)
in the crystallization tail liquid is 13.00 g/L, and the iron
content (calculated as TFe) is 9.10 g/L; the recrystalliza-
tion method has a significant effect on the removal of
iron in ammonium aluminum sulfate. After the iron is
removed from the crude ammonium aluminum sulfate
product by primary recrystallization, the aluminum con-
tent (calculated as Al2O3) in ammonium aluminum sul-
fate (water-containing) is 11.80%, and the iron content
(calculated as TFe) is 0.0856%.
F I G U R E 9 Effect of stirring speed on iron-removal rate and
aluminum crystallization rate
SHEN ET AL.
Experimental study on iron removal by second
recrystallization
Under the conditions of liquid/solid ratio of 1.4 ml/g,
temperature of 25
C, chemical reaction time of 30 min,
stirring speed of 400 r/min, conduct second recrystalliza-
tion purification on the ammonium aluminum sulfate
obtained by the first recrystallization purification, and
the iron-removal rate of second recrystallization is
93.47%, and the crystallization rate of aluminum is
84.74%. Through twice recrystallization, the iron-removal
rate is as high as 99.68%. The aluminum content (calcu-
lated as Al2O3) in the ammonium aluminum sulfate
(water-containing) is 11.90%, and the iron content (calcu-
lated as TFe) is 0.006653%.
3.2.2 | Removal of iron from ammonium
aluminum sulfate by ion exchange
From the above research results, it can be seen that the
recrystallization method has a high iron-removal rate,
but the recrystallization process of multiple times leads to
a complicated purification process of ammonium alumi-
num sulfate. The ion exchange method has the advantage
of high iron-removal rate, it is planned to use ion
exchange method to replace the third recrystallization,
the HYC-100 resin is selected to achieve the deep
removal of iron in ammonium aluminum sulfate, and it
is an aminocarboxylic acid chelating resin, which has a
good removal effect on metal ions and has a good regen-
eration ability.
Effect of flow speed on iron-removal rate
The flow speed has certain effects on the mass transfer
rate of ions penetrating the liquid film on the resin outer
layer as well as the ion exchange reaction rate.40 When
the flow speed is too high, the contact time between the
solution and the resin is too short, the exchange capacity
is small, and the resin utilization rate is low. Reducing
the flow speed can aid in the complete exchange of ions,
but too low of a flow speed reduces the mass transfer rate
of the liquid film, which may occasionally cause the mal-
distribution of water flow in the cross section of the resin
layer. Under the condition that the concentration of
ammonium aluminum sulfate solution is 0.65 mol/L and
the temperature is 65
C, the effect of flow speed on the
iron-removal rate is shown in Figure 10. The iron-
removal rate continues to decrease as the flow speed
increases. When the flow speed is increased from 1 to
13 ml/min, the iron-removal rate slowly decreases from
98.99% to 98.53%; this indicates that change in a low flow
speed has little effect on the iron removal ratio. When
the flow speed is increased from 13 to 17 ml/min, the
SHEN ET AL.
FIGURE 10 Effect of flow speed on iron-removal rate
iron-removal rate drops sharply to 97.56%. Considering
the iron-removal rate and iron removal efficiency, the
flow speed is determined to be 13 ml/min.
Effect of temperature on iron-removal rate
Temperature is an important factor affecting the iron
removal effect of ion exchange resins. If the temperature
is too high, the adsorption capacity of the resin will be
reduced, and even the adsorption capacity of the resin
will be permanently damaged; if the temperature is too
low, crystals of ammonium aluminum sulfate are easily
generated in the solution and block the resin column.
Under the condition that the concentration of ammo-
nium aluminum sulfate solution is 0.65 mol/L and the
flow speed is 13 ml/min, the effect of temperature on the
iron-removal rate is shown in Figure 11. The iron-
removal rate shows a downward trend with the increase
in temperature. When the temperature is increased from
55
C to 65
C, the iron-removal rate decreased slowly
from 98.79% to 98.53%; when the temperature continued
to increase to 70
C, the iron-removal rate dropped
sharply to 97.24%; When the temperature is below 65
C,
traces of ammonium aluminum sulfate crystals will
appear in the solution, which may cause clogging of the
resin column. By comprehensively considering the iron-
removal rate and the crystallization of ammonium alumi-
num sulfate, the temperature is determined to be 65
C.
The above experimental research shows that under
the conditions of ammonium aluminum sulfate solution
concentration of 0.65 mol/L, flow speed of 13 ml/min,
and temperature of 65
C, the iron-removal rate is as high
as 98.53%. The concentration of the ammonium alumi-
num sulfate solution after removing iron from the resin
is 0.65 mol/L, and the iron content (calculated as TFe) is
20.128 μg/ml. The ammonium aluminum sulfate
11 of 16
FIGURE 11 Effect of temperature on iron-removal rate
solution, after removing iron from the resin, is cooled
and crystallized at 10
C to obtain ammonium aluminum
sulfate crystals. The aluminum content (calculated as
Al2O3) in the ammonium aluminum sulfate crystal
(water-containing) is 11.90%, and the iron content (calcu-
lated as TFe) is 0.0000165%. The indexes of the process
flow are presented in Table 3.
3.3 | Preparation of high-purity alumina
by pyrolysis of ammonium aluminum
sulfate
3.3.1 | Synchronous thermal analysis of
ammonium aluminum sulfate (TGA-DSC)
The TGA-DSC curve of ammonium aluminum sulfate is
shown in Figure 12. The thermal decomposition process
of ammonium aluminum sulfate can be divided into
three weightlessness stages; after three stages of weight-
lessness, the final remaining amount is 11.03%, which is
basically consistent with the theoretical content of
11.25% of Al2O3 in ammonium aluminum sulfate
dodecahydrate.
Stage I of weight loss: Removal of crystallization water.
The commencement temperature of the water loss stage
was 42
C, and the finishing temperature was 241
C. The
weight loss ratio was 47.08%, and approximately 12 mole-
cules of water of crystallization were removed. Three sig-
nificant water loss processes corresponding to the three
endothermic peaks that occurred at 98
C, 114
C, and
214
C were observed. When the temperature rose to
180
C, approximately 10 molecules of water of crystalli-
zation were removed, the weight loss ratio was 39.54%,
and the TGA-DSC curve was stabilized. Within the
12 of 16 SHEN ET AL.

TABLE 3 Aluminum–iron separation in anatase sulfuric acid leaching solution

Iron inclusion Crystallization

rate/iron removal rate of Ammonium
rate aluminum aluminum sulfate
Technological indexes Test conditions % % TFe (%) Al2O3 (%)
Separation of iron and 0.68 mol/L Al3+, NH4+/Al3+ 13.79 82.77 1.323 10.80
aluminum in acid molar ratio 1.2, temperature
leaching solution by of 25
C, chemical reaction
ammonium aluminum time of 30 min, and stirring
sulfate crystallization speed of 300 r/min
Recrystallization method to Liquid/solid ratio of 1.4 ml/g, 94.97 83.28 0.0856 11.80
remove iron from temperature of 25
C,
ammonium aluminum chemical reaction time of
sulfate 30 min, and stirring speed
of 400 r/min
Experimental study on iron Liquid/solid ratio of 1.4 ml/g, 93.47 84.74 0.006653 11.90
removal by second temperature of 25
C,
recrystallization chemical reaction time of
30 min, and stirring speed
400 r/min
Removal of iron from 0.65 mol/L ammonium 98.53 84.70 0.0000165 11.90
ammonium aluminum aluminum sulfate solution,
sulfate by ion exchange flow speed of 13 ml/min,
and temperature of 65
C

was 574
C, and the inflection temperature was 520
C.

The weight loss amounted to 15.74%, which was basically
consistent with the theoretical weight loss: 14.63%. The
DSC curve showed a distinct endothermic peak at 527
C,
indicating that this stage was an endothermic process.
The corresponding pyrolysis reaction equation is as
follows:

NH4 AlðSO4 Þ2 ! 0:5Al2 ðSO4 Þ3 + NH3 + 0:5SO3 + 0:5H2 O:

ð9Þ

Stage III of weight loss: Removal of SO3. The com-

FIGURE 12 TGA-DSC curves of ammonium aluminum mencement temperature was 574
C, the finishing tem-
sulfate perature was 901
C, and the inflection temperature was
782
C. The weight loss in this stage was 26.13%, which
temperature range of 180–241
C, the water-removal conformed to the theoretical weight loss of 26.50%. The
effect was very weak: Only approximately two molecules corresponding pyrolysis reaction equation is
of water of crystallization were removed. The pyrolysis
reaction equation at this stage is 5Al2 ðSO4 Þ3 ! 0:5Al2 O3 + 1:5SO3 : ð10Þ

NH4 AlðSO4 Þ2  12H2 O ! NH4 AlðSO4 Þ2 + 12H2 O:
Stage II of weight loss: Removal of (NH4)2SO4 from
NH4Al(SO4)2. An analysis of the TGA-DSC curve showed
that the commencement temperature of the weight loss
process in this stage was 241
C, the finishing temperature
ð8Þ As indicated by the DSC curve, the three weight loss
stages of ammonium aluminum sulfate dodecahydrate
are endothermic processes; when the temperature rises to
891
C, an exothermic peak appears on the DSC curve,
which may have been the result of changes in some of
the Al2O3 crystal forms.
SHEN ET AL.
3.3.2 | Effect of calcination temperature
on the crystal form of alumina
The roasting test was carried out on the ammonium alumi-
num sulfate after removing impurities, the roasting tem-
perature was controlled to 800
C, 900
C, 1000
C, 1100
C,
1200
C, 1300
C, and the roasting time was determined as
2 h. Observation of the appearance of the roasted products
at different temperatures revealed that when the roasting
temperature was increased from 800
C to 900
C, the vol-
ume of the roasted product increased significantly, and its
whiteness also increased significantly; when the calcina-
tion temperature was gradually increased from 900
C to
1300
C, the volume of the calcined product gradually
decreased. In particular, when the calcination tempera-
ture increases from 1100
C to 1200
C, the volume of the
calcined product decreases more obviously, and the white-
ness also gradually increases. The XRD pattern of the cal-
cined product of ammonium aluminum sulfate at
different temperatures is shown in Figure 13.
Figure 13 shows that when ammonium aluminum
sulfate was calcined at 800
C, the calcination product
exhibited a sharp diffraction peak, and ammonium alu-
minum sulfate was initially decomposed to Al2(SO4)3.
When the calcination temperature was 900
C, the calci-
nation product exhibited weaker and broader diffraction
peaks, and ammonium aluminum sulfate was completely
FIGURE 13 XRD diffraction patterns of calcination products at 800
C, 900
C, 1000
C, 1100
C, 1200
C, and 1300
C
13 of 16
decomposed into γ-Al2O3. At a calcination temperature of
1000
C, many hetero peaks were observed, indicating
poor crystallization of the product, which was a mix of γ
and δ phases at this point. At a calcination temperature
of 1100
C, fewer hetero peaks were observed on the XRD
spectrum, and the main diffraction peaks tended to be
sharp; further, part of γ-Al2O3 was converted into δ-Al2O3
at this point. At a calcination temperature of 1200
C,
multiple distinct sharp diffraction peaks occurred, indi-
cating that the large amount of transition-crystal δ-Al2O3
had transformed into the stable α-Al2O3. At a calcination
temperature of 1300
C, narrow and sharp diffraction
peaks were observed on the XRD spectrum; the alumina
at this point were all at the α-Al2O3 phase.
According to the above analysis, the pyrolysis
sequence of ammonium aluminum sulfate is NH4Al
(SO4)212H2O ! NH4Al(SO4)2 ! Al2(SO4)3 !
γ-Al2O3 ! δ-Al2O3 ! α-Al2O3.
3.3.3 | Effect of calcination temperature
on specific surface area of alumina
The effect of calcination temperature on the specific sur-
face area of alumina is shown in Figure 14; the specific
surface area of alumina constantly decreased with
increasing calcination temperature. When the calcination
14 of 16 SHEN ET AL.

3.3.4 | Characterization of product

alumina

Alumina prepared at a calcination temperature of 1300
C

was selected for content analysis and SEM characteriza-
tion. The results are as follows.

F I G U R E 1 4 Effect of calcination temperature on specific
surface area of alumina
Purity analysis
Table 4 shows that the Al2O3 content of the high-purity
alumina prepared using the aforementioned process is
>99.99%, which corresponds to 4N-grade high-purity alu-
mina. The main impurities in this high-purity alumina
are Fe2O3, SiO2, and Na2O. Therefore, to prepare higher
purity alumina (5N and above), it is necessary to focus on
removing the remaining sodium and silicon in the
ammonium aluminum sulfate.

SEM morphology characterization

Figure 15 shows that the alumina particles are spherical
TABLE 4 Detection indexes of alumina
and uniformly distributed.
Main impurity content (%)

Al2O3 content (%) Fe2O3 SiO2 Na2O

4 | CONCLUSIONS
>99.99 0.0017 0.0034 0.0032

1. The experimental research results of the separation of

2. The results of the purification test of ammonium alu-
FIGURE 15 SEM images of calcination products at 1300
C
temperature was increased from 900
C to 1100
C, the
specific surface area of alumina slowly decreased from
148.26 to 117.96 m2/g. When the calcination temperature
reaches 1100
C, continue to increase the calcination tem-
perature, the specific surface area of alumina drops
sharply. When the calcination temperature is 1300
C, the
specific surface area of alumina is only 7.845 m2/g.
aluminum and iron via the ammonium aluminum
sulfate crystallization method showed that under the
conditions of an initial Al3+ concentration of
0.68 mol/L, NH4+/Al3+ molar ratio of 1.2, temperature
of 25
C, chemical reaction time of 30 min, and stirring
speed of 300 r/min, the inclusion rate of iron in the
sulfuric acid leaching solution of titanium ore was
13.79%, and the crystallization rate of aluminum was
82.77%. The crude ammonium aluminum sulfate
product contained 10.80% aluminum (calculated as
Al2O3) and 1.323% iron (calculated as TFe). The
ammonium aluminum sulfate crystallization method
can effectively separate the iron and aluminum in the
anatase acid leaching solution.
minum sulfate show that preliminary removal of iron
from crude ammonium aluminum sulfate product
was achieved through recrystallization. Under the
conditions of a liquid/solid ratio of 1.4 ml/g, tempera-
ture of 25
C, chemical reaction time of 30 min, and
stirring speed of 400 r/min, the iron-removal rate
reached 94.97% and the crystallization rate of alumi-
num was 83.28%; through first recrystallization, the
iron content (calculated as TFe) in ammonium alumi-
num sulfate was reduced from 1.323% to 0.0856%;
conduct second recrystallization purification on the
ammonium aluminum sulfate obtained by the first
recrystallization purification, the process conditions of
SHEN ET AL.
the second recrystallization are the same as the first, the
iron-removal rate of the second recrystallization is
93.47%, the crystallization rate of aluminum is 84.74%,
and the iron content in the ammonium aluminum sul-
fate through second recrystallization (calculated as TFe)
was reduced from 0.0856% to 0.006653%; HYC-100 ion
chelating resin is used to deeply remove iron from
ammonium aluminum sulfate by ion exchange, under
the conditions of ammonium aluminum sulfate solution
concentration of 0.65 mol/L, flow speed of 13 ml/min,
and temperature of 65
C, the iron-removal rate is as
high as 98.53%, and there is basically no loss of
aluminum; after repeated purification, the iron content
(calculated as TFe) in aluminum ammonium sulfate is
0.0000165%.
3. The test results of pyrolysis of ammonium aluminum
sulfate to prepare high-purity alumina show that the
thermal decomposition of ammonium aluminum sul-
fate is completed in three steps. The first step is to
remove 12 molecules of water of crystallization to
obtain anhydrous ammonium aluminum sulfate, the
second step is to remove the ammonium and part of
the sulfur in anhydrous ammonium aluminum sulfate
to produce aluminum sulfate, and the third step is to
remove the remaining sulfur from aluminum sulfate
to produce the final product alumina. Aluminum
ammonium sulfate is basically completely pyrolyzed
at a temperature of 900
C; as the temperature con-
tinues to increase, the pyrolysis product is still alu-
mina, but its properties change dramatically. XRD
analysis and specific surface area test of alumina prod-
ucts at different calcination temperatures show that
with the increase in calcination temperature, the crys-
talline form of alumina is gradually transformed from
γ-Al2O3 to the most stable α-Al2O3; its specific surface
area also decreases from 148.26 to 7.845 m2/g.
4. The purity of alumina with a calcination temperature
of 1300
C was tested. The alumina content was
>99.99%, the phase was α-Al2O3, the specific surface
area was 7.845 m2/g, and the alumina particles were
spherical and uniformly distributed. The process of
ammonium aluminum sulfate crystallization–
recrystallization and ion exchange roasting not only
achieved the separation of iron and aluminum in a
strong acid solution but also successfully prepared
high value-added products using the separated ammo-
nium aluminum sulfate as the raw material—4N
(99.99%)-grade high-purity alumina.
A C K N O WL E D G E M E N T
The authors would like to acknowledge the National
Natural Science Foundation of China (No. 51764023 and
No. 51464030) for the financial support.
15 of 16
ORCID
Likun Gao https://orcid.org/0000-0001-7354-1148
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