environments

Article
Recycling of Cement Kiln Dust as a Raw Material
for Cement
Minhye Seo, Soo-Young Lee, Chul Lee and Sung-Su Cho *
Plant Engineering Center, Institute for Advanced Engineering, Yongin 17180, Korea; minhye_s@iae.re.kr (M.S.);
sylee@iae.re.kr (S.-Y.L.); chullee0711@naver.com (C.L.)
* Correspondence: sungsu@iae.re.kr; Tel.: +82-31-330-7688




Received: 24 September 2019; Accepted: 16 October 2019; Published: 17 October 2019


Abstract: Cement kiln dust (CKD) is a major by-product of cement manufacturing and has the
potential to be recycled as a raw material if the high concentrations of chlorine and potassium are
removed. This study tested four leaching solutions (distilled water and three organic acids) and
determined the optimum reaction conditions. At a liquid/solid (L/S ratio) of 10, the removal efficiency
of formic, citric, and oxalic acid was higher than that of distilled water, but at L/S 20, distilled water
also achieved a high removal efficiency of Cl (≥90%) and K (≥70%). In addition, to minimize the
discharge of wastewater after leaching, the efficiency of ion-exchange resins for the recovery of
leaching solution was tested. When the cation- and anion-exchange resins were arranged together,
more than 95% of both Cl and K contained in the leaching solution could be removed. Leaching
solution without Cl and K was found to have a high leaching efficiency even after being recycled
three times, resulting in a significant reduction in wastewater emissions.

Keywords: cement dust kiln; recycling; leaching of Cl; K; leaching solution; ion exchange process

1. Introduction
Cement kiln dust (CKD) is a by-product of the cement manufacturing process and has traditionally
been considered as an industrial waste product. Global cement production capacity in 2017 was
~4.99 billion tons per year [1,2], while the CKD production rate ranged from 54 to 200 kg per ton
of produced cement clinker [3]. CKD is composed of fine, powdery solids and highly alkaline
particulate material, and is similar in appearance to Portland cement. Its size distribution and chemical
composition depends on production factors such as raw material, processing method, fuel, kiln type,
cement type, and dust collection method (e.g., cyclones, bag filters, or electrostatic precipitators). Finer
particles tend to exhibit a higher sulfate and alkali content. In general, CKD has a lower CaO and
SiO2 content than typical Portland cement (Table 1). Compared with cement, CKD is characterized by
higher alkalis (especially potassium), and chloride. The high alkali content precludes the recycling of
CKD into kilns, as this would exceed the maximum allowable value [4].
The increasing use of alternative fuels has driven a rise in chlorine input into kiln processes,
increasing the importance of chlorine bypass systems in order to avoid operational problems. In
particular, using waste fuel can increase the toxic metal content of the subsequent CKD [5]. A high
chlorine content in CKD can lead to various problems in its reuse. In general, the maximum chloride
content of cement is 0.10%, while the chloride contained in CKD may contain 0.35–15.4 wt%, depending
on its raw materials [6]. Chlorine is highly corrosive, and high levels of it in cement can encourage
steel corrosion. Several studies have reported that CKD can effectively improve soil strength and can
be used as an alternative to lime for soil stabilization [6,7]. Its alkaline properties and good absorption
capacity stabilize waste (instead of cement or lime) by reducing the moisture content and increasing the
bearing capacity [8]. In addition to this, it has also been injected into an asphalt concrete mixture and

Environments 2019, 6, 113; doi:10.3390/environments6100113 www.mdpi.com/journal/environments

Environments 2019, 6, 113 2 of 7

used as a mineral filler. However, CKD still contains corrosive substances such as chlorine, requiring a
suitable technology to render them harmless.
Some cement plants simply send CKD to landfills, but the increasing annual stockpile of CKD
and the high cost of its disposal requires an innovative solution that will allow CKD to be used in
construction. Lanzerstorfer [9] reported that chloride concentration from cement kiln bypass dust
(CKBD) depends on the particle size and can be removed by air classification. However, air classification
is only a pretreatment and has the disadvantage of simultaneously requiring a leaching process. Thus,
this study tested methods for the removal of chlorine and potassium ions from CKD in order to allow
its reuse as a cement raw material, and evaluated the removal efficiency of various leaching conditions
and the feasibility of recovering the leaching solutions through an ion-exchange system.

Table 1. Typical chemical composition of Portland cement and cement kiln dust (CKD).

Content CaO SiO2 K2 O Al2 O3 Cl− Ref.

64 22 0.3 5 <0.1 [6]
Portland cement (%) 63 20 - 5 - [10]
62 21 0.5 4 - [11]
38–50 11–16 3–13 3–6 0–5 [12]
CKD (%)
60.56 6.1 2.56 1.37 2.75 [13]

2. Materials and Methods

The CKD used in this study was obtained from Sampyo Cement, South Korea; it consisted mainly
of CaO with significant amounts of chloride, potassium, and sulfate anions (Table 2). The Cl and K ions
were leached using four agents: distilled water (DW) and the organic acids citric acid (99.5%, Daejung),
oxalic acid (99.5%, Junsei), and formic acid (85%, Daejung). The reaction times (1–30 min) of each
200 mL distilled water (DW) and 0.5 M organic-acid leaching solution were compared. The leaching
test of CKD was performed by changing the ratio of liquid and solid to 10 and 20. The CKD had a
low specific gravity and had limitations in mixing and reacting in a liquid phase, making it difficult
to further lower the L/S ratio. The removal efficiency of Cl− or K+ ions can be estimated using the
following Equation (1):

Leached Cl− (or K− )conc. in CKD (g)

Removal Efficiency (%) = × 100 (1)
Cl− (or K− )conc. in CKD (g)

The Cl and K ions leached from the CKD were configured in order to recycle the leaching solution
through the ion-exchange reaction (Figure 1). An ion-exchange resin was used in conjunction with an
ion-exchange resin (SAR20MBOH, Samyang Co., Ltd.) and cation-exchange resin (SCR-BH, Samyang
Co., Ltd.), respectively. Then, the CKD (L/S: 20) was added to the deionized leaching solution through
the ion-exchange resin, thereby removing Cl and K ions from the CKD.
The leaching and removal efficiency of the Cl and K ions from the CKD was evaluated using
X-ray fluorescence (XRF-1800, Shimadzu) after pelletizing with B2 O3 . The ion content in the leaching
solution was then measured by an ion chromatograph (DX-500, Dionex). Scanning electron microscopy
(MIRA3, Tescan) and energy dispersive spectroscopy (Bruker, XFlash 6130) were used to analyze the
morphology and impurities of the ion-exchange resins surface.
Environments 2019, 6, 113 3 of 7
Environments 2019, 6, x FOR PEER REVIEW 3 of 7

Flow diagram
Figure 1. Flow diagram for
for the
the leaching
leaching and
and ion-exchange
ion-exchange process of cement kiln dust.

Table 2. Properties of CKD powder from SAMPYO cement in South Korea.

Table 2. Properties of CKD powder from SAMPYO cement in South Korea.
Element CKD (wt%)
Element CKD (wt%)
Cl 39.10
Cl K 17.85
39.10
Ca 18.38
K Si 17.85
12.62
S 3.51
Ca Al 18.38
2.95
Fe 2.76
Si LoI * 12.62
2.83
* Loss on Ignition (105 ◦
S 3.51 C).

3. Results and Discussion Al 2.95

The removal efficiencies of FeCl and K were ~87% and 2.76~80%, under 0.5M formic acid. The removal
efficiencies were highest for formic acid, followed by oxalic acid, citric acid, and DW; the reaction time
LoI* 2.83
varied little between the solutions (Figure 2). As shown in Figure 2, the leaching reaction occurred
quickly and it can be seen that the leaching * Lossrate
on Ignition
was not(105 °C). any longer even though the reaction
increased
time increased. Suzuki et al. [14] reported that the salt produced, indicated by K2 O, could be recovered
3.
byResults
more thanand53% Discussion
by applying NaCl solution. In this study, however, potassium was able to remove
moreThethanremoval
80% in efficiencies
5 min. Similar results
of Cl and Khave
werebeen
~87%found in other
and ~80%, studies
under 0.5M onformic
organicacid.
acidThe
leaching
removalfor
the purpose of waste recycling [15,16]. Musariri et al. [15] reported that citric acid
efficiencies were highest for formic acid, followed by oxalic acid, citric acid, and DW; the reaction and malic acid both
produced
time varieda leaching rate of about
little between 70% within
the solutions 10 min
(Figure 2).inAs
a cobalt
shown leaching experiment.
in Figure In this study,
2, the leaching the
reaction
leaching
occurred rate did
quickly
Environments not
and
2019, 6, xincrease
it can
FOR besignificantly
PEER seen that theover
REVIEW time. rate was not increased any longer even4 ofthough
leaching 7

the reaction time increased. Suzuki et al. [14] reported that the salt produced, indicated by K2O, could
be recovered by more than 53% by applying NaCl solution. In this study, however, potassium was
able to remove more than 80% in 5 min. Similar results have been found in other studies on organic
acid leaching for the purpose of waste recycling [15,16]. Musariri et al. [15] reported that citric acid
and malic acid both produced a leaching rate of about 70% within 10 min in a cobalt leaching
experiment. In this study, the leaching rate did not increase significantly over time.

Figure 2. Ion
Figure removal
2. Ion removalefficiency
efficiencyofofCKD
CKD as
as aa function
function ofofthe
theleaching
leaching solution;
solution; (a) chloride
(a) chloride and (b)
and (b)
potassium. Reaction
potassium. conditions:
Reaction conditions:L/SL/S(Liquid
(Liquid solid ratio)==10,
solid ratio) °C.◦ C.
10,2525 1 atm.
1 atm.

To optimize the safety of CKD recycling, it is important to use solvents that are easy to handle
and with minimal environmental concerns. Of the leaching solutions used in this study, DW is the
easiest to handle, so its ion removal efficiency was further evaluated by reducing the CKD injection
amount to 5 wt% (Figure 3). The removal efficiencies of Cl and K were ~90% and ~83%, respectively,
for 1 min of extraction and were similar for up to 5 min of extraction, after which the remaining Ca
Environments 2019, 6, 113 4 of 7
Figure 2. Ion removal efficiency of CKD as a function of the leaching solution; (a) chloride and (b)
potassium. Reaction conditions: L/S (Liquid solid ratio) = 10, 25 °C. 1 atm.
To optimize the safety of CKD recycling, it is important to use solvents that are easy to handle and
with To optimize
minimal the safety ofconcerns.
environmental CKD recycling, it is important
Of the leaching to use
solutions usedsolvents that are
in this study, DWeasy to handle
is the easiest
and with minimal environmental concerns. Of the leaching solutions used in
to handle, so its ion removal efficiency was further evaluated by reducing the CKD injection amount this study, DW is the
to
5easiest to handle,
wt% (Figure so its
3). The ion removal
removal efficiency
efficiencies of Cl was
and further evaluated
K were ~90% by reducing
and ~83%, the CKD
respectively, for injection
1 min of
amount to and
extraction 5 wt% (Figure
were 3). for
similar Theupremoval
to 5 min efficiencies of Clafter
of extraction, and which
K werethe ~90% and ~83%,
remaining Ca respectively,
content was
for 1 min of extraction and were similar for up to 5 min of extraction, after which
analyzed. The leaching rate increased to 85% for up to 5 min, but Ca began to dissolve in the leaching the remaining Ca
content was
solution analyzed.
at longer Thetimes.
reaction leaching
Thisrate increased
clearly indicatesto that
85%the
forextraction
up to 5 min, but Ca
reaction timebegan
is antoimportant
dissolve
in the leaching solution at longer reaction times. This clearly indicates that the
parameter, with an optimal value of ≤5 min in a fixed-bed column. Golpayegani et al. [17] also reported extraction reaction
timethe
that is an important
chloride parameter,leaching
or potassium with an time
optimalwasvalue of ≤5 minparameter
an important in a fixed-bed
in ancolumn. Golpayegani
experimental model
et al. [17] also
considering reported
stirring rate,that the chlorideand
concentration, or potassium
temperature. leaching time was an important parameter in
an experimental model considering stirring rate, concentration, and temperature.

Figure 3. Ion removal efficiency of CKD with distilled water (DW) as a function of the reaction time;
Figure 3. Ion removal efficiency of CKD with distilled water (DW) as a function of the reaction time;
(a) removal of Cl, K, and concentration of Ca, (b) concentration of Cl and K including leached solution.
(a) removal of Cl, K, and concentration of Ca, (b) concentration of Cl and K including leached solution.
Reaction conditions: L/S = 20, 25 ◦ C. 1 atm.
Reaction conditions: L/S = 20, 25 °C. 1 atm.

The ion-exchange capacity was higher at lower flow rates; at 20, 40, and 80 mL/min, the removal
The ion-exchange capacity was higher at lower flow rates; at 20, 40, and 80 mL/min, the removal
rate of Cl ions was ≥99%, 97%, and 70%, and that of K ions was ≥99%, 97%, and 80%, respectively
rate of Cl ions was ≥99%, 97%, and 70%, and that of K ions was ≥99%, 97%, and 80%, respectively
(Figure 4). Liu et al. [18] reported an 80% removal efficiency using the anion-exchange method for
(Figure 4). Liu et al. [18] reported an 80% removal efficiency using the anion-exchange method for
the removal of chlorine ions from zinc-production wastewater, meeting the legal requirements for
the removal of chlorine ions from zinc-production wastewater, meeting the legal requirements for
wastewater recycling. Methods for Cl ion removal include chemical precipitation, flocculation, solvent
wastewater recycling. Methods for Cl ion removal include chemical precipitation, flocculation,
extraction, membrane separation, and ion exchange. The latter has many advantages, including high
solvent extraction, membrane separation, and ion exchange. The latter has many advantages,
reaction time, simplicity, and low construction/operation cost [18]. In this study, the Cl and K eluted
including high reaction time, simplicity, and low construction/operation cost [18]. In this study, the
from CKD was removed easily and effectively via ion-exchange resin, and the optimal operation speed
Cl and K eluted from CKD was removed easily and effectively via ion-exchange resin, and the
with a fixed-bed column was 40 ml/min. The potential treatment capacity was 267 g-K/L-resin and
255 g-Cl/L-resin, respectively.
 Environments 2019, 6, x FOR PEER REVIEW 5 of 7

Environments 2019, 6, 113 5 of 7

optimal operation speed with a fixed-bed column was 40 ml/min. The potential treatment capacity
was 267 g-K/L-resin and 255 g-Cl/L-resin, respectively.

Environments 2019, 6, x FOR PEER REVIEW 5 of 7

optimal operation speed with a fixed-bed column was 40 ml/min. The potential treatment capacity
was 267 g-K/L-resin and 255 g-Cl/L-resin, respectively.

Figure 4. Ion removal efficiency for recycling of spent leaching solution.

Figure 4. Ion removal efficiency for recycling of spent leaching solution.

SEM analysis of the resin before and after ion exchange showed that cation-resin size ranged
from 100 to 700 µm and anion-resin size ranged from 500 to 800 µm (Figure 5). After the reaction, the
ion-exchange resin had a rougher surface than before, and surface analysis using energy dispersive
spectroscopy (EDS) showed that fresh and spent resin had different components. After the ion exchange,
the resin surface contained 12.9% K and 13.5% Cl and the ions in the solution were effectively removed
(Figure 4). Figure 4. Ion removal efficiency for recycling of spent leaching solution.

N O S Al Si K Ca Fe

(a) Fresh 27.2 37.9 34.8 - - - - -

Cation resin (%)
(b) Spent - 42.6 20.2 3.0 2.5 12.9 13.3 5.5

N O F Cl Ca

(c) Fresh 67.7 28.8 3.6 - -

Anion resin (%)
(d) Spent N84.7 O - S -
Al Si 13.5
K Ca 1.8 Fe

(a) Fresh 27.2 37.9 34.8 - - - - -

Cation resin (%)
(b) Spent - 42.6 20.2 3.0 2.5 12.9 13.3 5.5

N O F Cl Ca

(c) Fresh 67.7 28.8 3.6 - -

Anion resin (%)
(d) Spent 84.7 - - 13.5 1.8

Figure 5. SEM images and EDS analysis of ion-exchange resins; (a) fresh cation-resin, (b) spent
cation-resin, (c) fresh anion-resin, (d) spent anion-resin.
 SEM analysis of the resin before and after ion exchange showed that cation-resin size ranged
from 100 to 700 μm and anion-resin size ranged from 500 to 800 μm (Figure 5). After the reaction, the
ion-exchange resin had a rougher surface than before, and surface analysis using energy dispersive
spectroscopy (EDS)
Environments 2019, 6, 113 showed that fresh and spent resin had different components. After the 6ion of 7
exchange, the resin surface contained 12.9% K and 13.5% Cl and the ions in the solution were
effectively removed (Figure 4).
After leaching,
After leaching, thetheKKandandClCl
ions in the
ions in solution werewere
the solution removed by ionby
removed exchange, while the
ion exchange, leaching
while the
solution was recovered and reused up to three times (Figure 6). The removal efficiencies
leaching solution was recovered and reused up to three times (Figure 6). The removal efficiencies of K and ofCl
extracted
K from the CKD
and Cl extracted from were found
the CKD to be
were similar,
found indicating
to be that leaching
similar, indicating thatsolution
leachingcan be effectively
solution can be
recycled. Recycling the leaching solution can significantly reduce the wastewater
effectively recycled. Recycling the leaching solution can significantly reduce the wastewater generated from the
CKD treatment,
generated from thewhichCKD can have a positive
treatment, which caneffect on the
have processeffect
a positive operation.
on the process operation.

Figure 6. Leaching test of CKD with recycled leaching solution. Reaction conditions: Reaction
Figure 6. Leaching test◦ of CKD with recycled leaching solution. Reaction conditions: Reaction
conditions: L/S = 20, 25 C. 1 atm.
conditions: L/S = 20, 25 °C. 1 atm.
4. Conclusions
4. Conclusions
This study assessed the use of different leaching solutions for removing chloride and potassium
from CKDstudy
This assessed
to allow the in
its reuse usecement
of different leaching solutions
manufacturing. Although fororganic
removingacidschloride and as
were twice potassium
effective
from CKD to allow its reuse in cement manufacturing. Although organic acids were
as distilled water, the latter was selected for further tests due to its higher handling safety and twice as effective
ease of
as
recycling. Distilled water was able to remove over 90% of Cl and over 70% of K within 1 min underease
distilled water, the latter was selected for further tests due to its higher handling safety and the
of recycling.
condition of Distilled
L/S 20. Inwater was ablereaction,
the leaching to remove theover 90% of Cl and in
Ca concentration over
the70%
CKD of increased
K within 1upmin
to under
5 min,
the condition
however, of L/S
Ca was 20. In
eluted at the leaching
>5 min, reaction,
reducing thecontent
the Ca Ca concentration
in the CKD.inIt thewasCKD increased
confirmed thatup to 5
control
min,
of thehowever, Ca was
reaction time eluted
is an at >5 min,
important reducing the Ca content in the CKD. It was confirmed that
parameter.
control of the reaction time is an important
Furthermore, Cl and K could be removed parameter.
from the leachate through ion exchange to allow
Furthermore, Cl and K could be removed
leaching solution recycling and to minimize wastewater from thegeneration.
leachate through ion exchange
The ion-exchange to allow
capacity was
leaching solution recycling and to minimize wastewater generation. The ion-exchange
255 g-Cl/L-resin and 267 g-K/L-resin under a flow rate of 40 mL/min, and all showed similar removal capacity was
255 g-Cl/L-resin
efficiencies of 95%andor267
moreg-K/L-resin underand
when recycled a flow ratethree
eluted of 40 times
mL/min, and
after ionall showed similar removal
exchange.
efficiencies of 95% or more when recycled and eluted three times after ion exchange.
Author Contributions: Conceptualization, M.S. and S.-S.C.; methodology, M.S. and S.-Y.L. and C.L.; formal
Author
analysis,Contributions: Conceptualization,
M.S., C.L. and S.-Y.L.; M.S. draft
writing—original and S.-S.C.; methodology,
preparation, M.S. and S.-Y.L.
M.S.; writing—review and and C.L.;M.S.
editing, formal
and
analysis, M.S., C.L. and S.-Y.L.; writing—original
S.-S.C.; project administration, S.-S.C. draft preparation, M.S.; writing—review and editing, M.S. and
S.-S.C.; project administration, S.-S.C.
Funding: This study was supported by the Energy Development Technology Program of the Korea Institute of
Energy Technology Evaluation and Planning (KETEP) granted financial resources from the Ministry of Trade,
Industry and Energy, Korea (20182010202100).
Conflicts of Interest: The authors declare no conflict of interest.
Environments 2019, 6, 113 7 of 7

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