Vol. 1 (2), 2014, 28–34

Cement notation: C: CaO, S: SiO2, A, Al2O3, F: Fe2O3,
H: H2O, CH: Ca(OH)2, CSH: Cacium silicate hydrate.
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Journal of Chemistry and Materials Research
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Original Research
Utilization of Ca–Lignosulphonate Prepared From Black Liquor Waste
as a Cement Superplasticizer
H. H. M. Darweesh*
Refractories, Ceramics and Building Materials Department, National Research Centre, Dokki, Cairo, Egypt
Received 14 July 2014; received in revised form 07 August 2014; accepted 09 August 2014
Abstract
The preparation of calcium lignosulphonate (LS), its application as a superplasticizer (SP) and its influence on normal consistency, fluidity, setting
and strength development of Portland cement-silica fume pastes were investigated. Results showed that the water of consistency increases with silica
fume content, but decreases in the presence of LS. Water reduction due to superplasticizer increases with the dose. Setting times (initial and final)
elongated with LS dose up to 0.4 % and then became nearly constant. The increase of silica fume content in superplasticized mixes increases the
fluidity, especially with high SP dose (0.4 and 0.6 wt. %), and hence the gap of water reduction increases. Also, the combined water content and
compressive strength of the OPC pastes enhanced with silica fume incorporation up to 9% SF mixes after which the extra dose had no significant or
bad effect. Diffrtrntial thermal Analysis (DTA) showed that the free lime content of the LS-containing pastes decreased due to its consumption
through the pozzolanic reactivity of silica fume. Scanning electron microscopy (SEM) elucidated the well crystallized and morphological change of
the formed binder (CSH) compared with those of the control mix.
Keywords: OPC; silica fume; superplasticizer; fluidity; setting; strength; DTA; SEM.
1. Introduction
Superplasticizers are admixtures added to cement or
concrete during mixing with water to increase the flowing
characteristics of the paste. These admixtures have the ability
to increase the workability and reduce the amount of mixing
water during the preparation of cement pastes or concrete [1–
9]. Lignosulphonates, a byproduct of the pulp and paper
industry that could be obtained from the spent sulfite pulping
liquors, are the most available which has excellent dispersing
properties and are utilized as superplasticizers in concrete,
cement and gypsum pastes to maintain adequate fluidity.
Jumadurdiyev et al. [10] prepared the Ca-lignosulphonate
from molasses, a byproduct of sugar industry, to use as a
retarding and water-reducing admixture for concrete.
Lignosulphonates are anionic surfactants which are excellent
water-reducing agents in concrete construction. The
lignosulphonates are relatively inexpensive and their water
reducing properties could be exploited at minimal cost.

* Corresponding author.
E-mail address: hassandarweesh2000@yahoo.com (H H M. Darweesh).
All rights reserved. No part of contents of this paper may be reproduced or
transmitted in any form or by any means without the written permission of ORIC
Publications, www.oricpub.com.
However, the variance in their composition, especially their
sugar content, could induce significant problems in set
retardation and air entrainment [10,11].
There is an interaction of the plasticizing additives of
concrete mixtures due to their effective components with the
surface of solid particles of the suspension, especially with
that of cement [1,3]. As a result, there is a considerable
influence on the rheological properties of suspensions, the
hydration kinetics and the formation of solid structure of the
cement binder. The nature and mechanism of action of
plasticizing additives have not yet been explained in a
satisfactory way [5,11]. The use of the various plasticizing
admixtures or water-soluble polymer modified systems as
dispersing agents for improving and modifying the
workability of cement pastes or concrete as well as for their
plasticizing and air-entraining effects at a considerably low
polymer: cement ratios, however, these admixtures enhance
the performance of concrete mixtures [1,6].

Table 1 Chemical composition of the Raw Materials, wt. %.
Oxides
Materials
L.O.I SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2
O
SO3 Blaine S.
Area,cm2/g
OPC 2.64 20.12 5.25 3.38 63.13 1.53 0.55 0.3 2.54 3400
SF 1.22 94.82 0.55 2.12 – – 0.07 0.4
9
0.7 21000
36 F. Author et al. / Journal of Chemistry and Materials Research xxx (2014) xxx–xxx
Accordingly, the main objective of the present study is the
preparation of Ca-lignosulphonate from the black liquor
waste of pulp and paper industry to study the effect of the
prepared Ca-lignosulphonate on the setting, fluidity and
mechanical properties of blended cement pastes containing
different ratios of silica fume.
O(H)
CH-OH
CH-O-
CH2-OH
OCH3
Fig. 1. Chemical Formula of Lignin.
OCH3
CH-OH
OH
Lignin
SO3
--
CH-SO3
OCH3
OH
Lignin
Fig. 2. Sulphonation of Lignin by sulphite process to form Lignosul-
phonate.
2. Experimental and methods
2.1.Raw materials
The raw materials used in the present study are Ordinary
Portland cement (OPC), Silica fume (SF) and Ca–
lignosulphonate (LS). The OPC sample with a Blaine surface
area of 3300 cm2
/g is delivered from the Suez Portland
Cement Company, Egypt. While, the SF sample with a
surface area of 21 m2
/g was provided by Ferrosilicon alloys
Company, Edfo, Upper Egypt. The Ca–lignosulphonate
sample was prepared and isolated from the black liquor waste
of paper industry. The chemical analysis of OPC and SF is
shown in Table 1. The mineralogical composition of the OPC
sample was C3S, 55.10 %, β-C2S, 16.72 %, C3A, 6.43 % and
C4AF, 12.08 % as calculated from Bogue's equations [12].
2.2.Preparation of Ca-lignosulphonate
Ca-lignosulphonatewas isolated from the black liquor of
sulfite pulping as follows: The pulp was filtered off from the
cooking liquor of the sulfite cooking of paper industry waste
by using 25 % calcium sulphide (CaS) at 170 ºC for 1.5 hour.
The black liquor was evaporated on water bath and then dried
in a vacuum oven at 80 ºC for 8 hours.
The used Ca-lignosulphonate was composed of 20%
Na2SO3, 58.2 % consumed sulfite, 41.91% solid content
[13], viscosity [14], η 1.91, 8.8% sulpher, 94.32 yeild %, pH
value 6.66 [15]. The introduction of sulphonate groups occurs
mainly in the side chain of the phenolic rings of the lignin
[10] which could be represented in Figs. 1 and 2, respectively.

Table 2 The cement mixes of the raw materials, wt. %.
Mixes
Materials
M0 M1 M2 M3 M4 M5 M6
OPC 100 97 94 91 88 85 80
SF 0 3 6 9 12 15 20
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of paper
industry.
The chemical analysis of OPC and SF is shown in Table 1.
The mineralogical composition of the OPC sample was C3S,
55.10 %, β-C2S, 16.72 %, C3A, 6.43 % and C4AF, 12.08 % as
calculated from Bogue's equations [12].
2.2.Preparation of Ca-lignosulphonate
Ca-lignosulphonatewas isolated from the black liquor of
sulfite pulping as follows: The pulp was filtered off from the
cooking liquor of the sulfite cooking of paper industry waste
by using 25 % calcium sulphide (CaS) at 170 ºC for 1.5 hour.
The black liquor was evaporated on water bath and then dried
in a vacuum oven at 80 ºC for 8 hours.
The used Ca-lignosulphonate was composed of 20%
Na2SO3, 58.2 % consumed sulfite, 41.91% solid content
[13], viscosity [14], η 1.91, 8.8% sulpher, 94.32 yeild %, pH
value 6.66 [15]. The introduction of sulphonate groups occurs
mainly in the side chain of the phenolic rings of the lignin
[10] which could be represented in Figs. 1 and 2, respectively.
2.3.Cement batches and methods
Seven cement batches were studied in the present work
denoting the symbols: M0, M1, M2, M3, M4, M5 and M6.
Compositions of the different cement batches are shown in
Table 2. Batches were mechanically blended in a porcelain
ball mill (Lab. monomill, Pulverisette 6– FRITSCH,
Germany) for one hour using 3 balls to assure the complete
homogeneity. The Ca-lignosulphonate dissolved in the
mixing water was added to the cement mixes M0-M6 with
the dosage of 0.0, 0.1, 0.2, 0.3, 0.4, 0.5 and 0.6 wt. % of the
cement. The fluidity of superplasticized mixes was
determined by mini-slump test [16]. The superplasticized
mixes were stirred with water by a glass rode for 30 min.,
then re-mixed for one minute using mechanical mixer before
the cone filling and the pat area was measured. The standard
water of consistency as well as setting time of the prepared
cement pastes were directly determined by Vicat apparatus
[17,18]. The cement pastes were mixed and moulded into one
inch cubic stainless steel moulds (2.5 x 2.5 x 2.5 cm3
),
vibrated manually for two minutes and on a mechanical
vibrator for another two minutes. The moulds were stored
inside a humidity cabinet for 24 hours at 23 ±1 ºC and 100 %
R.H., then demoulded and cured under water till the time of
testing for compressive strength after 1, 3 , 7 , 28 and 90
days. The compressive strength [19] was carried out using a
hydraulic testing machine of the Type LPM 600 M1
SEIDNER (Germany) having a full capacity of 600 KN. The
loading was applied perpendicular to the direction of the
upper surface of the cubes. The compressive strength was
calculated from the equation:
a
S
S
KNL
C
)(
=
(1)
where, Cs is the compressive strength (MPa), L is the load
(KN) and Sa is the surface area (cm2
).
The combined water content (Wn) of the hydrated
samples predried at 105 ºC for 24 hours was determined on
the bases of ignition loss at 1000 ºC for 30 minutes from the
equation:
100
)(
2
21
×
−
=
W
WW
Wn
(2)
where Wn, W1 and W2 are combined water content, weight of
sample before and after ignition, respectively.
The phase compositions of some selected samples were
investigated using infrared spectroscopy (IR), differential
thermal analysis (DTA) and scanning electron microscopy
(SEM) techniques. The IR analysis was carried out using a
Perkin Elmer FT-IR spectrometer in the range of 4000 – 400
cm–1
. DTA analysis was performed by the DTA-50 WSI-
Shimadzu Differential thermal analyzer at a heating rate 20
ºC/min. up to 1000 ºC. The SEM images were obtained by
JEOL–JXA–840 electron analyzer at accelerating voltage of
30 KV. The fractured surfaces were fixed on Cu–stubs by
carbon paste and then coated with a thin layer of gold.
Fig. 3. The IR spectra of the prepared Ca-lignosulphonate.
3. Results and discussion

3.1.Infra Red spectra of lignosulphonate
Fig. 3 shows the infra red spectra (IR) of Ca–
lignosulphon-ate. The absorption band at 3450–3420 cm–1
is
due to the hydroxyl groups of lignin. The broadening of bands
reveals that the OH group is not free but entering into
different modes of hydrogen bonding. The shift of O–H band
of lignin to lower frequency 3406 cm–1
after sulfonation
indicated that the hydro-gen bonds of hydroxyl group are
stronger. Absorption bands at 2937 cm–1
are related to – CH3
and – CH2. No bands at 1765 cm–1
indicating the C=O group
therefore the principle change that occurred during
sulfonation is in the C=O region. The presence of absorption
bands in the region 1600–1500 cm–1
confirmed the aromatic
structure of lignosulphonate, while the absorption at 1465 cm–
1
is attributed to aromatic C–H deform-ation in methyl or
methylene groups, which are considerably affected by
methoxyl (– OCH3) groups. The absorption band at 1425 cm–
1
is due to aromatic skeletal vibration that strongly coupled by
C–H in plane deformation. However, the band in the region
of 1420–1430 cm–1
is due to C–H related to bands of
methoxyl groups. The absorption band at 1212 cm–1
is due to
guaiacyl units. The absorption band at 1035–1025 cm–1
is
assigned to aromatic C–H out-plane deformation. The absorp-
tion at 1030 cm–1
is assigned to aromatic C–H in-plane defor-
mation. The disapprearrance of the band at 825 cm–1
indicates
the presence of guaiacyl units in lignosulphonate. The absorp-
tion band at 650–550 cm–1
is due to C–S stretching [10,20].
Fig. 4-Effect of lignosulfonate dose on the
w orkability of cement pastes mixed with SF.
120
140
160
180
200
220
240
260
0 0.2 0.4 0.6 0.8
Dose, w t.%
Patarea,cm2
M1 (w /s= 0.50) M2 (w /s=0.55
M3 (w /s= 0.60) M4(w /s= 0.65)
Fig. 4. Effect of lignosulfonate dose on the workability of cement
pastes mixed with SF.
3.2.Mini-slump Test
Fluidity of the cement paste of different batches was deter-
mined through the mini–slump test. Fig. 4 shows the effect of
lignosulphonate polymer addition at 0.2, 0.4, and 0.6 wt. %
on the workability of cement pastes with different ratios of
silica fume (SF): (3, 6, 9 and 12 wt. %). It is clear that the
workabi-lity improved with lignosulphonate addition up to
0.4 % and any further addition had no significant effect on
the workabi-lity.
Fig. 5 illustrates the water reduction percent of
superplasti-cizer dose which calculated by the comparison of
pat area of the used SP dose with that of a pate area of the
blank batches with different water/solid ratios. The water
reduction increased with the dose of SP. The increase of silica
fume content in superplasticized mixes tends to increase the
fluidity of mixes especially with high SP dose (0.4 and 0.6 wt.
%). This is mainly due to that the higher amount of
lignosulfonate has adverse effect on the specific properties of
cement pastes, particularly workability or fluidity. Therefore,
the water redu-ction is increased and the optimum dose of
superplasticizer considered being 0.4 % and the optimum
batch is M3.
3.3.Water of consistency
Water of consistency of the OPC (M0) and the various
ble-nded cement pastes (M1–M6) mixed with different ratios
of lignosulphonate is represented in Fig. 6. It is clear that the
wat-er of consistency increases gradually with SF content.
This is mainly due to the high surface area of SF [1,2,12,21].
Moreo-ver, the water of consistency was gradually decreased
with the lignosulphonate ratio up to 0.4 %. This is due to that
the lingo-sulphonate is a water-reducing agent. With
lignosulphonate ratio > 0.4 %, the water of consistency tends
to be constant. This is due to that the particles of
lignosulphonate adsorbed at the surfaces of SF and OPC
grains preventing their influence and also hinder the
hydration of the cement [12,21].

Fig. 7-Initial and final setting times of
cement pastes premixed with
lignosulfonate.
100
120
140
160
180
200
220
240
260
280
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8
Polym er dose, %
Settingtime,min.
M0 M1
M2 M3
M4 M5
M6
F.S.T
I.S.T
Fig. 7. Initial and final setting times of cement pastes premixed
with lignosulphonate.
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Fig. 5-Water reduction of specified polymer
dose of cement pastes mixed with SF.
15
20
25
30
35
40
0.2 0.4 0.6
Dose, wt.%
Waterreduction,%
M1 M2 M3 M4
Fig. 5. Water reduction of specified polymer dose of cement pastes
mixed with SF.
Fig. 6-Water of consistency of cement
pastes prem ixed w ith variable ratios of
lignosulfonate.
20
24
28
32
36
40
0 0.1 0.2 0.3 0.4 0.5 0.6
Lignosulfonate contents, %
Waterofconsistency,%
M0 M1 M2 M3
M4 M5 M6
Fig. 6. Water of consistency of cement pastes premixed with
variable ratios of lignosulphonate.
3.4.Setting times
The initial and final setting times of the OPC (M0) and
the various blended cement pastes (M1–M6) premixed with
differ-ent dosages of lignosulphonate are given in Fig. 7. It is
clear that the setting times (initial and final) increased
slightly with the SF content as well as the lignosulphonate
dose. The elong-ation of setting times continued with up to
0.4 % LS polymer dose and then become nearly constant.
This means that the setting times delayed with
superplasticizer and/or silica fume addition. The retention of
hydration progress can be explained that the formed
hydration products were adsorbed on the non-hydrated
cement grains reducing the hydration rate. The ligno-
sulphonate was adsorbed on cement grains through the Ca+2
bridging which reduce the calcium ion percentage in solution.
This removal of Ca ions will prevent them from entering into
setting and hydrating reaction of cement systems which
results in retarding the hydration [22]. Also, active silica
fume partic-les reacted with the produced calcium hydroxide
from hydra-tion reaction to form additional hydration
products. These hyd-ration products reduce hydration
progress by forming adsorbed thin layers on the cement
grains. Consequently, M3 could be selected to be the
optimum batch and 0.4 % of the lignosulph-onate as the
optimum dose under the experimental conditions used in this
investigation.
3.5.Combined water contents

Fig. 8-Com bined w ater contents of cement
pastes premixed w ith 0.4 % lignosulfonate
cured up to 90 days.
14
16
18
20
1 3 7 28 90
Curing tim e, days
Combinedwatercontents,%
M0 M1 M2 M3
M4 M5 M6
Fig. 8. Combiened water contents of cement pastes premixed
with 0.4 % lignosulphonate cured up to 90 days.
Fig. 9-Compressive strength of cement
pastes premixed w ith 0.4 %
lignosulfonate cured up to 90 days.
20
30
40
50
60
70
80
1 3 7 28 90
Curing time, days
Compressivestrength,MPa
M0 M1 M2 M3
M4 M5 M6
Fig. 9. Compressive strength of cement pastes premixed with 0.4
The combined water contents of the various blended
cement pastes (M0–M6) premixed with the optimum dose of
lignosulphonate (0.4 %) are represented as a function of
curing time up to 90 days in Fig. 8. Generally, the combined
water content of the various cement pastes increased
gradually with curing time. This is mainly attributed to the
continuous form-ation of hydration products from the
chemical reactions betw-een the different phases of OPC with
water to form C–S–H and sulphoaluminate hydrates. This is
often responsible for the increase of combined water contents
[11,15]. Furthermore, the SF can react also with the released
Ca (OH)2 during the hydr-ation of C3S and β–C2S to form
additional hydration products as CSH and calcium
aluminosilicate hydrates. This causes further increase in the
combined water contents of cement pastes [5,23]. The
combined water content of all cement pastes tends to decrease
with SF content of more than 9 % due to the higher amount
of mixing water used for the preparation of the pastes. The
results suggest that M3 achieved the highest comb-ined water
contents among other mixes.
3.6.Compressive strength
The compressive strength of the hardened pastes of the
various blended cement mixes (M0–M6) in the presence of
the optimum dose of lignosulphonate (0.4 %) are graphically
plotted as a function of curing time up to 90 days and given
in Fig. 9. It is clear that as the curing time prolonged, the
compr-essive strength gradually increases with a sharp
increase in the compressive strength during the early ages of
hydration (1–28 days). This is mainly due to the continual
deposition of the formed hydration products into the pore
structure of the hardened cement pastes. This occurred at a
higher rate during the early ages. Hence, the total porosity
decreases while the bulk density increases. This is
accompanied with an increase in the compressive strength
[15,24]. The strength of the blended cement pastes (M1–M6)
premixed with 0.4 % lignosulphonate increased with SF
content up to 9 % and then decreased. This is mainly
attributed to that the lignosulphonate activates the different
phases of the OPC and the hydration reaction of SF with the
released Ca(OH)2 which positively affected the mechanical
strength. Also, the good dispersion caused by the
lignosulphonate admixture and the good compaction during
moulding improve and enhance the compressive strength.
The decrease of compressive strength observed with higher
amounts of SF is mainly due to the dilution effect resulting of
replacement of higher amounts of the cementing material
with SF. Furthermore, the higher amounts of SF largely
increased the mixing water which negatively affected the
mechanical strength and also decreased the activation effect
of the lignosulphonate.
3.7.Differential Thermal Analysis
The differential thermal analysis (DTA) of cement pastes
of M0 as well as of M2, M4 and M6 premixed with
superplast-icizer is shown in Fig. 10. The endothermic peaks
at the temperature ranges 106 –110 ºC and 475 –490ºC are
mainly due to the dehydration of CSH and the decomposition
of free calcium hydroxide, respectively. The broad
endothermic peak at the temperature range 730 –750 °C is
essentially due to the carbonation of CSH formed during the
handling of samples. The exothermic peak at about 900ºC is
attributed to the transf-ormation of CSH to β–CS (para
wollastonite) [24,25].

M0 M2
M4 M6
Fig. 11. The SEM micrographs of the OPC (M0) and M2, M4 and M6
pastes hydrated up to 90 days.
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Fig. 10. DTA analysis of M0, M2, M4 and M6 cement pastes
premixed with superplasticizer.
It is clear that the intensity of the characterized peak of
free lime decreased gradually with SF addition (M2 and M4),
but tends to increase slightly with higher ratio of SF (M6).
The in-creased intensity of dehydrated CSH peak and the
decrease of the free calcium hydroxide (CH) are attributed to
the normal hydration of cement phases and to the pozzolanic
reactivity of SF which reacts with CH forming CSH, in
addition to the acti-vation and dispersing effects of the
lignosulphonate to the cement mixes.
3.8.Scanning Electron Microscopy
The scanning electron microscopy (SEM) of M0, M2, M4
and M6 mixed with 0.4 wt. % of lignosulphonate
superplastic-izer were investigated through the scanning
electron microsc-opy (SEM) as shown in Fig. 11. The results
indicated the morphology change of binder (CSH) from blank
and other mixes that contained variable amounts of silica
fume. The M2 photo showed more dense structure than that
of the blank. Also, the binder in photo M4 is more amorphous
than in blank. The M4 photo shows more elongated and
fibrous structure (less amorphous) which was reflected on the
strength develop-ment of the samples. The M6 photo showed
more porous and higher crystalline binder. So, the strength
was largely decrea-sed compared with other blended cement
mixes.
4. CONCLUSION
The addition of silica fume to Portland cement pastes
incr-eases the water of consistency and elongated the setting
times (initial and final) due to its high surface area. With the

incorp-oration of lignosulphonate (LS) admixture, the W/C
ratio decr-eases with its dose while setting times (initial and
final) increa-sed up to 0.4 % beyond which no significant
effect has been observed. Also, the increase of silica fume
content in superpla-sticized-mixes increases the fluidity of
cement pastes, especially with high SP dose (0.4 and 0.6 wt.
%) and therefore the magnitude of water reduction increases.
Hence, the lignos-ulphonate admixture has a synergetic
effect. It acts as a high range water reducer and a set-retarder.
The chemical combined water as well as compressive strength
increased with SP up to 0.4 % and then decreased slightly. It
can be concluded that, the compressive strength of the OPC
pastes is improved and enhanced with SP incorporation. The
DTA showed that the free lime content of the LS–containing
pastes was slightly decreased due to the pozzolanic reactivity
of silica fume to react with Ca (OH)2. At 20 % SF, although
the particles of LS adsorbed on the surfaces of OPC grains
and temporary prevents its hydration, the Ca(OH)2 decreased
further. The SEM investigation manifested the morphological
change of the formed C–S–H having a higher degree of
crystallinty compa-red with those of the control mix.
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