G. ÇIL, K. YILDIZ: EVALUATION OF SECONDARY ALUMINIUM DROSS IN CALCIUM ALUMINATE CEMENT
541–546
EVALUATION OF SECONDARY ALUMINIUM DROSS IN
CALCIUM ALUMINATE CEMENT
OVREDNOTENJE SEKUNDARNE ALUMINIJEVE @LINDRE V
KALCIJEVEM ALUMINATNEM CEMENTU
Gökhan Çil
*
, Kenan Yildiz
Sakarya University, Metallurgy and Materials Engineering, Sakarya, Turkey
Prejem rokopisa – received: 2022-05-05; sprejem za objavo – accepted for publication: 2022-08-19
doi:10.17222/mit.2022.491
In this study, the evaluation of aluminium dross from secondary aluminium production in calcium aluminate cement was investi-
gated. Salt compounds were removed significantly from the secondary aluminium dross by washing. Mixtures of washed dross
and quicklime were prepared to obtain a cement additive by considering the standard cement with low alumina and they were
sintered at 1250 °C for 5 h. The phases of mayenite, monocalcium aluminate, grossite, gehlenite, larnite, periclase and spinel
were detected in the sintered samples using an X-ray diffraction analysis. Tests of the normal consistency, setting time and com-
pressive strength were carried out at replacement levels of (2.5, 5, 7.5, 10 and 12.5) w/% of the cement additive to determine the
physical properties of the cement paste/mortar. Increasing the level of the cement additive in the commercial calcium aluminate
cement (ISIDAC 40) accelerated the setting time of the mortar and decreased workability.
Keywords: secondary aluminium dross, recycling, calcium aluminate, cement
V raziskavi je opisano ovrednotenje aluminijeve `lindre nastale pri predelavi sekundarnega aluminija, ki je bila uporabljena kot
dodatek aluminatnemu cementu. Spojine soli v sekundarni aluminijevi `lindri so o~istili z izpiranjem z vodo. Pripravljeno
me{anico tako o~i{~ene `lindre in `ivega apna so `gali 5 ur pri 1250 °C ter jo uporabili kot dodatek k standardnemu cementu z
nizko vsebnostjo aluminija. Z rentgensko difrakcijsko analizo so ugotovili, da sintrana me{anica vsebuje majenit, mono kalcijev
aluminat, grosit, gelenit. larnit, periklaz in {pinel. Izvedli so teste konsistence, ~asa posedanja in tla~ne trdnosti pri (2,5, 5, 7,5,
10 in 12,5) w/% sintranega dodatka in dolo~ili fizikalne lastnosti me{anice cementna pasta/malta. Nara{~anje vsebnosti dodatka
komercialnemu Ca-Al cementu (ISIDAC 40) je pospe{ilo ~as posedanja malte in zmanj{alo njeno sposobnost za oblikovanje.
Klju~ne besede: sekundarna aluminijeva `lindra, recikliranje, kalcijev aluminat, cement
1 INTRODUCTION
Aluminium is widely used in various industries due
to its conductivity, light weight and strong corrosion re-
sistance. Nowadays, there are two different methods in
aluminium production: primary production using the raw
material (bauxite ore) and secondary production using
waste products.
1
Primary aluminium dross including aluminium prod-
ucts and scraps is re-melted in secondary aluminium pro-
duction. The molten aluminium in the furnace is covered
by a stream of molten salt, which absorbs the non-metal-
lic compounds in the raw material. The dark-coloured
top layer, called black dross, is removed by skimming
before the molten metal is absorbed. Secondary alu-
minium slag mainly contains compounds of Al, O, Na,
N, K, Mg, Si, Cl, F and small amounts of Ti, S, Mn, V
and Fe.
2,3
The recycling and disposal of dross, released
by the aluminium industry, is amongst the most chal-
lenging problems in the world. Dross is solid waste that
can cause serious environmental pollution and is hazard-
ous to public health. A large proportion of the released
dross is disposed to landfills, causing a loss of valuable
metals and polluting ground water. About 20 % of this
dross is black dross and the rest is white dross released
from primary aluminium production. About 95 % of this
waste is landfilled each year. It is declared that almost
five million tons of white and black dross are produced
worldwide per year. In addition, the reaction of alu-
minium dross with moisture or water vapour may pro-
duce dangerous flammable and poisonous gases such as
CH
4
,NH
3
,PH
3
,H
2,
H
2
S, etc. For these reasons, it is nec-
essary to create a recycling mechanism for the alu-
minium dross produced in these industries.
4–9
Secondary aluminium production requires a lower
energy consumption than primary aluminium production.
The energy requirement of secondary aluminium produc-
tion is only5%oftheenergy used for primary alumi-
nium production.
8,10
The recycling and reuse of industrial
waste and by-products are also very essential in cement
and concrete production. Traditional by-products such as
granulated blast furnace slag, fly ash or silica fume are
evaluated as cementing materials in the cement industry.
Besides, various wastes are generated in aluminium re-
fining facilities.
11
Pereira et al.
12
investigated the me-
chanical behaviour of Portland cement mortars contain-
ing salt slags produced from the aluminium scrap
re-melted in rotary furnaces. It was reported that the me-
Materiali in tehnologije / Materials and technology 56 (2022) 5, 541–546 541
UDK 666.948 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 56(5)541(2022)
*Corresponding author's e-mail:
gkncil@gmail.com (Gökhan Çil)

chanical properties of concrete are suitable when up to
10 w/% of cement is replaced by salt slag as compared
with the control concrete. In addition, Yoshimura et al.
13
used aluminium dross as the raw material to replace cal-
cined alumina. Moreover, Ewais et al.
14
studied the use
of aluminium sludge and aluminium dross in the produc-
tion of calcium aluminate cement.
Calcium aluminate cements (CACs) are named dif-
ferently depending on their alumina (Al
2
O
3
) content and
chemical composition. Typical compositions of calcium
aluminate cement are summarized in Table 1.
15
The use
of cement containing 40 % of alumina is higher than the
use of cement with a high alumina content; it is preferred
for specific characteristics such as abrasion resistance or
refractoriness. The main clinker phases of calcium
aluminate cement (CAC) are CA (monocalcium alumi-
nate: CaAl
2
O
4
), C
12
A
7
(mayenite: Ca
11
Al
17
O
33
) and CA
2
(grossite: CaAl
4
O
7
). Calcium aluminate cement with
37–54 % of Al
2
O
3
contains a substantial amount of C
2
AS
(gehlenite: Ca
2
Al
2
SiO
7
), which is not hydrated. The
mayenite phase (C
12
A
7
) reacts quickly with water and
plays a significant role in the hydration mechanism. The
reaction of the grossite phase (CA
2
) with water is quite
slow at ambient temperature. It can be accelerated by in-
creasing the temperature.
16,17
Calcium aluminate cement (CAC) is the preferred
product in various industries due to its superior proper-
ties such as fire resistance, abrasion resistance, scour re-
sistance and acid resistance.
18
Also, it allows concrete
applications in cold weather, being able to gain durabil-
ity even at temperatures below 0 °C. In recent years,
CAC has been widely used with high-priced agents as re-
pair materials.
19
The main purposes of this work are to investigate and
evaluate secondary aluminium dross as an additive mate-
rial in commercial calcium aluminate cement and to con-
tribute to the recycling of these wastes in the cement in-
dustry.
2 EXPERIMENTAL PART
2.1 Materials and method
Secondary aluminium dross used in this study was
evaluated as a source of Al
2
O
3
. It was supplied from
Sahinler Metal Co., Turkey. Calcium oxide (quicklime)
was used to increase the CaO content of the dross. Cal-
cium oxide was supplied from Nuh Construction Prod-
ucts Co., Turkey. The dross was ground for 30 min at
1300 min
–1
using a Mertest LB200 ring mill. After grind-
ing, the particle size of aluminium dross was measured
with a Malvern-Mastersizer 2000 and it was ground to a
size below 100 μm. A chemical analysis was carried out
using a Rigaku D/MAX/2200/PC X-ray fluorescence
(XRF) spectrometer. The quicklime used in this study
contained 99 % CaO and 1 % MgO. The elemental com-
position of secondary aluminium dross obtained with the
XRF analysis is given in Table 2. The elemental analysis
and XRD indicate that unwashed dross contains mainly
Al
2
O
3
(37.47 %) and salts like NaCl and KCl.
Table 2: XRF elemental analysis of secondary aluminium dross
Elemental composition
Amounts
(w/%)
Al
(Al2O3)
19.98
(37.47)
Na 15.88
K 3.77
Cl 22.57
Ca 1.41
Fe 1.94
Mg 1.72
Si 0.41
S 0.22
Others
(Ti, Cr, Mn, Cu, Zn, Ba)
4.97
O balance
Table 3: Chemical composition of ISIDAC 40
Chemical composition Amounts (w/%)
SiO2
3.60
Al2
O
3
39.80
Fe2
O
3
17.05
CaO 36.20
MgO 0.65
SO3
0.04
Loss on ignition 0.30
(Na2O+K
2O) 0.16
Cl 0.0090
S 0.01
The sintered samples consisting of washed alumi-
nium dross and calcium oxide, recognised as the cement
additive, were ground for 20 min at 600 min
–1
using a
planetary mono mill. In this process, 40 tungsten carbide
(WC) balls with a diameter of 10 mm were used in a
250 mL WC bowl and the ball-to-sample weight ratio
G. ÇIL, K. YILDIZ: EVALUATION OF SECONDARY ALUMINIUM DROSS IN CALCIUM ALUMINATE CEMENT
542 Materiali in tehnologije / Materials and technology 56 (2022) 5, 541–546
Table 1: Typical compositions of calcium aluminate cement (w/%)
15
Type of cement Al
2
O
3 CaO
Fe2O3 +
FeO
FeO SiO
2
TiO
2 MgO
K2O+
Na
2O
SO
3
40%Al
2
O
3
40–45 42–48 < 10 < 5 5–8 ~ 2 < 1.5 < 0.4 < 0.2
50%Al 2
O
3
49–55 34–39 < 3.5 < 1.5 4–6 ~ 2 ~ 1 < 0.4 < 0.3
50%Al 2O3 (low Fe) 50–55 36–38 < 2 < 1 4–6 ~ 2 ~ 1 < 0.4 < 0.3
70%Al 2O3 69–72 27–29 < 0.3 < 0.2 < 0.8 < 0.1 < 0.3 < 0.5 < 0.3
80%Al 2
O
3
79–82 17–20 < 0.25 < 0.2 < 0.4 < 0.1 < 0.3 < 0.7 < 0.2

was chosen to be 20. The grinding process was dry. The
commercial calcium aluminate cement (ISIDAC 40) pro-
duced by Çimsa Cement Co. (Turkey) in accordance
with the EN 14647 standard
20
was used as the cement
material. The chemical composition of ISIDAC 40 is
given in Table 3.
2.2 Sample preparation
In order to carry out the experiments, cement mix-
tures were prepared by adding the cement additive to the
commercial calcium aluminate cement (ISIDAC 40) with
different proportions. The details of the mixture propor-
tions are illustrated in Table 4. Silica-based CEN stan-
dard sand with a maximum grain diameter of 2 mm pre-
pared in accordance with the EN 196-1
21
standard was
used as the aggregate in order to obtain mortar mixtures.
It was supplied from Limak Co. (Turkey).
Table 4: Mixture proportions (w/%)
Mix code 123456
ISIDAC 40 100 97.5 95 92.5 90 88.5
Cement Additive – 2.5 5 7.5 10 12.5
The setting time experiments with the prepared ce-
ment paste mixtures were carried out using a Toni Tech-
nic automatic setting time tester at an ambient tempera-
ture of (20 ± 2) °C and 50–60 % relative humidity
according to the requirements of the EN 196-3
22
stan-
dard. Water was added to 500-g cement samples taken
from each cement mixture to get enough workability and
then the setting time tests were carried out.
Compressive strengths were measured with prismatic
moulds with dimensions of (40 × 40 × 160) mm. Mortar
preparation was conducted according to the EN 14647
and EN 196-1 standards. The specimens of mortar were
prepared by mixing 1350 g of CEN standard sand (sil-
ica-rich) with 500 g of cement (mixing 1–6) and 200 mL
of water. For all the mixtures, the water-to-cement ratio
(w/c) was kept constant at 0.4. These measurements
were carried out after curing periods of6hand24hus -
ing the Toni Technic testing machine. All the specimens
were kept in the curing chamber with a temperature of
(20 ± 1) °C and a minimum relative humidity of 90 %.
All the specimens were demoulded after 6 h and the
specimens to be tested after 6 h were tested immediately
after demoulding. The specimens to be tested after 24 h
were stored in the curing chamber after demoulding.
3 RESULTS AND DISCUSSION
In the studies on aluminium dross, it was found that a
high content of aluminium oxide was present in the dross
and that the main phases were aluminium metal, Fe
2
O
3
,
SiO
2
,N a
2
O, AlN, MgO while the dross also contained
small amounts of Ti, S, Mn, V and Fe compounds. In ad-
dition, it was reported that salts such as NaCl or KCl and
small amounts of the chloride, nitride and fluoride phases
with different compositions were encountered.
23–25
Alu-
minium dross was subjected to water washing for 30 min
and 60 min to remove the high chlorine content. Results
of the XRF elemental analysis of secondary aluminium
dross after water washing are given in Table 5.I tw a s
observed that the amount of chlorine in the compound
was removed by increasing the washing time. After
washing the aluminium dross for 60 min, the alumina
content of the dross increased from 37.74 % to 68.03 %
and the chlorine content of the dross decreased from
22.57 % to 0.033 %.
Table 5: XRF elemental analysis of the washed secondary aluminium
dross (w/%)
Chemical
composition
Washing
for 30 min
Washing
for 60 min
Al
(Al2
O
3
)
30.61
(57.82)
36.02
(68.03)
Na 6.60 0.07
K 1.66 0.71
Cl 9.60 0.033
Ca 2.50 3.84
Fe 1.85 2.11
Mg 2.34 2.89
Si 0.56 0.756
Ti 0.665 1.51
S––
O balance blance
The amount of calcium oxide in the washed alu-
minium dross is not high enough to form calcium
aluminate clinker phases of the cement additive. CaO
was added to 60 min-washed aluminium dross with a
CaO/dross ratio of 3/5 and mixed in for 10 min. The pur-
pose of using this ratio was to obtain composition values
close to EN 14647. The composition of the cement addi-
tive and EN 14647 limits are given in Table 6.
Table 6: Chemical composition of cement additive and EN 14647 lim-
its (w/%)
Chemical composition Amounts EN 14647 limits
SiO2
1.01 –
Al2O3 42.51 35-58
Fe2
O
3
1.89 –
CaO 40.48 –
MgO 3.37 –
TiO2 1.57 –
Na2
O+K
2
O 0.4 max. 0.40
SO3
– max. 0.50
S – max. 0.10
CI 0.020 max. 0.10
In some studies on commercial low-alumina cements,
it was reported that cement clinker phases consisted of
the CA, CA
2
,C
2
AS, C
2
S, C
12
A
7
phases.
26–30
According to
the XRD analysis of the produced cement additive shown
in Figure 1, the sample sintered at 1250 °C for5hwas
G. ÇIL, K. YILDIZ: EVALUATION OF SECONDARY ALUMINIUM DROSS IN CALCIUM ALUMINATE CEMENT
Materiali in tehnologije / Materials and technology 56 (2022) 5, 541–546 543

composed of the Ca
12
Al
14
O
33
(mayenite-C
12
A
7
), CaAl
4
O
7
(grossite-CA
2
), CaAl
2
O
4
(monocalcium aluminate-CA),
Ca
2
SiO
4
(larnite-C
2
S) and Ca
2
Al(AlSiO
7
) (gehle-
nite-C
2
AS) phases. Along with these phases, there were
small quantities of MgAl
2
O
4
(spinel-MA) and MgO
(periclase) due to the high Mg content in the dross.
D10, D50 and D90 sizes corresponding to the particle
sizes at the 10 %, 50 % and 90 % points on the cumula-
tive distribution for the cement additive were found to be
2.05 μm, 14.38 μm and 39.52 μm, respectively. It was re-
alized that the particle size was suitable for the prepara-
tion of the cement mixture. The results of the particle
size analysis are supported by the SEM image of the ce-
ment additive, given in Figure 2. It is proposed to use
the cement additive in various percentages of cement.
Figure 3 presents the normal consistency obtained for
various percentages of the cement additive. It was ob-
served that the workability decreased and the water re-
quirement increased depending on the increase in the ce-
ment additive proportion in the paste. While the water
requirement was 26 % for the commercial cement, it was
35.3 % for the commercial cement with 12.5 % amount
of the cement additive. The percentage of the water to be
added to the mix was greater for larger amounts of the
cement additive.
The setting times of the cement pastes at different re-
placement levels are shown in Figure 4. The increasing
cement additive content accelerates the hardening. Ac-
cording to the EN 14647 standard, the initial setting time
should not be less than 90 min. It is seen from the results
obtained for all the mixtures that the setting times are
within the standard requirements.
According to the EN 14647 standard, the compres-
sive strength of calcium aluminate cement, tested in ac-
cordance with the EN 196-1 standard, should not be less
than 18 MPa after 6 h and 40 MPa after 24 h. For our
study, the compressive strength at different replacement
levels is shown in Figure 5. It was found that the in-
creasing amount of the cement additive in the mixture
adversely affected the mechanical properties. In the ce-
ment mixtures prepared with 0–12.5 w/% cement addi-
tives, the compressive strength of the concrete decreased
by 65.2 % for the specimens kept for 6 h and by 58.9 %
G. ÇIL, K. YILDIZ: EVALUATION OF SECONDARY ALUMINIUM DROSS IN CALCIUM ALUMINATE CEMENT
544 Materiali in tehnologije / Materials and technology 56 (2022) 5, 541–546
Figure 3: Variation in the normal consistency with the replacement of
cement by the cement additive
Figure 1: XRD analysis of the cement additive sintered at 1250 °C for
5h
Figure 4: Relationship between the setting time and cement additive
content Figure 2: SEM image of the cement additive

for the specimens kept for 24 h. The 7.5 w/% replace-
ment of the commercial cement with the cement additive
is selected as the optimum cement mix since it meets the
requirements of the international standard.
Arimanwa et al.
31
investigated the effect of alu-
minium waste, as a supplementary cementitious material,
on concrete properties. They found that the addition of
aluminium dross decreased both the initial and final set-
ting times of the cement. They also found that work-
ability was decreased due to the water absorbed by alu-
minium dross from the mix. Nduka et al.
32
investigated
the influence of aluminium dross on the mechanical and
durability properties of sandcrete blocks. The water ab-
sorption was found to be increased with the increased re-
placement percentage of dross. Ozerkan et al.
33
found
that the setting time was decreased up to the 15 % re-
placement of cementitious material.
Aluminium dross was suggested to be used in the
production of eco-concrete in the study by Javali et al.
34
They produced several mixtures of Portland cement, alu-
minium dross, sand and granular iron slag. For alu-
minium dross, different replacement levels were consid-
ered: (5, 10, 15 and 20) w/%; the optimal level was
determined to be 5 w/%. In another study by Trinet,
35
an
increase in the amount of aluminium dross mixed into
Portland cement caused a decrease in the compressive
strength. These results were verified in studies by Reddy
and Neeraja and Ozerkan et al.
5 CONCLUSIONS
It is possible to use secondary aluminium dross as the
material added to cement with low alumina after washing
and sintering it with quicklime at optimum conditions.
The use of a high volume of the cement additive pre-
pared from aluminium dross is not appropriate because
of its high water-absorption capacity.
An increase in the cement additive content causes a
decrease in both the initial and final setting times of the
cement. This may be due to a higher surface area of the
cement additive. The shortening of these times reduces
the workability of the mortar and therefore the addition
of the cement additive should be limited. The compres-
sive strengths decline with the increasing cement addi-
tive proportion in the cement mortar. Replacements of
the commercial cement by the cement additive of up to
7.5 w/% provide for the compressive strengths of the
concrete determined by the international standard re-
quirements.
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