Microcrystalline cellulose as a reinforcement

agent to cement pastes

M.S. Mohammed
Department of Chemical Engineering, National Research Centre, Cairo, Egypt
A.E.-S.I. Ahmed
Department of Chemistry, Faculty of Science, University of Zagazig, Zagazig, Egypt, and
R.M. Osman
Department of Chemical Engineering, National Research Centre, Cairo, Egypt

Abstract
Purpose – A try to find some useful applications for some products prepared from agricultural waste by mixing them with cement to act as
reinforcement agents. The paper aims to discuss these issues.
Design/methodology/approach – Cement was mixed with microcrystalline cellulosic (MCC) fibres prepared from baggase, soaked in mixing water,
followed by cubic pastes formation. The mixing was performed using different ratios of MCC; 0.5, 0.75, 1 and 3 per cent. The cement properties were
followed at timed intervals, up to 90 days. The initial and final setting times of the pastes were determined. Bulk density, apparent porosity and
compressive strength of the harden cement pastes were also identified. The hydration kinetic was followed by identifying free lime ratio and chemically
combined water content. The structure of the hard cement pastes was followed by SEM, FTIR, DSC and XRD.
Findings – It was noticed that the weight of the prepared cement pastes using MCC was reduced, while the compressive strength was increased. In
addition, lower ratios of MCC have shown better results at early ages of hydration and reported higher compressive strength than control. No
interaction was reported between the fibres and cement constituents based on the performed analysis.
Research limitations/implications – Different types of agricultural wastes can be compared in producing the best type of MCC for the same purpose
of this research.
Practical implications – This piece of work has suggested a simple way to convert a product prepared from agricultural wastes in a small uniform size
to a reinforcement agent to cement. Consuming this type of waste reduces the risks resulting from its burning at some countries such as Egypt.
Originality/value – MCC fibres have well-known binding properties and used successfully on wide range in medical applications for tablets
production with low costs. These fibres have reduced the pastes weight and increased the compressive strength using low ratios of them. Moreover,
there is no indication of a reaction between these fibres and cement constituents.

Keywords Environment, Waste, Recycling, Concrete, Waste recovery

Paper type Research paper

Introduction (Ahmed et al., 2012, 2013a, b). Between the suggested

Burning agricultural wastes such as rice straw is an issue at some
rice producing countries. The risk to human health at these
regions is very high. In spite of the existence of some suggested
applications for this waste; paper industry, charcoal production,
water treatment and animal food production, still the amount
of straw is very big (Mansour et al., 2007; Suramaythangkoor
and Gheewala, 2010; Ahmed et al., 2012, 2013a, b). This forces
the farmers to burn it which results each year in a black
cloud in the sky of some countries like Egypt which produces
a serious air pollution problem (Abou Zeid et al., 2008;
Garas et al., 2008; Ahmed et al., 2012, 2013a, b). The problem
is not only affecting population health but it affects some other
sectors, such as tourism and cultural heritage. This has drastic
effects to the economy at these third world countries
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Pigment & Resin Technology
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q Emerald Group Publishing Limited [ISSN 0369-9420]
[DOI 10.1108/PRT-05-2013-0038]
applications to recycle agricultural waste MCC was prepared
and used for some pharmaceutical applications (El-Sakhawy
and Hassan, 2007). MCC has binding properties which held the
components of the pharmaceutical tablets together upon
compressing (El-Sakhawy and Hassan, 2007; Landı́n et al.,
1993; Westermarck et al., 1999). It was prepared in an easy way
from cellulose pulps using diluted acids and present in markets
as a commercial product (El-Sakhawy and Hassan, 2007).
Using waste fibres as reinforcement agents to cement has
enormous potential in recycling materials for civil
construction. Various types of synthetic and natural fibres
have been used in cementations matrices to enhance the
mechanical properties of the composite such as tensile and
flexural strengths, toughness, impact resistance and fracture
energy (Neithalath, 2006). Cellulose-cement composites are
in use for their light weight at high fibres volume and for their
low production costs (Neithalath et al., 2004). Many authors
have demonstrated that mortar and concrete properties can
significantly be modified, at both fresh and hard states, by
polysaccharides (Ghio et al., 1994; Singh et al., 2003;
Peschard et al., 2004; Soroushian et al., 2006) or cellulose
addition (Soroushian et al., 2012).

104
 Microcrystalline cellulose
M.S. Mohammed, A.E.-S.I. Ahmed and R.M. Osman
For this reason, we have assumed in this study that using
fibres in a uniform micro size with good binding properties
may help in improving the strength and producing light
weight pastes. Moreover, fibres with this size may enables
filling the gabs between particles which produces smooth and
uniform surface for cement cubes. In addition, this study was
aiming to investigate any possible interaction between the
fibres and cement constituents.
To achieve these goals, MCC was soaked in the mixing
water of pastes preparation in different ratios. Physical and
mechanical properties of prepared pastes were studied at
timed intervals (three, seven, 28 and 90 days). The structure
and the composition of the hard cement pastes were studied
using SEM, FTIR and XRD at the same time intervals.
Experimental
Materials
Ordinary Portland cement was provided by Suez Cement
Company, Suez, Egypt. Microcrystalline cellulose (MCC)
was obtained from El-Gomhoria Chemicals Company,
Zagazig, Sharkia, Egypt.
Specimen preparation
The composition of the investigated mixtures is provided in
Table I. Cement and MCC were mixed on a roller in a
porcelain ball mill for one hour. Standard water of consistency
(ASTM designation; C191) was used in cement pastes mixing
followed by moulding the pastes in 1 inch mould to produce
cubes like samples with this diameter. The mould was kept in
desiccators saturated with water vapour (100 RH) at room
temperature (23 ^ 28C) for 24 hours. The cubes were placed
in tap water up to 90 days. At timed intervals (three, seven,
28 and 90 days), a group of stored samples was collected,
removed from water and dried at 1058C for 24 hours followed
by keeping it in desiccators for analysis.
Determination of physical and mechanical properties
The physical and mechanical properties of prepared pastes
were determined by identifying the bulk density, apparent
porosity and compressive strength (Heikal et al., 2000). Bulk
density was determined through weighing hardened paste
samples in water and air (saturated surface dry). Each
measurement was conducted in replicates (at least three
similar cubes). Bulk density was calculated using equation (1).
After the determination of bulk density (d) the samples were
placed in drier for 24 hours, cooled in desiccators and
weighed. The apparent porosity was calculated using
equation (2). Compressive strength of prepared pastes was
identified by breaking cubes of prepared samples in replicates
(three cubes per paste at each time interval).
Table I Composition of the investigated mixtures
OPC MCC
P0 100.0 0.00
P1 99.50 0.50
P2 99.25 0.75
P3 99.00 1.00
P4 97.00 3.00
105
Pigment & Resin Technology
Volume 43 · Number 2 · 2014 · 104 –110
Equation (1) calculation of bulk density:
Bulk density ðdÞ ¼ ðsaturated weight=volume of sampleÞ
ðg=cm3 Þ
While volume of sample ¼ ðsaturated weight
2 suspended weightÞ=
density of liquid ðwaterÞ
So the bulk density ðdÞ ¼ ½saturated weight=
ðsaturated weight
2 suspended weightÞ

£ 1 ðg=cm3 Þ
ð1Þ
Equation (2) calculation of apparent porosity:
Apparent porosity ¼ ½ðsaturated weight 2 dried weightÞ=
volume of sample
%
Apparent porosity ¼ ½ðsaturated weight
2 dried weightÞ=
ðsaturated weight
2 suspended weightÞ
%
ð2Þ
Kinetic of hydration
This was followed by determining the ratio of free lime and
chemically combined water content for each paste at different
time intervals. The free lime was identified using the
Egyptian specification and Hewlett method (Javellana and
Jawed, 1982; Hewlett, 2002). The chemically combined water
content was determined as explained by Heikal et al. (2000).
Analysis
Some of the hydrated cement pastes were investigated using
XRD, FTIR, DSC and SEM. X-ray fluoreF was performed
using AXIOS, WD – XRF sequential spectrometer
(PANalytical, 2005). X-ray diffraction (XRD) was performed
using BRUKER apparatus for XRD, Axs, D8-ADVANCE
(Germany 2001). FTIR analysis was recorded using KBr (2 mg
of sample/198 mg KBr) discs with Genesis-II FT-IR
spectrometer at frequencies in the range from 4,000 to
400 cm2 1. The samples were prepared using alkali halide
pressed disk technique as it gives a further reduction in
scattering (Errington, 1997). Scanning electron microscope
(SEM) was also used in investigating the microstructure of
samples surface. This was carried out by using of electron
probe micro-analyser, Japan of model JXA – 840A attached
with an EDAX unit, with accelerating voltage 30 KV,
magnification 10-400.000 £ . DSC analysis was performed at
a heating range from 308C to 6008C. Some selected samples
were investigated using a differential thermal analyser LABSYS
TG-DSC 1600 rod, SETARAM, France; with heating rate
108C/min using alumina crucible and in argon atmosphere.
Results and discussion
MCC was extracted from agricultural wastes and used
successfully in pharmaceutical tableting. It can hold the tablet
constituents together in presence of lowest possible moisture
level. The hydroxyl groups in MCC enable it to absorb water
 Microcrystalline cellulose
M.S. Mohammed, A.E.-S.I. Ahmed and R.M. Osman
and to have adhesion character. In addition, using these fibres in
such uniform low size enables the fibres to fill the gabs between
particles to some extent to produce smooth surfaces and
increase the strength. Moreover, this can help in producing light
weight cement pastes with high compressive strength.
Cement pastes were blended with MCC in different ratios;
0, 0.5, 0.75, 1 and 3 per cent, to produce paste samples P0,
P1, P2, P3 and P4, respectively. The characteristics of
blended pastes were followed at timed intervals (three, seven,
28 and 90 days) from immersing in tap water.
Initial and final setting times, as well as water of consistency,
for cement pastes are shown in Table II. The water of
consistency has increased with increasing the ratio of MCC due
to the absorption behaviour of the cellulosic material resulting
from hydroxyl groups present in its structure. This behaviour of
the fibres enhances their binding and adhesion properties which
are expecting to increase the cement strength. Also, as the
amount of MCC increases the initial and final setting times were
retarded due to the increase in water content resulting from
MCC presence. The origin of retardation could be also linked to
the adsorption of the admixture (MCC) to the first produced
hydrates forming a less permeable coat resulting in slowing
down the rate of silicate hydration. This causes a delay in the
formation of both CSH and portlandite.
The bulk density of OPC and MCC cement pastes is
graphically plotted in Figure 1. The bulk density of all cement
pastes was increased with curing time due to the precipitation
of the hydration products in the originally water filled-spaces
constituting the capillary pores of the pastes. Therefore, the
Table II Initial and final setting times as well as water of consistency for the prepared cement pastes
Sample Water of consistency, %
P0
P1
P2
P3
P4
Figure 1 Bulk density of OPC and the hydrated cement pastes
Bulk density, g/cm3
2.2
2.1
Pigment & Resin Technology
Volume 43 · Number 2 · 2014 · 104 –110
bulk density of the cement pastes has increased with
progressive hydration. It was found that the bulk density has
decreased with increasing the cellulose content; this is
attributed to the low density of MCC and also the CSH
decreasing due to the decrease of OPC.
The apparent porosity of the hydrated cement pastes has
decreased with curing time for the entire cement pastes,
Figure 2. This is due to the continuous hydration of cement
clinker and the accumulation of hydration products in the
pores of cement paste. From Figure 2 it can be seen as well
that the apparent porosity of pastes blended with MCC is
higher than that of OPC (P0) at early ages (three and seven
days) while it started to be lower at later ages. The decrease in
the apparent porosity lower than that of OPC at latter ages
(0.5-3 per cent MCC) may be attributed to the possibility that
MCC can act as active sites for CSH precipitation.
Figure 3 is representing the compressive strength of the
hardened cement pastes as a function of curing time.
The compressive strength of the hardened cement pastes
has increased with time for the entire samples; this is mainly
attributed to the increase in the amount of hydrated products,
in particular calcium silicate hydrate (tobermorite-like gel)
which is the main source of strength. It can be seen that
MCC-cement pastes with ratios from 0.5 to 0.1 per cent
MCC have shown higher percentage of compressive strength
than OPC. MCC – cement pastes prepared using 3 per cent
MCC have shown the same results at later ages.
The combined water was identified as shown in Table III.
It was noticed that in most cases that the combined water has
Setting time (min)
Initial Final
27.50 165 240
28.00 200 280
29.60 211 283
30.70 221 292
33.74 234 445
P0 P1 P2
P3 P4
10 100
Curing time, days
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M.S. Mohammed, A.E.-S.I. Ahmed and R.M. Osman Volume 43 · Number 2 · 2014 · 104 –110

Figure 2 Apparent porosity of OPC and the hydrated cement pastes Table IV Free lime content for different pastes
36 P0 P1 P2 P3 P4
34 P0 P1 P2 3 7.4 8.1 7.5 6.7 6.7
32 P3 P4 7 7.7 8.3 8.2 7.0 6.7
30 28 7.8 8.2 8.0 7.4 6.8
Apparent porosity, %

90 8.1 8.0 8.0 7.0 7.1

28
26
24 was noticed. This may be due to the adsorption of lime to
cellulose at high concentrations of it.
22
Different tools of analysis, FTIR, X-Ray, SEM and DSC were
20 used to investigate if there are any new phases have been formed
18 due to the presence of MCC. Looking into the FTIR analysis the
16 usual and expected characteristic peaks for cement pastes were
appeared at the entire time intervals with all MCC ratios. An
14
example is shown in Figure 4. There is no indication for a
12 formation of any new phases that can be seen from FTIR.
10 100 Figure 4 is showing the FTIR spectra of MCC-cement hydrated
Curing time, days pastes at 90 days, respectively. The main characteristic peaks can
be summarized as follows: the absorption band at 3,641 cm2 1
was attributed to the n1 vibrations generated by the hydroxyl
Figure 3 Compressive strength of OPC and the hydrated cement pastes group coordinated to Ca2þ in the Ca(OH)2 (Eskander et al.,
2011), while the wide band at 3,441 cm2 1 was assigned to the
900
same vibrations generated by the OH bonds in water. The
bending vibrations due to the HZOZH in water appeared at
800 1,649 cm2 1. The n3 and n2 stretching bands generated by CZO
Compressive strength, kg/cm2

in the calcite were appeared at 1,430 and 870 cm2 1, respectively,

700
(Rodrı́guez et al., 2010). The band in the region 1,000-900 cm2 1
is due to the presence of silicate group (Bensted, 1976). The main
hydration product (CSH) can be detected from the absorption
600 band at 970 cm2 1, which is assigned to the asymmetrical SiO4
stretching frequency. It indicates the polymerisation of silicate
500 units, SiO4, with the formation of CSH phase (Peschard et al.,
2004). CSH has already been formed for all cement pastes and no
P0 P1 P2 significant different at 90 days.
400 P3 P4 The XRD patterns of the hydrated cement pastes P2 and
P4 cured up to 90 days in tap water are shown in Figure 5.
300 It is clear that, no differences between OPC, P2 and P4 were
10 100 recorded. The regular peaks were recorded as expected from
Curing time, days normal OPC. Figure 6 is showing the SEM of P1 and P3.
Thin film of MCC was observed in P3 (samples prepared
using 1 per cent MCC). Performing the DSC analysis also
Table III Combined water of different pastes
P0 P1 P2 P3 P4 Figure 4 FTIR of different cement pastes hydrated at 90 days
3 13.1 11.7 08.9 10.3 12.2
7 13.7 09.7 09.3 10.4 13.5
28 14.4 11.5 10.8 11.5 15.9
90 14.8 12.9 14.9 17.1 19.3

P4
increased with time due to the increase in hydration products
P3
by hydration progress. A slight decrease for pastes with lower
ratios of MCC was recorded at early ages but at later ages
values begin to be closer to usual. At 90 days, it can be seen P2
that pastes with ratios of MCC from 0.75 to 3 per cent have P1
recorded similar or higher combined water than OPC.
Looking into the free lime identification results, Table IV,
it can be seen that the lime ratio was increased with curing
time, for OPC, due to the continuous liberation of calcium
3,500 3,000 2,500 2,000 1,500 1,000 500
hydroxide during the hydration process (Hewlett, 2002).
For the mixed pastes with MCC a slight decrease at later ages Wave number, cm–1

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 Microcrystalline cellulose Pigment & Resin Technology
M.S. Mohammed, A.E.-S.I. Ahmed and R.M. Osman Volume 43 · Number 2 · 2014 · 104 –110

Figure 5 XRD of OPC and micro cellulose cement pastes prepared using 0.75 and 1 per cent MCC hydrated at 90 days

H- Hatrurite L- larnite
P P- Portlandite C- Calcite
P H
C P
P L P
L P
P4

P2

OPC

10 20 30 40 50 60
2-Theta

Figure 6 SEM of MCC-cement pastes containing (a) 0.5 per cent and (b) 1.0 per cent MCC at different magnification values (2,000-2,500)

a_2000 b_2000

20 µm X2000 20 µm X2000

a_2500 b_2005

20 µm X2500 20 µm X2500

indicated the same results as above, no new phases have
been recorded, and the expected decomposition behaviour
was recorded for all pastes, examples are shown in Figure 7.
The previous analysis has shown that there are no new
formed phases have been recorded due to the presence
of MCC. The cement still carries its normal characteristic
features in spite of presence of MCC up to 3 per cent. In spite
of this, one can say that the compressive strength has
increased with increasing the ratio of MCC and the
weight has decreased due to the light weight of cellulosic
material. These results indicating that some products that can
be prepared from agricultural wastes can be used as

108
 Microcrystalline cellulose
M.S. Mohammed, A.E.-S.I. Ahmed and R.M. Osman
Figure 7 DSC thermogram of a) comparison between P2 and P4 at 90 days while a) and b) are representing P2 and P4, respectively, at different time
intervals
8 28 days
7 P2
6 90 days
P4
5
DSC mW
4
3
2
1
0
100 200 300 400 500 0 100
Temperature, °C
(a)
admixtures to cement bastes to increase its compressive
strength and to reduce its weight without any effect to the
composition.
Conclusion
Applying MCC as an admixture to cement pastes has
increased the water of consistency with increasing the MCC
ratio which results in retarding initial and final setting time.
Bulk density has decreased with increasing the MCC ratio
while the apparent porosity has increased at early ages. MCC
gives compressive strength higher than that of OPC using
1 per cent MCC while the same results were obtained using
3 per cent at latter ages. No new phases were detected by
MCC addition. Adding small amounts of MCC 0.5-3 per cent
gives cement with low bulk density and porosity but with high
strength (light weight high strength cement).
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Corresponding author
A.E.-S.I. Ahmed can be contacted at: a.i.ahmed@surrey.ac.uk
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