RESEARCH ARTICLE O.A. Jimoh, T.A. Otitoju, H. Hussin, K.S. Ariffin and N.

Baharun, 1
S. Afr. J. Chem., 2017, 70, 1–7,
<http://journals.sabinet.co.za/sajchem/>.

Understanding the Precipitated Calcium Carbonate (PCC)

Production Mechanism and Its Characteristics in the
Liquid–Gas System Using Milk of Lime (MOL) Suspension
a b a
Onimisi A. Jimoh , Tunmise A. Otitoju , Hashim Hussin ,
Kamar Shah Ariffina,* and Norlia Baharuna
a
School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia, 14300 Nibong Tebal,
Penang, Malaysia.
b
School of Chemical Engineering, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia.

Received 3 April 2016, revised 15 August 2016, accepted 5 September 2016.

ABSTRACT
This study investigates the effect of operating variables and influence of milk of lime (MOL) conditions in PCC using a modified
reactor. The variables includes: Ca(OH)2 feed concentration at 0.5 M–2.0 M and CO2 flow rates at 224.0 mL min–1 and
379.5 mL min–1, on the particle morphology and size in the gas–liquid route precipitation. The particle morphology and texture as
well as the chemical content were sufficiently authenticated using X-ray diffraction (XRD), Fourier transform infrared spectros-
copy (FTIR), scanning electron microscope (SEM) and X-ray fluorescence (XRF). Experimental data show that lower concentra-
tion (<1.0 M) favoured the formation of rhombohedra calcite crystals with the particle size below 100 nm. However, increase in
concentration and gas flow rate yielded a coarser crystal particles. Two polymorphs were produced at 1 M reactant, i.e. rhombohedra
calcite with CO2 flow rate of 224 mL min–1 and prismatic calcite at 380 mL min–1. Molarities higher than 1 M yielded a coarser
prismatic crystals, and also has a tendency to crystallize into scalenohedron species especially with higher reactant concentration.
KEYWORDS
Milk of lime, precipitated calcium carbonate, morphology, particle size, carbonation.

1. Introduction ambient pressure. There are anhydrous phases of aragonite,

Precipitated calcium carbonate (PCC) is a filler used in many vaterite, calcite and hydrated phases of monohydrocalcite as
applications, like papers, plastics, rubbers, paints, drugs and so well as hexahydrocalcite.6 The anhydrous CaCO3 can be classi-
on. Its high purity, well-ordered particle size and morphology fied as rhombic calcite, needle-like aragonite or spherical
makes it the white filler of choice.1 In paint production, PCC vaterite and among them calcite is known to be the most stable
has established itself as a primary extender due to its unique phase under ambient atmospheric conditions.7 The formation of
properties such as its low basic colour, high weather resistance, any of these three polymorphs is strictly dependent on some
relative abrasiveness, low electrolyte content, non-toxicity and parameters such as the temperature, supersaturation and pH of
the pH stabilizing effect. Different kinds of crystal are suitable reaction solution.8 The control of calcium carbonate polymorphism
for a particular application and only the right PCC can boost is an intricate interplay amid thermodynamic and kinetic factors.9
the quality of the end products. Precipitated calcium carbonate The work by Ciullo10 shows that high purity PCC (>95 %) can be
produced with a prismatic and rhombohedral-shape has maxi- produced using pseudo-catalytic lixiviant to selectively extract
mum light dispersion at 0.4 to 0.5 µm sized particles while a calcium from slag material before being dissolved as PCC. Also
scalenohedral-shaped precipitated calcium carbonate has maxi- Adams11 showed that high purity PCC can be produced from
mum light dispersion of 0.9 to 1.5 µm particles.2 PCC of steel slag using ammonium salts to selectively extract calcium
nanometer sized with rhombohedral morphology are highly from slags. They reported that the smallest solid to liquid ratio of
effective for use as coating in a paper making.3 5 g L–1 resulted in maximum calcium extraction efficiency (73 %)
There are several approaches in the prior art to synthesize PCC while using 100 g L–1 produced the lowest extraction efficiency of
having definite property like high purity, most of which are 6 %. Liu et al.12 tested the performance of two organic acid
conversely focussing on this single property only. Although the (succinic and acetic acid) for the possible extraction of calcium
processes do not allow full control of other properties such as from steel slag for PCC production. They reported that the
crystal morphology, particle sizes, etc.4 carbonation of succinic acid leachate did not result in the pro-
The advantage of PCC lies in the prospect of tailor making the duction of PCC, whereas, the carbonation of acetic acid leachate
products with definite particle morphology, particle size and resulted in the synthesis of PCC.
distribution as well as specific surface area (BET). PCC is a A study by Suwanthai et al.13 shows that high purity PCC
refined natural form of limestone using techniques. The purity (mainly calcite) can be synthesized from gypsum waste by using
can be increased to 99.9 % or 99.999 %, and grain size can be an acid gas (H2S) to improve the aqueous dissolution of the
controlled in a range from submicron to more than 10 micron.5 poorly soluble CaS14, produced high purity PCC (mainly amor-
Calcium carbonate occurs in different crystalline polymorphs at phous) from medium and low grade limestone using strongly
* To whom correspondence should be addressed. E-mail: [email protected] acidic cation exchange resin. This improvement was due to
ISSN 0379-4350 Online / ©2017 South African Chemical Institute / http://saci.co.za/journal
DOI: http://dx.doi.org/10.17159/0379-4350/2017/v70a1
RESEARCH ARTICLE O.A. Jimoh, T.A. Otitoju, H. Hussin, K.S. Ariffin and N. Baharun, 2
S. Afr. J. Chem., 2017, 70, 1–7,
<http://journals.sabinet.co.za/sajchem/>.

the reaction of HCO3– in aqueous solution during the slaking Table 1 Experimental designs for the experiments.
reaction process. Valuable information from their work shows
that they were able to eliminate the influence of impurities Experiment Reactant concentration Gas flow rate –CO2
No. /M /mL min–1
during the carbonation reaction. Furthermore, Chen et al.15
studied a reaction precipitation of calcium carbonate by bubbling PCC A1 224.0
CO2 gas through a double-tube gas injection nozzle into milk of 0.2
PCC A2 379.5
lime (MOL) solution in an agitated closed batch reactor. In their
PCC B1 224.0
study, they observed that particle morphology and nucleation 0.56
PCC B2 379.5
were closely related to the reaction pH of solution.
PCC C1 224.0
The recarbonation process is the most common technique of 0.8
PCC C2 379.5
producing PCC. It is a complex process and involves simultaneous
dissolution of Ca(OH)2 and CO2 as well as the crystallization of PCC D1 224.0
PCC D2 1.0 379.5
CaCO3. Carbonation is generally carried out in a series of reactors
PCC D3
under closely controlled operating conditions to produce the
required PCC morphology and particle size distribution (PSD). PCC E1 224.0
1.5
PCC E2 379.5
Luo et al.16 studied the synthesis of vaterite PCC via carbonation
route under controlled pH condition. They reported that buffer PCC F1 224.0
PCC F2 2.0
solution highly influence the polymorphic phase of PCC while 379.5
PCC P8
CO2 concentration and rate of gas flow have no significant influ-
ence. Furthermore, high purity spherical vaterite particles can be
synthesized under controlled reaction conditions. the terms of crystal morphology and growth sizes of PCC
This work investigates the transition effects of reactant con- formed under specific operating conditions and parameters
centration and gas flow rate on PCC morphology and crystallite setting. In this case, precipitation or recarbonation processes
size using gas–liquid route via a modified batch-wise, bubble- were conducted at two predetermined CO2 gas flow rates over a
column type reactor. period of 60 and 90 min resident time. Reactant concentrations
were fixed between 0.2 and 2.2 M, and conducted at ambient
2. Materials and Experimental Methodology temperature and pressure conditions, respectively.
In this research, limestone used for the experiments was The pH, reaction temperature, conductivity/resistivity and
calcined in a muffle furnace at an optimum disassociation total dissolved solid (TDS) of the reactant during the stages of
temperature and resident time. The raw materials used in this recarbonation process were closely monitored (using Istek
research are high purity limestones, which are generally free K4000-EC) for the product characteristics and process mechanism
from any major contaminants (purity >98 %) for ‘milk of lime’ analysis. The resultant PCC after recarbonation were recovered
with less than 2 % impurities made of mostly silica (SiO2). How- by filtering through membrane filter, washed using distilled
ever, the impurity does not present any significant discoloration water and dried at 105 °C for 24 h and subsequently analyzed for
in the final PCC. morphology, particle size distribution, and purity. Effects of the
Chunks of limestone were crushed into a manageable size concentration and CO2 flow rates on particle morphology and
range of 10–20 mm diameter before calcined in a muffle furnace size were investigated. The degree of recarbonation to form PCC
at an optimum disassociation temperature and resident time. was determined by loss on ignition (LOI). The morphology
High reactive and low decrepitating quicklime (CaO) was and particle size of PCC of each samples were examined under
attained at an optimum calcining temperature of 1100 °C at scanning electron microscope (SEM). Prior to SEM examination,
90 min. The resulted quicklime is then hydrolyzed into distilled these PCC powders were dispersed in methanol and ultrasoni-
water to produce creamy hydrated-lime. In the slaking process, cally treated to reduce particle aggregation.
lumps of quicklime disintegrated to produce creamy white
smooth paste of hydrated-lime Ca(OH)2 suspension, and is sub- 3. Results and Discussion
sequently diluted in excess distilled water to produce different In the carbonation process, solid Ca(OH)2 is first dissolved as
‘milk of lime’ molarities. The resulting ‘milk of lime’ suspension soluble Ca2+ and OH– ions, while CO2 is absorbed in water in the
is then screened to remove any coarse grits and impurities to less form of weak H2CO3 and then converted to H+, HCO3– and CO32–
than 105 µm. Presence of trace amount of aluminium-silicate ions. Then Ca2+ combines with CO32– to form CaCO3, whilst H+
bearing minerals such as fine clay particles, carbonaceous and OH– merge to form H2O. The rate of recarbonation seems
matters, over burned or residual calcium carbonate generally directly related to the reactant concentration, bubbling time and
has insignificant effect on the slaking process. The resulted PCC CO2 gas flow rate conditions, and eventually affects the charac-
produced from various experimental designs were carried out to teristics of the resulting PCC.
characterize its crystal morphology, particle size distribution
pattern, state of agglomeration, and chemical purity. Table 1 Ca(OH)2(aq.) + CO2(g) Þ CaCO3 + H2O
shows the experimental designs for these experiments.
3.1. Effects on Conductivity and pH
2.1. Precipitation/Recarbonation Process Reactant concentration at a particular time during the course
These experiments were carried out in a one liter modified of the reaction can be monitored by conductivity and pH.
batch-wise, bubble-column type reactor (Fig. 1) containing During the course of precipitation, the pH, conductivity (Fig. 2)
500 mL milk of lime with a constant stirring speed of 300 rpm (the and TDS values gradually decreases in tandem with the prog-
optimum stirring speed in this experiment). The experiment ress of recarbonation process and abruptly dropped to the low-
was designed to investigate and foresee the influence of reactant est level at specific moments during the course of precipitation.
concentration and gas flow rate towards resulted PCC character- At low initial concentrations, the solid Ca(OH)2 is rapidly dis-
istics and precipitation process mechanisms. This is especially in solved and depleted in a short period of time during the course
RESEARCH ARTICLE O.A. Jimoh, T.A. Otitoju, H. Hussin, K.S. Ariffin and N. Baharun, 3
S. Afr. J. Chem., 2017, 70, 1–7,
<http://journals.sabinet.co.za/sajchem/>.

Figure 1 Modified batch-wise, bubble-column type reactor.

of precipitation to form PCC crystallite. Rapid consumption of that a complete PCC precipitation process was attained at a
Ca2+ and OH– witnessed a decrease in pH of 12 to neutral (pH 7), point where there were no more excess Ca2+ available. Higher
TDS and conductivity values. reactant concentrations need a longer bubbling time, and this
This consequently will affect the characteristics of produced can be compensated by increasing the gas flow rate. Excess gas
PCC, e.g. particulate sizes and crystal morphology. Dissolution supply only resulted in dissolved CO2 to form a weak HCO3–,
of Ca(OH)2 and CO2 increases the concentration of ionic charges and normally show a slight rebound in conductivity values
dissolved species, i.e. Ca2+, OH–, HCO3–, CO32–, CaOH+ and (Fig. 2).
CaHCO3+ during recarbonation. Progress in recarbonation,
gradually generated CaCO3 in the form of solids particles (less 3.2. Effect on Resistivity, Total Dissolved Solid (TDS) and
dissolved species), hence reduces the electrokinetic ability as Temperature
well as resulted to decrease in conductivity ability. This indicates Figure 3 shows a sudden and brief peak-up in resistivity

Figure 2 The changes in trend of (a) conductivity labelled A–F and (b) pH labelled A–F during the course of PCC precipitation process.
RESEARCH ARTICLE O.A. Jimoh, T.A. Otitoju, H. Hussin, K.S. Ariffin and N. Baharun, 4
S. Afr. J. Chem., 2017, 70, 1–7,
<http://journals.sabinet.co.za/sajchem/>.

Figure 3 (a) Sudden and briefly peak-up in resistivity values and (b) exothermic heat released during the recarbonation process at 379.5 mL min–1 gas.

values, which occurred at the same ‘dropped points’ as in pH of PCC increased with longer bubbling times. It seems that oper-
and conductivity trends. TDS values were also exhibiting similar ating temperature around 50 °C favoured crystallization of
trend as in conductivity and pH. rhombohedra calcite PCC. XRD pattern for experimental design
The TDS (mg L–1) usually drop to zero simultaneously with pH as shown in Table 1 is almost identical and consistent because
and conductivity at the same moments. Higher reactant concen- of the complete formation to calcite phase in all experimented
tration of 2.0 M and 1.5 M (PCC-E2 and PCC-F2) requires longer samples. All the samples show almost similar peak position and
recarbonation time. This can also be shortened by increasing the intensity. No peaks of Ca(OH)2 was present, thus indicating a
gas flow rate. However, morphology and other crystal character- complete recarbonation. Marked different in crystal morphology
istic of resulted PCC would not be the same. PCC precipitation is characteristics as shown by SEM micrographs (Fig. 5) can only be
an exothermic chemical reaction. In this study, the rise in tem- revealed by Fourier transform infrared spectroscopy (FTIR).
perature during the course of precipitation were observed in the FTIR spectrum shows typical absorption peaks of calcite around
order of 10 to 15 °C (Fig. 3). Higher reactant concentrations (e.g. 1433, 874 and 713 cm–1 (Fig. 4). This indicates that the formed
2.M in PCC F2) yielded greater amount of heat as compared to PCC have, somewhat, variation in crystal morphology or atomic
the lower one. structure during precipitation, which is hard to be defined by
the XRD spectrum.
3.2.1. XRD and FTIR Analysis
Figure 4 shows the gradual changes in the XRD patterns of 3.2.2. Chemical Composition and Purity
PCC produced at various operating variables and conditions. Tables 2 and 3 presents the results of XRF and LOI analysis.
Gradual increase in intensity was in tandem with phase con- LOI is best used to determine CaCO3 content. The mass loss
centration or growth rate of PCC followed by the reduction of corresponds to the released amount of CO2 (44 wt.%) during the
Ca(OH)2. Irrespective of reactant temperature, the growth rate firing process above dissociation temperature of limestone.

Figure 4 (a) XRD and (b) FTIR spectra of selected synthesized PCC produced at different operating variables and conditions.
RESEARCH ARTICLE O.A. Jimoh, T.A. Otitoju, H. Hussin, K.S. Ariffin and N. Baharun, 5
S. Afr. J. Chem., 2017, 70, 1–7,
<http://journals.sabinet.co.za/sajchem/>.

Figure 5 Crystal morphology and particles size distribution of lower (A2, D3) concentration and higher concentration (D2, B2, F2) PCC from this ex-
periments and also PCC-P8 after Ariffin.21

Results indicated that the produced PCC is very high in purity rhombohedra crystal morphology. At a lower reactant concen-
with an average of about 98.6 %. Other components, which are tration (e.g. PCC-A1-0.2 M), well-developed cubic-like, rhombo-
normally inherited from precursor stone are often less than hedra calcite were generally formed within the size order of 50
1.5 %. to 100 nm (Fig. 5). This result obtained by using the modified
reactor can be compared with results by several authors using
3.2.3. Crystal Morphology chemical additives to achieve smaller PCC particle sizes.
Figure 4 shows examples of the crystal phases of PCC produced Konopacka-ºyskawa et al.17 synthesized PCC particles using
at the selected concentrations, gas flow rates and bubbling times. aqueous of isopropyl alcohol, n-butanol and glycerol as solvent
Generally, calcium carbonate mineral phases crystallized into on lime slurry using carbonation process. They reported that an
three common crystal polymorphs (calcite, aragonite and increment of reactive mixture of isopropyl alcohol and
vaterite). However, there are other crystal morphologies that n-butanol concentration resulted in the high yield of smaller
have been discovered depending on different kind of operating PCC particles of approximately 2.5 µm. However, finer PCC
techniques and reactant used. At ambient conditions, calcite is a particles size of 0.1–0.59 µm were formed when single solution of
thermodynamically stable form of carbonate and has cubical 20 % glycerol concentration was used. Feng and Yon18 reported
RESEARCH ARTICLE O.A. Jimoh, T.A. Otitoju, H. Hussin, K.S. Ariffin and N. Baharun, 6
S. Afr. J. Chem., 2017, 70, 1–7,
<http://journals.sabinet.co.za/sajchem/>.

Table 2 XRF Analysis of PCC. Table 3 LOI (%) of synthesized PCC.

Component /wt.% Expt. Before fired After fired LOI CaCO3

–sample no /g /g /% /%
PCC A2 PCC D1
PCC A1 1.0017 0.5672 43.38 98.60
Al2O3 0.17 0.15
PCC A2 1.0003 0.5673 43.29 98.38
SiO2 0.24 0.19
K2O 0.015 Trace PCC B1 1.0060 0.5641 43.93 99.84
CaCO3 99.0 98.0 PCC B2 1.0015 0.5598 44.10 100.0
Fe2O3 0.034 0.014 PCC C1 1.0020 0.5601 44.10 100.0
NaO 0.019 0.02 PCC D1 1.0009 0.5620 43.85 99.66
CuO 0.10 0.10 PCC D2 1.0002 0.5592 44.09 100.0
SrO – 0.02 PCC E1 1.0054 0.5627 44.03 100.0
P2O3 – 0.03 PCC E2 1.0029 0.5685 43.31 98.43
MgCO3 – 1.1 PCC F2 1.0008 0.5701 43.04 97.81

Figure 6 Crystallization hypothesis for PCC production in the liquid-gas system from Ca(OH)2 suspension.

an average particle size of 1 to 3 µm at ambient temperature tion control. By varying such variables and conditions, we were
when EDTA and terpineol were used. Studies by Xiang et al.19 able to understand and manipulate crystal morphology and
also reported that addition of 1 % (w/w) ZnCl2 shows an obvious other characteristics like crystallite size and distribution patterns
decrease in PCC particle size and 0.2 µm diameter of spherical by using limestone as a starting commercial material. A low reac-
PCC particles was formed. tant concentration (0.2 M) favours the formation of cubic-like,
Further increase of flow rate (379 mL min–1) resulted in slightly rhombohedra calcite with almost uniform particle size distribu-
coarser PCC (PCC-A2). This is consistent with the work by tion. Increasing the reactant concentration to specific levels, e.g.
Agnihotri et al.20, that the particle size decreases with decrease in up to 0.56 M, prismatic calcite morphology start to emerge. At
CO2 concentration. Reactant concentration (PCC-B1-0.5M) often higher level ‘milk of lime’ concentration such as at 2.0 M and
doubled the crystal size of these rhombohedra PCC within the 2.2 M, scalenohedron calcite was gradually formed. The crystal-
order of 100 to 150 nm. Higher gas flow rate at 379 mL min–1 does lization hypothesis would be useful in predicting the production
not result to much change in size of this PCC-B2. At the of desired PCC characteristics rather than varying those operat-
224 mL min–1 gas flow rate, the resultant PCC-D1 retained its ing variables. This model diagram can easily be modified to
initial rhombohedron shape. Gradual transformation of calcite include effects of reactant temperature, pressure and presence
rhombohedra to prismatic (seed-like) calcite morphology was of additives later.
only observed at the 1.0 M with 379.5 mL min–1 (PCC-D2) gas
flow rate. This PCC-D2 possesses a crystal dimension of 175 nm Acknowledgement
by 100 nm. At the higher concentration of 2.22 M (PCC-P8), The second author acknowledges Universiti Sains Malaysia
scalenohedron calcite PCC was precipitated. ‘Milk of lime’ con- (USM) for an e-science fund fellowship grant.
centrations higher than 1.0 M, usually exhibit prismatic
‘seed-like’ PCC morphology (PCC-F1 and PCC-F2). They usually References
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