High purity (>99%) precipitated calcium carbonate, PCC was synthesized from abundant waste material (carbide sludge), generated during acetylene gas production. The reaction influencing parameters based on temperature, flow rate, total dissolved solid and carbide lime concentration were investigated.

1. ORIGINAL ARTICLE
Utilization of milk of lime (MOL) originated from carbide lime
waste and operating parameters optimization study for potential
precipitated calcium carbonate (PCC) production
Onimisi A. Jimoh1,2 • Norsuria Mahmed4 • P. U. Okoye3 • Kamar Shah Ariffin1
Received: 28 October 2015 / Accepted: 6 September 2016
Ó Springer-Verlag Berlin Heidelberg 2016
Abstract Vast amounts of carbide lime waste generated as
a by-product of acetylene gas production require urgent
utilization to avert handling and disposal difficulties. The
carbide lime waste is often rich in calcium hydroxide
(Ca(OH)2), rendering it an alternative potential precursor
for precipitated calcium carbonate (PCC) production. The
study demonstrated that suspension of carbide lime can be
utilized to synthesize PCC at favorable conditions. The
characteristics and crystal morphology of the lime and as-
synthesized PCC were determined using X-ray fluores-
cence and scanning electron microscope. The influencing
reaction parameters based on temperature, flow rate, total
dissolved solid and carbide lime concentration were
investigated. Under specific reaction conditions of 2 M
carbide lime concentration, final pH of 6.98, 90 min, and
452.30 mL/min CO2 flowrate, high purity of 99 % PCC
was attained. The produced PCC from carbide lime meets
end user requirement on a par with conventional PCC
products.
Keywords Carbide lime Á Precipitated calcium carbonate Á
Total dissolved solid Á Waste utilization
List of symbols
K Molar conductivity (Sm2
/kmol)
k Conductivity (conductance per meter S/m)
C Concentration (kmol/m3
or mol/L)
M Molarity (mol/L)
Introduction
As a result of the fast and alarming depletion of mineral
resources, attention has been redirected to the identification
of more eco-friendly and renewable alternative sources.
Waste from acetylene gas production, which is rich in
calcium, is an alternative high-quality hydrated lime source
(Kenny and Oates 2000). Usually, the carbide sludge is
washed into settling ponds, creating a lime mud that poses
difficulties in utilization. Although there is no approved
method for carbide sludge disposal, the large lime ponds
remain a reservoir for soil liming material that is compa-
rable in quality to basic hydrated lime. These large ponds
for settling lime mud adversely impact the environment
(Ayeche and Hamdaoui 2012). Furthermore, the charac-
teristic of carbide lime, such as high alkalinity (pH 12.5),
unpleasant odor, irritation to skin and throat poses severe
difficulty in handling (Armour 2003). In addition, the lime
manufacturing process is energy intensive and generates
undesired CO2 (Ma et al. 2015; Watkins et al. 2010) as an
unavoidable by-product. However, the unique mineral
compositions of carbide lime waste such as high calcium
hydroxide (Ca(OH)2) and other minor minerals of carbon,
ferrosilicon, silica, traces of inert mineral confers on it a
suitable potential material for many applications. Particu-
larly, the high calcium hydroxide content of carbide lime
can be utilized in hydroxyapatite production, catalysis, and
precipitated calcium carbonate (PCC) production.
& Kamar Shah Ariffin
kamarsha@usm.my
1
School of Materials and Mineral Resources Engineering,
Universiti Sains Malaysia Engineering Campus,
14300 Nibong Tebal, Malaysia
2
Department of Geology, Federal University Lokoja,
Lokoja, Nigeria
3
School of Chemical Engineering, Universiti Sains Malaysia,
14300 Nibong Tebal, Malaysia
4
School of Materials, Universiti Malaysia Perlis, 02600, Arau,
Perlis, Malaysia
123
Environ Earth Sci (2016)75:1251
DOI 10.1007/s12665-016-6053-z

2. Recent advances in the utilization of carbide lime have
focused on PCC production because of its humongous
applications. As long as PCC meets certain purity
requirement, it can be utilized as an artificial pigment in
paper, plastics, drug carriers in pharmaceuticals, sealants,
food industries, paint manufacturing and fillers in adhe-
sives (Nasser et al. 2015; Thenepalli et al. 2015). As a filler
material, it provides high tensile reinforcement due to its
unique particle size and morphology (Sae-oui et al. 2009).
PCC is usually produced via three routes, namely the cal-
cium hydroxide–sodium hydroxide, calcium chloride–
sodium carbonate double salt decomposition process, and
carbonization process (Onimisi et al. 2016). All these
routes utilize milk of lime usually generated from lime-
stone. The limestone is first calcined (*1000 °C) to form
CaO. Thereafter, the obtained lime is screened to remove
impurities in the limestone and the lime is dispersed in
water to form milk of lime. Finally, CO-2
gas is passed in
the milk of lime resulting in calcium carbonate precipita-
tion. Therefore, the CO2 produced during the calcium
carbide production can as well be channeled to produce
PCC. This will minimize or compensate for the high
energy input during calcium carbide production. The car-
bonation process enables PCC of a given specification to be
produced in a dedicated plant, irrespective of the local
geology. The fineness of the particles, as well as the crystal
morphology (e.g., aragonite, calcite), is controlled by
temperature, concentration of reactants and time. The
process is environment-friendly and does not emanate toxic
pollutants (Suwanthai et al. 2015).
As a continuous effort to utilize waste materials gener-
ated from industries, researchers have produced PCC using
varying wastes from gypsum and steel slags (Mattila et al.
2012). Ciullo (1996), reported that high purity PCC
([95 %) can be produced using pseudo-catalytic lixiviant
to selectively extract calcium from slag material before
being dissolved as PCC. Also, ammonium salts have been
used to selectively extract calcium from steel slag, result-
ing in high purity PCC product and reduction in CO2
emission (Adams 2005; De Crom et al. 2015). They
reported that the smallest solid to liquid ratio 5 g/L resulted
in the maximum calcium extraction efficiency (73 %),
while the reverse using 100 g/L produce the lowest
extraction efficiency of 6 %. Liu et al. (2016), investigated
the performance of two organic acids (succinic and acetic
acid) for the possible extraction of calcium from steel-
making slag for PCC production. They observed that the
carbonation of succinic acid leachate did not result in the
production of PCC, while the carbonation of acetic acid
leachate resulted in the synthesis of PCC. Furthermore,
studies by Suwanthai et al. (2015) hinted that high purity
PCC (mainly calcite) can be synthesized from gypsum
waste by using an acid gas (H2S) to improve the aqueous
dissolution of the poorly soluble CaS. Huang et al. (2007)
produced high purity PCC (mainly amorphous) from
medium and low-grade limestone using strongly acidic
cation exchange resin. This improvement was due to the
reaction of HCO3
-
in aqueous solution during the slaking
reaction process. Valuable information from their study
indicated that impurities were eliminated during the car-
bonation reaction.
The use of carbide lime waste for the synthesis of PCC
has not been adequately reported. Therefore, the appro-
priate techniques, operating conditions and physical prop-
erties of carbide lime sludge in PCC production were
envisaged for the first time in this study. Also, the influ-
encing parameters that control the precipitation process,
products morphology and particle size were thoroughly
investigated.
Experimental methodology
Material
In order to carry out this experiment, calcium carbide
produced by MCB industries Sdn. Bhd (Malaysian Carbide
Berhad), Kemunting, Taiping was used. The typical
chemical composition [by X-ray fluorescence (XRF)] of
the CaC2 is tabulated in Table 1. Pure CO2 gas was sup-
plied by Merck. Conductivity meter-Istek 455C model for
pH, reaction temperature, conductivity and total dissolved
solid (TDS) online monitoring.
Hydrated milk of lime precipitation
Hundred grams calcium carbide was dissolved in 1 L
double distilled water, resulting in acetylene gas liberation
and precipitation of hydrated lime (Ca(OH)2). When the
reaction is complete, observed from high pH [12, the
resultant hydrated lime is then dried in an oven at 105 °C
for 8 h, and subsequently screened to obtain 125 lm
powder. In this investigation, various concentration of milk
of lime was prepared from the carbide lime powder and
experimented in accordance with operating variables as
designed in Table 2. Milk of lime suspension produced by
dissolution of dried carbide lime powder was screened to
remove any coarse grits that may affect PCC particle
morphology.
Precipitated calcium carbonate production
The precipitation of calcium carbonate production using
CO2–Ca(OH)2 was carried out in an agitated reaction
vessel (a 1000 mL rounded glass with a multi-socket
reaction vessel). CO2 gas was bubbled through the batch
1251 Page 2 of 7 Environ Earth Sci (2016)75:1251
123

3. reactor containing Ca(OH)2 generated from the carbide
lime sludge. The pH, temperature and conductivity changes
taking place during the course of the precipitation reaction
were monitored by the conductivity meter. A high pH ([9)
generally indicated the presence of free lime and a corre-
sponding high surface potential. Effects of the milk of lime
concentration, CO2 gas flow rates, reaction time on particle
morphology and size were investigated. Finally, the syn-
thesized PCC was screened below 45 lm, dewatered, dried
and then characterized.
PCC characterization
The morphology and particle size of PCC for each sample
were examined by scanning electron microscope (VPSEM,
Carl Zeiss, SUPRA35VP model). Prior to SEM examina-
tion, the various PCC powder samples were dispersed in
methanol, ultrasonically treated to reduce particle aggre-
gation then coated with gold to improve material
conductivity. The chemical composition of the powdered
samples was analyzed using a Rigaku RIX 3000 X-ray
fluorescence spectroscopy. Powder samples were used to
make fusion bead before analyzing elements.
Results and discussion
In this reaction, feed concentration, gas flow rate and
reaction time are the important operating variables to
control PCC properties. The particle formation and growth
process in the precipitation, which depend directly on the
supersaturation of solution, vary with the milk of lime
concentration, time and gas flow rate. The rate of particle
growth and the particle is critically determined by the
mixing of milk of lime suspension and gas phases. Hence,
the stirring efficiency suggests that if Ca(OH)2 dissolution
reaction regime is chemically or diffusional controlled.
Therefore, all the experiments were conducted above
Table 1 Typical chemical
composition of CaC2 and PCC
(by XRF)
Composition (wt%) MCB carbide Other typical carbidea
PCC (exp. 8)
SiO2 0.75 0.34–3.40 0.44
SiO2 ? insoluble – 0–2.2 –
Al2O3 ? Fe2O3 0.365 1.2 0.169
Al2O3 0.270 0.06–8.80 0.12
Fe2O3 0.095 0.01–0.11 0.049
CaO 58.6 54–57.40 –
K2O 0.0003 0.01–0.03 –
MgO 0.29 0.098–0.22 –
SO3 0.10 – 0.033
P2O5 0.035 – –
SrO 0.05 – 0.014
CaCO3 – – 99 ??
Free carbon 9.10 – –
CO2 – 2.0 –
LOI 30.43 30.05–44.30
MCB Malaysian carbide Berhad
a
Muntohar et al. (2016) and Othman et al. (2015)
Table 2 Experimental operating variables setting and carbonate content of resultant PCC
Experiment no. Molarity
(M)
Reaction
time (min)
Flow rate
(mL/min)
CaCO3 content
of PCC (wt%)
Final pH
of reaction
1 (PCC 1) 1.0 60 262.60 76.86 7.91
2 (PCC 2) 90 83.55 6.82
3 (PCC 3) 60 452.30 77.98 7.83
4 (PCC 4) 90 85.64 6.92
5 (PCC 5) 2.0 60 262.60 74.25 8.12
6 (PCC 6) 90 88.93 7.0
7 (PCC 7) 60 452.30 81.57 7.71
8 (PCC 8) 90 99.18 6.98
Environ Earth Sci (2016)75:1251 Page 3 of 7 1251
123

4. [400 rpm to overcome mass transfer barrier and sustain
the PCC production to chemically controlled reaction
regime.
Influence of reactant concentration and reaction
time on PCC production
At different milk of lime molar concentration (1 and 2 M),
varying time (60 and 90 min) and flow rates (262.60 and
452.30 mL/min), PCC of various shapes and purity were
produced. The yield of PCC is presented in Table 2, while
the morphology of the resultant PCC for the 8 experiments
are presented in Figs. 1 and 2, for 1 and 2 M milk of lime
molar concentration, respectively. Observably from Table 2,
1 M milk of lime concentration at 60 min reaction time and
262.60 mL/min CO2 gas flow rate, resulted in a cluster of
short or long structured prismatic scalenohedron shapes
(Fig. 1a, PCC-1) with estimated individual particle size less
than 0.5 lm. The scalenohedron shapes formation is likely
as a result of Ca(OH)2 pH close to 13. However, the indi-
vidual particle size appears coarser, double or triple of PCC-
1 size, at prolonged reaction time (90 min) (Fig. 1b, PCC-
2). Mattila et al. (2012), reported in their study of PCC
production using steel slag that coarse particle sizes evolve
as a result of longer reaction time. Increasing the Ca(OH)2
concentration to 2 M at 262.60 mL/min CO2 flow rate and
60 min reaction time, displayed a well-defined rosette
scalenohedron calcite (Fig. 2e, PCC-5). However, increase
in bubbling time of CO2 from 60 to 90 min tends to produce
even more distinct rosette scalenohedron calcite crystal
(Fig. 2f, PCC-6) with more marked spindle-like feature
rather than prismatic look (Feng et al. 2007). This can be
explained by increased mass transfer of CO3
2-
into the
solution and consequent increase in ionic strength of the
milk of lime. The mass transport of these carbonate ions into
the solution is a function of the stirring efficiency and can be
tailored by appropriate selection of stirring speed. Hence, the
optimum purity and desirable scalenohedron calcite PCC
morphology was obtained at 2 M milk of lime concentra-
tion, 90 min reaction time and 452.30 mL/min CO2 gas
flowrate (Fig. 2h, PCC-8).
Influence of CO2 gas flow rate on PCC yield
The CO2 inlet gas was supplied through a frit of 10–40 lm
which resulted in a gas bubble of 1.2 mm diameter. Pro-
duction of PCC requires small bubble size to overcome
mass transfer barrier and enhance liquid to gas contact
leading to smaller particle sizes. The purity of obtained
PCC at 1 M Ca(OH)2 molar concentration and fixed
PCC-1 PCC-2
PCC-3 PCC-4
Fig. 1 Images of the synthesized PCC (PCC-1 to PCC-4) produced at a reactant concentration of 1 M
1251 Page 4 of 7 Environ Earth Sci (2016)75:1251
123

5. reaction times (60 and 90 min) increased marginally
(Table 2) as CO2 flow rate increased (262–452 mL/min).
However, different crystals morphology was observed at
different reaction times which are attributed to increasing
CO2 flow rate. The PCC-3 (Fig. 1c) produced at similar
conditions as PCC-1, displayed a cubic-like rhombohedron
crystal morphology particle. This can be explained by the
presence of lower ionic strength or OH-
of the Ca(OH)2
suspension with higher a presence of CO2 gas, promoting
the yield of rhombohedron crystals. Similarly, PCC-4
produced at same conditions [1 M Ca(OH)2 and 90 min]
and different CO2 flowrate as PCC-2 presented a closely
packed cluster of dendritic-like (radiated) scalenohedral
PCC particles, prismatic to needle-like crystals (Fig. 1d).
In general, increasing the bubbling rate not only reduced
the particle size but also resulted in a change in crystal
morphology. For the higher reactant concentration (2 M
Ca(OH)2), boosting the rate of CO2 flow triggered gener-
ation of finer PCC powder. In spite of that, PCC-6 (Fig. 2f),
with a good scalenohedral crystal was attained, increasing
the flow rate and bubbling time has significantly reverted
the crystal shape again into cubic-like, rhombohedron PCC
(Fig. 2h, PCC-8).
Temperature–conductivity relationship
Conductivity sensors are usually used to measure the
concentration of total dissolved solids (TDS) during PCC
production. The conductivity of acid or base depends on
both ion concentration and ion mobility. The ion mobility
is promoted by temperature which increases about 2 % for
each °C increase in temperature. The degree at which
temperature affects conductivity depends on the types of
ions involved. The gradual temperature increase, and
decreasing conductivity and TDS at precipitation reaction
regime are presented in Figs. 3, 4 and 5. From Fig. 3, the
conductivity for 8 PCC experiments decreases steadily
with increasing precipitation time. Similarly, the TDS
decreases as the conductivity decreases (Fig. 4). Since the
pH is a measure of hydrogen ion concentration, hence,
lower pH (i.e., higher H?
ion concentration) translates to
higher conductivity. It is crucial to end the precipitation
reaction at optimum pH where efficient and effective
conversion of milk of lime to CaCO3 is achieved and
before the CO2 concentration becomes too high (increased
acidity) to initiate dissolution of the suspended CaCO3
precipitate. The initial pH of the milk of lime is greater
PCC-5 PCC-6
PCC-7 PCC-8
Fig. 2 Images of the synthesized PCC (PCC-5 to PCC-8) produced at a reactant concentration of 2 M
Environ Earth Sci (2016)75:1251 Page 5 of 7 1251
123

6. than 12.5. The final pH monitored presented a variation of
7.0–6.8 for all PCC’s produced at 90 min reaction time.
However, pH of the PCC’s produced at 60 min reaction
time varied in the range of 8.1–7.7 as observed from
Table 2. Consequently, the yield of CaCO3 varied with the
pH, where all PCC’s produced at final pH of 7.0–6.8 dis-
played higher yield of CaCO3 compared to those produced
at pH of 8.1–7.7. The pH around 7 signifies the end of the
precipitation reaction. Hence, the higher pH and conse-
quent lower CaCO3 yield for all PCC’s produced at 60 min
suggests possible incomplete precipitation of CaCO3. The
exponential decrease in the conductivity and TDS is
attributed to a decreasing number of free ions during the
precipitation reactions as the ions react to form solids. The
exponential decrease in TDS depends on the initial milk of
lime concentration and CO2 flow rate. Hence, the con-
centration of the solution at any time can be measured
using the mathematical relation (Eq. 1)
K ¼ k=C ð1Þ
where K (Sm2
/kmol), is the conductivity, k correction
factor (typically 0.7) and C is the concentration.
On the other hand, the recarbonation process which is
thermodynamically exothermic resulted in minimal heat
emission during the precipitation of CaCO3 (10–16 °C).
The temperature increase also depends on the concentra-
tion of initial milk of lime. As mentioned earlier an insight
into the effects of temperature–conductivity–TDS rela-
tionship suggests that as solution temperature increases up
to 40 °C (Fig. 5), the conductivity and TDS decreases
exponentially because of decreasing number of mobile ions
in the solution. This indicates that precipitation has
occurred.
X-ray fluorescence (XRF) studies
The XRF of the carbide waste and PCC-8 obtained at best
synthesis conditions are shown in Table 1. Evidently,
calcium oxide is the main mineral element of the carbide
waste with 54.96–57.40 and 58.6 % for computed and
obtained Malaysian carbide waste (Muntohar et al. 2016;
Othman et al. 2015). The slightly higher content of cal-
cium oxide in this work (Malaysian calcium oxide) sug-
gests greater potential for its utilization in PCC
production. Hence, chemical compositions of the calcium
carbide (Table 1) revealed no CaCO3 content in the raw
material, while synthesized PCC-8 contains 99 wt%
CaCO3. The other components (SiO2, Al2O3, Fe2O3, MgO
and P2O5) combined are ranged below 1 wt%, repre-
senting typical contents of minor importance. The effect
of impurities associated with the synthesized PCC seems
to be very insignificant as they are less than 1 % when
combined. The data clearly fall within the limiting values
known for pure PCC. Based on this XRF results, the
synthesized PCC from the carbide lime can be classified
as a high purity PCC.
Fig. 3 Conductivity declining during the course of precipitation of
PCC at various rates
Fig. 4 TDS declining in tandem with the progress of precipitation of
PCC at various rates
Fig. 5 Temperature of reactant increases as the precipitation pro-
ceeds as much as 16 °C
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123

7. PCC purity
The best PCC purity obtained at favorable precipitation
conditions are presented in Table 2. Evidently, PCC-8 is
outstanding with 99 % CaCO3 content and other minor
chemical elements under conditions of 2 M concentration
of milk of lime, 452.30 mL/min CO2 flow rate and 90 min
reaction time. The 99 % PCC produced from carbide lime
waste was estimated from the XRF studies and can be
compared with the commercial PCC. As discussed earlier,
the difference in morphology is a consequence of variable
reactant concentration, temperature, measure of final pH,
CO2 flow rate and reaction time, which advertently influ-
ences the particle size of resulting PCC. It should be noted
that agglomeration during the crystallization of PCC was
unavoidable, and the degree of agglomeration have a sig-
nificant effect in particle analysis. Dry PCC is very difficult
to disperse properly and have a tendency to form larger
crystal clusters. Particle size analysis by sedimentation
method frequently failed to provide satisfy results.
Depending on the preset operating variables and conditions
of the process, the scanning electron micrographs, SEM
(Figs. 1, 2) showed that most of the synthesized PCC are in
the range of 0.1–0.5 lm.
Conclusion
Conclusively, carbide lime sludge generated from acet-
ylene gas production can be successfully utilized to pro-
duce PCC. Operating parameters, such as CO2 gas flow
rate, temperature, reaction time, final pH and initial
hydrated lime concentration, influence the resulting pur-
ity, morphology and particle size of PCC. Increasing CO2
flow rate (from 262.60 and 452.30 mL/min) showed a
negligible increase in the obtained PCC purity; however,
the resulting crystal morphology changed significantly.
Also, the conductivity and TDS of the lime solution
decreased as the temperature increases during the pre-
cipitation reaction which can be attributed to in situ
decreasing mobile ions. Hence, at 2 M hydrated carbide
lime concentration, CO2 flow rate of 452.30 mL/min, and
pH of 6.98, 99 % pure PCC was achieved in 90 min
reaction time. Finally, regular, uniform crystalline of
scalenohedral, prismatic and blocky rhombohedron with a
definite particle size of 0.1–0.5 lm was obtained in all the
experiment.
Acknowledgments The Authors sincerely wish to thank people
whose assistance has made this effort became a reality, especially to
technical staff of the School of Materials and Mineral Resources
Engineering and Ministry of Science, Technology and Innovation
(MOSTI) Malaysia under e-science fund research Grant (603316).
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