Journal of Wuhan University of Technology-Mater. Sci. Ed. www.jwutms.net Feb.

2017 51

DOI 10.1007/s11595-017-1557-2

Viscosity of Kaolin Slurries: Effects of Dispersant

and Urea-Intercalation

QIU Xiumei1,2, LIU Yadong3, ALSHAMERI Aref 1, ZHU Xiaoyan1, YAN Chunjie1*
(1. Engineering Research Center of Nano-Geomaterials of Ministry of Education, China University of Geosciences, Wuhan 430074, China;
2. Hubei Province Geological Experimental Testing Center, Wuhan 430034, China; 3.Hubei Urban Construction Vocation and Technological
College, Wuhan 430205, China)

Abstract: Good fluidity (low viscosity) of highly concentrated kaolin is highly needed in paper-coating
industry. We put forward an effective route to improve the viscosity concentration of Beihai kaolin slurries. The
effects of various factors such as solid content, pH, dispersant content, and urea-intercalation on the viscosity of
kaolin slurries were investigated. The results revealed that the viscosity of kaolin slurries significantly decreased
with decreasing solid content or with increasing pH and dispersant content. It was worth noting that urea-
intercalation was proven to be an efficient method for promoting the dispersion of highly concentrated kaolin as
compared with adding dispersant. The intercalation ratio of urea-intercalated kaolin was increased from 17.36%
with 2% of urea addition to 81.30% with 6% of urea addition. Meanwhile, the viscosity concentration of raw
kaolin slurry was improved from 65.0% to 70.13% after the intercalation of urea with 6% addition, which
was attributed to finer particle size, increased pH value and more negative charges of urea-intercalated kaolin.
Therefore, the route is effective to improve the dispersion of highly concentrated kaolin for paper-coating.
Key words: beihai kaolin; dispersion; urea-intercalation; viscosity concentration

1 Introduction using a rotary viscometer at 60 rpm and is typically

Kaolinite, a clay mineral with 1:1 layer structure,
is abundantly stored on the earth and also world-widely
distributed. Owing to its unique properties, kaolin has
been applied in various areas, such as paper, cosmetics,
paint, rubber, plastics and ceramics industries,
especially in paper-making industry[1].
Kaolin is widely used as filler or coating to
smooth the surface and improve the brightness, opacity,
gloss and ink of paper in paper-making industry. The
high aspect ratio plates of kaolin exhibit good sheet
coverage and printability, which are very beneficial
for paper-coating applications[2]. Also, the fluidity of
highly concentrated kaolin is very important in the
processing of paper coating[3], which can be evaluated
by its viscosity or viscosity concentration. Viscosity
concentration is specified as a percentage value when
the viscosity is measured at 500 mPa·s and 22 ℃
©Wuhan University of Technology and SpringerVerlag Berlin Heidelberg 2017
(Received: Oct. 20, 2015; Accepted: Nov. 8, 2016)
QIU Xiumei(仇秀梅): Ph D; E-mail: qiuxiumeiqq@126.com
*Corresponding author: YAN Chunjie (严春杰): Prof.; Ph D;
E-mail: chjyan2005@126.com
Funded by Chinese Ministry of Land and Resources
(No.201311024)
used to evaluate a concentration of kaolin slurry in
kaolin industry. Usually, a relatively higher viscosity
concentration can result in a better fluidity of highly
concentrated kaolin slurry. For example, the viscosity
concentration of high quality kaolin (marked as ZT-
0A) used in paper-coating should achieve 70.0%[4]. To
our best knowledge, the kaolins produced from Brazil
and America usually show a viscosity concentration
above 70.0%, however, the viscosity concentrations
of kaolins produced from Pakistan, Zambia and China
are approximately 55.8%[5], 68%[5] and 50%-65%[6],
respectively, which precludes their utilization in paper-
coating industry. Beihai area (in China) has about 500
million tons kaolin reserves. Beihai kaolin possesses
a relatively low viscosity concentration (65.0%) as
compared with Brazilian and American kaolins, so that
it could not be used on high-speed coating machine
(>70.0%), which limits its applications in paper
manufacturing industry[7].
Recently, a large amount of effort has been paid
to improve the viscosity concentration of kaolin,
leading to its good paper-coating effect. It was found
that the viscosity concentration of kaolin slurries
was influenced by many factors, such as particle
shape, particle size distribution, particle thickness,
52 Vol.32 No.1 QIU Xiumei et al: Viscosity of Kaolin Slurries: Effects of Dispersant and ...
morphology, aggregation, surface charge, mineralogical
and chemical impurities in the clay[8,9]. Efforts have
been made through adjusting these properties to
improve the fluidity of kaolin slurries[10,11]. Mechanical
grinding, dispersants stirring and chemical delamination
were adopted to modify the fluidity of kaolin slurries
especially in the industry [12,13] . Dispersants were
usually employed to improve the dispersion of kaolin
particles. For instance, polyelectrolytes were often
selected as dispersants to make kaolin slurries stable
through creating electrostatic interaction and steric
hindrance[14]. Chemical delamination of kaolin which
was induced by intercalation of molecules such as
urea[5], dimethyl sulfoxide[15], and potassium acetate[16],
combining with mechanical comminution could cause
the weakness of interlayer hydrogen bonds. Therefore,
the layers of kaolin were easily displaced relatively to
one another to get a better dispersion. The physical and
chemical properties, crystal structure, as well as surface
chemistry of kaolinite particles could be modified
by intercalation technique[17]. Our previous work has
confirmed that urea-intercalated kaolin could be applied
for paper coating due to its excellent properties[5,18],
while without explaining its mechanism.
This work focuses on improving the fluidity
(viscosity concentration) of Beihai kaolin (Guangxi
Province, China). The influence of solid content,
pH, dispersant content and urea-intercalation on
the viscosity of kaolin slurries was systematically
investigated in order to make the viscosity
concentration of Beihai kaolin satisfy the requirement
of paper-coating (>70.0%). Particular attention was
given to illuminating the dispersion mechanism of urea-
intercalated kaolin, which was critical for application
in paper coating.
2 Experimental
2.1 Materials
Water-washed kaolin was collected from Beihai
District in Guangxi Province of China. The chemical
composition of the kaolin product measured by
X-ray fluorescence (XRF, PANalytical AXIOS mAX)
spectrometry is shown in Table 1. Sodium polyacrylate
(MW=3 000 g/mol, DC-FS) was supplied by Shandong
Gaoxu Chemical Co., Ltd. (Shandong, China). Urea of
analytical grade was purchased from Tianjin Chemical
Reagent Co. Ltd. (Tianjin, China).
2.2 Preparation of urea-intercalated kaolin
(slurries)
The urea intercalated kaolin was synthesized
by intercalation layer method. Beihai kaolin with the
moisture of 5 wt% and a certain amount of urea were
mixed together. The mixture was ground for about 30
minutes at room temperature and then put into a sealed
reactor which was kept in a vacuum oven at 90 °C
for 2 h to obtain urea-intercalated kaolin. The amount
of added urea was selected as 0 wt%, 2 wt%, 4 wt%,
6 wt%, and 8 wt% of kaolin and urea-intercalation
products were identified as KAO, KU-2, KU-4, KU-6,
KU-8, respectively.
2.3 Test methods
X-ray powder diffraction patterns were recorded
on a Brucker diffractometer (XRD, D8-FOCUS,
BrokerAXS Germany) with CuKα radiation (Kα
= 0.1541 8 nm, 0.5 °/min) between 5 and 50 °.
Semi-quantitative weight percentages of samples
were calculated by using mineral intensity factors.
The morphologies of samples were observed on
a scanning electron microscope (SEM, SU8010,
Hitachi Japan) under an acceleration voltage of 10
kV and on a transmission electron microscope (TEM,
CM12/STEM, Philips Netherlands) at a working
voltage of 120 kV. A Malvern 2000 particle size/
zeta potential analyzer (Britain) was used to analyze
both the particle size distribution (PSD) and the zeta
potential of kaolin samples. The kaolin powders were
dispersed in deionized water and stirred for 10 min
before PSD analysis. The zeta potential of the kaolin
slurries with 0.04 g/L concentration was measured
as a function of pH across the range 4-9 in deionized
water after ultrasonic vibration for 15 min. The pH of
the suspension was varied with 12 M HCl and 6.61 M
HNO3 solutions in order to avoid excessive dilution of
the samples during the experiment[7,19]. The whiteness
was determined by a WSB-2 whiteness meter (China)
according to procedures[4]. The apparent viscosity was
measured by a rotary viscometer (SNB-2, Shanghai,
China). Viscosity concentration of kaolin slurries was
calculated according to the formula mentioned in
Ref.[4].
Journal of Wuhan University of Technology-Mater. Sci. Ed. www.jwutms.net Feb.2017
3 Results and discussion
3.1 Characteration of Beihai kaolin
Raw kaolin (marked as KAO) collected from
Beihai area, occurs as granite weathered residual
deposit. The most intense reflections of the raw kaolin
mainly correspond to kaolinite (0.717 0 nm) and illite
(0.996 9 nm), as shown in Fig.1. The weak reflection
at 2θ = 8-10 ° in the raw kaolin sample was attributed
to illite impurity which possessed a calculated content
of about 3 wt% by semi-quantitative analysis. The
presence of illite impurity had a negative impact on
the application of kaolin in paper-coating and was also
indicated by the high content of K2O in the raw kaolin
(Table 1). Beihai kaolin showed a full width at half
maximum (FWHM(001)) of 0.45 ° (2θ) according to
(001) diffraction peak in Fig. 1 and an average flake
thickness along c-axis of 183 Å[7], which meant its thin
plates. Hinckley index (HI) termed by Hinckley can
represent the crystal order of kaolinite, which could
be revealed by the relative heights of X-ray reflections
peak in the region 19-22 ° (2θ). Beihai kaolin exhibited
a HI of 1.196 7, low crystallinity. The calculated I(020)/
I(1ī0) ratio of Beihai kaolin was 0.95 according to
Ref.[20], which also revealed the bad crystallographic
order of kaolinite. Low crystallinity of Beihai kaolin
sample resulted in irregular morphology and poor
viscosity concentration for paper-coating.
53
Fig.2 exhibits the morphology of Beihai kaolin
through SEM and TEM analyses. The SEM images
revealed that the particles diameter of the raw kaolin
was in the range of microns, and exhibited kaolinite
as the main mineral. The particles of Beihai kaolin
had irregular pseudo-hexagonal edge, coarse surface
and large diameter-thickness ratio (Fig.2(a)). Irregular
edge of kaolin particles indicated more breakage
bonds in the structure of kaolinite, which made Beihai
kaolin become more difficult to scatter in paper-
coating industry. TEM analysis was adopted for further
investigation of the surface morphology. Fig.2(b) shows
that Beihai kaolin particles mostly appeared as pseudo-
hexagonal shaped particles. However, there were some
defects on the surface of Beihai kaolin plates, such as
surface breakage, probably resulting from mechanical
damage or crystallographic defects. These defects
strongly affected the surface properties and viscosity of
kaolin slurry.
The physical properties of raw kaolin listed in
Table 2 display that Beihai kaolin was soft in texture
with a whiteness of 89.1% and a viscosity concentration
of 65.0% (pH = 6.24). Compared with paper-coating
grade kaolin, the viscosity concentration of Beihai
kaolin was much lower than the requirement for paper-
coating (>70.0%). So it was difficult to be directly
used in high-speed coating machine in paper industry.
Some efficient method for promoting the viscosity
concentration of Beihai kaolin was urgently needed.
3.2 Effects of pH, solid content and dis-
persant
The viscosity of kaolin slurries was affected
by lots of factors, such as particle size, particle
54 Vol.32 No.1 QIU Xiumei et al: Viscosity of Kaolin Slurries: Effects of Dispersant and ...
shape, temperature, pH value, solid content and
dispersant[10,11,21-23]. In order to improve the viscosity
concentration of Beihai kaolin, detailed research has
been carried out to investigate the effects of solid
content, pH value, and dispersant content on the
viscosity of kaolin slurries.
Fig.3 Influence of solid content and pH on the viscosity of Beihai
kaolin slurries
Different contents of kaolin powders were
dispersed in distilled water. Fig.3 reflects the influence
of solid content and pH on the viscosity of Beihai
kaolin slurries. It could be found that the dispersion
of kaolin particles was significantly affected by the
content of kaolin. Viscosity measurements made on
kaolin slurries showed that the viscosity versus solid
content was linear at low solid content, nonlinear at
intermediate and dilatant at high solid content. This
phenomenon was in agreement with Ref.[24]. The
viscosity increased slowly with increasing solid content
below 65.0 wt%, then increased rapidly. With the
increase of solid content, edge(+)/face(−) contacts was
promoted, the formation of card-house networks[21] was
facilitated and therefore the viscosity of kaolin slurries
was increased. On the basis of the results, in an effort
to make the influence of solid conten on viscosity
of kaolin slurries become minimum, 65.0 wt% was
selected as the optimal solid content for further studies.
The viscosity of kaolin slurries in distilled water
as a function of pH was also plotted in Fig.3. The
viscosity of kaolin slurries decreased with increasing
pH up to about 8.5, and then slightly increased. The
basal planes of kaolin particles were negatively
charged and were unrelated to pH value. The edge
charges created by the dissociation of silanol and
aluminol groups of kaolin changed from positive at
low pH to negative at higher pH[25]. At low pH values,
the particles in the kaolin slurry were coagulated. At
higher pH values, both the edge and basal faces were
negatively charged to form the face to face contacts
(band-like structure) with reduced viscosity of kaolin
slurries[25]. The increment of pH value could improve
the dispersion of kaolin powders through increasing the
negative charges on kaolin particles.
Fig.4 Viscosity concentrations and zeta potential of kaolin slurry
(65.0% solid content, pH = 8.5) with different content of
DC-FS dispersant
Sodium polyacrylate was a common dispersant
in paper-coating industry and used at the condition of
pH 7-9. Fig.4 shows the viscosity concentrations and
zeta potential of kaolin slurry (65.0% solid content,
pH = 8.5) with different content of DC-FS dispersant.
It was clearly seen that dispersant (DC-FS) content
had a siginificant effect on the dispersion of kaolin
powders. The viscosity concentration of kaolin slurries
increased rapidly with increasing additive amount of
DC-FS dispersant and reached a maximum (68.05%) at
a dispersant content of 4 wt‰, indicating the saturated
adsorption of carboxylic groups (-COO-) on the surface
of kaolin particles. Lots of -COO- contained in DC-
FS dispersant formed hydrogen bond with -OH on the
surface of kaolin and made kaolin particles negatively
charged. The electric double layers of kaolin expanded,
resulting in the electrostatic repulsion among kaolin
particles. The impact of DC-FS dispersant on the
surface charge of kaolin particles could be explored by
Zeta potential. Over the whole range concentration of
the dispersants, the zeta potential values were negative,
as the additive amount increasing, the zeta potential of
kaolin suspensions gradually changed much strongly
negative. This was mainly ascribed to the dispersant
which has adsorbed onto the surface of kaolin particles.
Moreover, the negative magnitude of the zeta potential
increased significantly, as the dispersants gradually
covered the surface of kaolin particles (4 wt‰), the
zeta potential reached a saturation state at last (-58
mV). It was in accord with the results of viscosity
concentration showed in Fig.4. Meanwhile, sodium
Journal of Wuhan University of Technology-Mater. Sci. Ed. www.jwutms.net Feb.2017 55

polyacrylate solvated to produce lots of short polymer urea-intercalated kaolin was higher than that of DC-FS
chains which contacted with water molecules to dispersed kaolin slurries. When urea content was more
form polymer interfaces between kaolin particles and than 6 wt%, the viscosity concentration of kaolin slurry
water moleculars. The steric hindrance made kaolin was prone to reach a plateau. In order to discuss the
slurries stably dispersed and reach a highest viscosity reason why the intercalation of urea into kaolin could
concentration of 68.05%. increase the viscosity concentration of kaolin slurries,
Based on the above results, solid content, pH, detailed studies on the morphology, particle size
as well as dispersant had complex influence on the distribution, and surface properties of urea-intercalated
viscosity (concentration) of Beihai kaolin. It certainly kaolin were investigated.
suggested that the viscosity concentration of kaolin
slurries cannot meet the requirement for paper-coating
by just changing these properties.
3.3 Effect of urea-intercalation
To obtain a high viscosity concentration of kaolin
slurry, different content of urea was intercalated into
the raw kaolin. X-ray diffraction patterns of urea-
intercalated kaolin products are shown in Fig.5. The
patterns of urea-intercalated kaolin showed a new
diffraction peak at d = 1.073 3 nm, assigning to the
intercalation of urea molecules [18]. Urea molecules
intercalated into the layer and formed hydrogen bond
with kaolinite. The intercalated ratios of samples KU-
2, KU-4, KU-6, and KU-8 were respectively 17.36%,
44.38%, 81.30% and 82.64%, which were calculated
based on the formula [26] and are listed in Table 2.
The intercalation ratio increased with increasing
urea content. The results were consistent with earlier
reported values[5].

Fig.6 shows the morphologies of raw kaolin and

The physical properties of samples KU-2, KU-
4, KU-6 and KU-8 are represented in Table 2. The
whiteness of all samples was about 89% with no
significant variations as compared with raw kaolin.
The viscosity concentration of urea-intercalated kaolin
slurries rapidly increased with increasing urea content
until urea content reached 6 wt%. For example, the
viscosity concentration increased from 65.0% of raw
kaolin to 70.13% of kaolin containing 6 wt% of urea.
It could be found that the viscosity concentration of
urea-intercalated kaolin. Compared with other samples,
KU-6 and KU-8 samples were composed of more fine-
grained particles. An obvious change in particle size
distribution of urea-intercalated kaolin could be found
in Fig.7. The average diameter of samples KAO, KU-2,
KU-6 and KU-8 were respectively 334.3, 302.5, 265.7
and 259.9 nm, which was in agreement with the results
of SEM (Fig.6). After the intercalation process, kaolin
particles were centralized and thinner and the content
of finer particles was increased. It was beneficial for the
dispersion of kaolin particles and the improvement of
viscosity concentration (Table 2).
56 Vol.32 No.1 QIU Xiumei et al: Viscosity of Kaolin Slurries: Effects of Dispersant and ...
Meanwhile, the pH of kaolin slurries changed
from acid to neutral due to the intercalation of urea
(Table 2). In addition, the zeta potential of KAO, KU-
2, KU-4, KU-6, and KU-8 were -40.5, -49.5, -54.9,
-55.7, and -56.0 mV, respectively (Table 2). The
pH value of slurries increased from 6.24 (raw kaolin
slurry) to above 7.00 (urea intercalated kaolin), which
resulted from the addition of urea. The following
reactions (1) and (2) could be identified according to
Ref.[5] when urea was dissolved in the slurries. As the
pH value of kaolin slurries was close to alkaline, kaolin
particles dispersed well, the viscosity of the slurries
became lower and the solid content of the slurries
could be improved. Kaolin particles were prone to be
delaminated with increased pH and increased solid
content.
CO(NH2)2 + H2O → (NH4)2CO3
(NH4)2CO3 + H2O → 2NH3·H2O + CO2
Based on the above analysis, the intercalation
of urea into the layers of kaolin revealed efficient
improvement in the viscosity concentration of kaolin
slurries. Urea-intercalation showed some different
dispersing functions for kaolin particles as compared
with sodium polyacrylate. A possible dispersion
mechanism of urea-intercalated kaolin slurries has been
illustrated in Fig. 8. There were three functions of urea-
intercalation on the dispersion of kaolin powders. One
was that urea molecule intercalated into the layer of
kaolinite resulting in fine particles, which was good
for dispersion of kaolin particles. Second one was that
part of urea molecules took off from the interlayer
and adsorbed on the edge of kaolin, which limited
the formation of edge(+)/face(-) contacts structure.
Therefore, kaolin particles could uniformly disperse in
deionized water to obtain high viscosity concentration.
The third one was that the dissolution of urea in water
could increase the pH and improve the negative charges
of kaolin slurries, which contributed to the dispersion
of highly concentrated kaolin. In conclusion, urea-
intercalation could improve the dispersion of highly
concentration kaolin particles to satisfy the requirement
for paper coating through creating finer particle size,
increased pH value as well as more negative charges.
4 Conclusions
In summary, the influence of solid content, pH,
DC-FS dispersant content, and urea-intercalation on the
viscosity or viscosity concentration of Beihai kaolin
have been thoroughly investigated. The viscosity of
(1)
kaolin slurries decreased with decreasing solid content,
increasing pH and dispersant content. The viscosity
(2) concentration increased from 65.0% for the raw kaolin
slurry to 68.05% for kaolin slurry with 4‰ of DC-
FS dispersant, but could not meet the requirement
for paper making industry (>70.0%). Compared with
DC-FS dispersant, urea-intercalation was proven to
be an efficient method for the dispersion of kaolin
particles. The solid content of slurries at the viscosity
of 500 mPa·s increased from 65.0% to 70.13% due to
intercalation of urea, and reached the level for paper-
coating. Urea-intercalated kaolin showed finer particle
size, higher pH value, more negative charges and
higher viscosity concentration than those of raw kaolin.
It would be interesting to perform a systemic study on
the mechanisms of stability and dispersion of urea-
intercalation in other layered clay minerals for paper-
coating.
Journal of Wuhan University of Technology-Mater. Sci. Ed. www.jwutms.net Feb.2017
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