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Evaluation of Boron Containing Clay Wastes in Cement

Production
a b
M. Özdemir & A. Uǧurlu
a
Department of Chemical Engineering , Eskişehir Osmangazi University , Eskişehir, Turkey
b
DSİ Technical Research and Quality Control Department , Ankara, Turkey
Accepted author version posted online: 24 May 2011.Published online: 08 Apr 2011.

To cite this article: M. Özdemir & A. Uǧurlu (2011) Evaluation of Boron Containing Clay Wastes in Cement Production,
Materials and Manufacturing Processes, 26:9, 1130-1135, DOI: 10.1080/10426914.2010.536928

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 Materials and Manufacturing Processes, 26: 1130–1135, 2011
Copyright © Taylor & Francis Group, LLC
ISSN: 1042-6914 print/1532-2475 online
DOI: 10.1080/10426914.2010.536928

Evaluation of Boron Containing Clay Wastes in Cement Production

M. Özdemir1 and A. Uǧurlu2
1
Department of Chemical Engineering, Eskişehir Osmangazi University, Eskişehir, Turkey
2
DSİ Technical Research and Quality Control Department, Ankara, Turkey

The evaluation of clay wastes (CW) containing boron additives in mortar are reported in this study. CW grounds were added to ordinary
Portland Cement (OPC) with different proportions (0%–20%). The effects of CW on the mechanical properties of mortar were analyzed by fresh
and hardened concrete tests. The obtained results were compared with those of control samples and Turkish Standards (TS). The results showed
that strength values of all specimens containing 1.5% of CW were higher than that of the control sample. With the replacement of 2.5–5.0% of
OPC by CW, the strength values were nearly equal to that of control sample. The durability of CW added cement was also examined with the
measurements of the weight losses of samples exposed to NaCl solution and MgSO4 solution. The CW affected the durability negatively in a
low level.
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Keywords Boron; Cement; Durability; Evaluation; Strength; Waste.

Introduction ratio, is an economical loss. The utilization of various

Turkey has 803 million tons of boron reserves, which
consist of 63% of the total world boron reserves. The
most important boron ores in Turkey are colemanite,
ulexite, and tincal. Products obtained from the ores are
concentrated tincal, borax pentahydrate, borax decahydrate,
anhydrous borax, boric acid, and sodium perborate. Turkey
is the second producer following the United States
with 1.72 million tons of boron minerals production
per year. In Etibank Kırka Borax Plants, 800,000
tons/year of concentrated tincal, 160,000 tons/year of borax
pentahydrate, 60,000 tons/year of anhydrous borax, and
17,000 tons/year of borax decahydrate are obtained from
tincal [1]. Every year, 120,000 tons clay wastes (CW),
known as the first clay waste (CW1), and the second clay
waste (CW2), are formed in the concentrated tincal unit
and the borax pentahydrate unit during the production. In
the concentrated tincal unit, natural tincal is beneficiated
by crushing, screening, and scrubbing. The produced
concentrate tincal contains % 34–35 B2 O3 and its particle
size is about 6 mm. Before scrubbing, the crushed tincal ore
is sieved using a sieve with 6 mm size, and the remaining
part on the sieve is called as CW1. In the borax pentahydrate
unit, the concentrate tincal is charged to a stirred reactor.
Boron from the concentrate tincal is extracted with water
at 95–100
C. The extraction solution is passed from a
sieve and the undissolved part having smaller than 6 mm
particle size (CW2) is taken above this sieve. CW containing
about 9–20% B2 O3 are discharged to the plant area, and
simply accumulated in there. Boron compounds cause
some environmental problems. Furthermore, the disability
of utilizing these wastes, containing B2 O3 , in a quite high
Received July 28, 2010; Accepted October 19, 2010
Address correspondence to Mine Özdemir, Department of Chemical
Engineering, Eskişehir Osmangazi University, Eskişehir 26480, Turkey;
E-mail: mnozdemi@ogu.edu.tr
1130
industrial wastes is important to saving the environment
from degradation.
Cement is made essentially from a calcareous material
and from alumina and silica. It is produced by grinding
the raw materials, mixing them in certain proportions,
and burning in a rotary kiln at a temperature of
up to about 1450
C when the material sinters and
partially fuses into balls known as clinker. Clinker is
mainly composed of tricalcium silicate (3CaO · SiO2
C3 S)),
dicalcium silicate (2CaO · SiO2
C2 S)), tricalcium aluminate
(3CaO · Al2 O3
C3 A), and tetracalcium aluminoferrite
(4CaO · Al2 O3 · Fe2 O3
C4 AF). In addition, there exist
minor compounds such as MgO, K2 O Na2 O TiO2 , and
Mn2 O3 . The resulting product, Portland cement is produced
by adding gypsum to the clinker in the ratio of 3–5% and
then grinding the obtained mixture. Cement production is
one of the most energy intensive ones in mineral processing
industries. The energy consumption of a dry process cement
plant is 700–900 kcal/kg of clinker [2]. The burning process
provides 40 to 60% of the production cost. The cement
plants also emit large volumes of dust and CO2 during the
process. It is necessary to add various mineral additives
such as natural or industrial wastes to the clinker to reduce
the cost of cement production and the polluting effects of
cement process [3, 4]. Thus, the addition of CW will reduce
both energy cost and CO2 emission and will contribute to
the production of an environmentally friendly cement.
The use of wastes containing boron as additives in
the production of cement, mortar, and concrete were
examined in the studies reported in the recent literature.
In these studies, boric acid wastes including reactor waste,
borogypsum, and sludges as well as colemanite concentrator
wastes, tincal concentrator wastes, and borax pentahydrate
wastes were added to Portland and trass cements, clinker,
and concrete in various ratios. In addition, the effects
of wastes on the physical and mechanical properties of
cement were also investigated [5–8]. In the present study,
 EVALUATION OF BORON CONTAINING CLAY WASTES 1131

the effects of NaCl and MgSO4 on the durability of Table 2.—Properties of OPC.
cement, containing boron, were investigated as an original
Chemical
contribution to the previous literature. Furthermore, the
analysis and Physical and mechanical
ultrasonic pulse transmitting time of the mortar containing properties Weight (%, w/w) properties
boron was measured. The principal aim of the present study
is to investigate the use of CW (CW1, CW2), containing CaO 6317 Specific gravity 3.08
boron as a cement additive in mortar. For this purpose, MgO 125 Blaine (cm2 /g) 3450
SiO2 2124 Compressive strength (MPa)
cement samples were produced by adding CW1 and CW2 to Al2 O3 496 2 days 20.2
ordinary Portland cement (OPC) at the various proportions Fe2 O3 316 7 days 38.2
(0%, 1.0%, 1.5%, 2.5%, 5.0%, 7.5%, 10%, 15%, and Na2 O 006 28 days 49.0
20%). The effects of CW on the mechanical properties K2 O 050 Flexural strength (MPa)
SO3 235 2 days 1.9
of mortar were evaluated by conducting the following Cl− 0002 7 days 3.5
tests: compressive strength, flexural strength, ultrasonic Ignition loss 220 28 days 6.5
pulse transmitting time, setting time, volume change, and Initial setting time (h min) 2. 30
durability. Insoluble residue 110 Final setting time (h min) 3.25
Volume expansion (mm) 3
Experimental study
Materials
Method
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In this study, CW (CW1, CW2) were obtained from

Etibank Kırka Borax Plant, while OPC was provided from In the experiments, a three-cell mold in the dimensions
Eskişehir Cement Plant in Eskişehir, Turkey. Initially, of 40 × 40 × 160 mm was used. Cement, waste, sand,
CW was dried in the air and then dried in the oven at and water were well mixed, and the obtained mortar was
60
C for 1 hour. Subsequently, they were ground and compressed according to the standards, then put into the
sieved through 0.0125 mm. Some physical and chemical molds and vibrated by an external vibrator. After the top
features of CW and OPC used in the research are given surface of the mold was smoothened by a steel plate, the
in Tables 1 and 2. An X-ray diffractogram (XRD) of the mortar samples were left for 24 h for the first hydration
CW were obtained by an X-ray diffractomer (Philips PW under 20 ± 1
C and 90% water saturated air. Subsequently,
1830) using CuK radiation. It was seen that the CW1 the demolded mortar samples were left in lime-saturated
consisted mainly of dolomite (CaMg
CO3 2 ), amorphous water for 28 days. After these treatments, mortar samples
matter (SiO2 ), calcite (CaCO3 ), feldspar (NaAlSi3 O8 ), and were dried and tested by applying the hardened concrete
charlesite (Ca6 Al15 Si05
SO4 2 B
OH12 O4 · 26
H2 O); and test methods.
CW2 consisted mainly of dolomite, amorphous matter, The compressive strength and flexural strength were
calcite, and feldspar. The CW1 and CW2 have a slight determined according to TS 24. The setting time and volume
pozzolanic character due to their slightly amorphous change tests were performed using a Vicat apparatus and Le
structures and low SiO2  Al2 O3 , and Fe2 O3 contents. Chatelier apparatus, respectively, as described in TS 24 [9].
The CW1 and CW2 were added to cement in the ratios The obtained values were compared with control samples
of 0%,1.0%, 1.5%, 2.5%, 5.0%, 7.5%, 10%, 15%, and 20% according to TS 19 [10]. The ultrasonic pulse transmitting
(w/w), separately. Each of the prepared cement samples time was measured by a Pundit apparatus, which employs a
was taken in the amount of 450 g and mixed with 1350 g digital read-out of the time for the pulse to travel a measured
of Rilem Cembureau standard sand and 225 ml of water distance, according to ASTM C 597-09 [11]. Furthermore,
according to TS 24 [9]. The samples without CW were durability tests were applied to the mortar samples cured
prepared as control samples. for 28 days by using NaCl and MgSO4 solutions. The
weight losses of samples were measured after they were
immersed in the solutions containing 40 g NaCl/L and 40 g
Table 1.—Chemical and physical properties of CW1 and CW2. MgSO4 /L for 60 days, separately. These solutions were
Component CW1 (%, w/w) CW2 (%, w/w) changed with fresh solutions every two weeks, and thus their
concentrations were kept constant. All tests were maintained
B2 O3 19.78 9.63 at a controlled laboratory temperature of 20 ± 1
C. The
CaO 15.86 20.24
MgO 14.26 17.31 results given are the average of three values.
SiO2 15.47 12.09
Na2 O 6.13 5.60 Results and discussion
Al2 O3 2.05 1.35
Fe2 O3 1.72 1.44 Cement samples were initially obtained by adding CW
K2 O 1.36 1.04 to OPC at various ratios. In order to determine the effects
Loss on ignition 23.37 31.3
Specific gravity 2.24 2.08
of CW on the mechanical properties of the mortar samples
Blaine (cm2 /g) 2820 2830 prepared with these cements, the tests such as compressive
Initial setting time 28 h 15 min 21 h 3 min strength, flexural strength, ultrasonic pulse transmitting
Final setting time 116 h 3 min 93 h 17 min time, setting time, volume change, and durability tests were
Residue on 200 m (%) 0.9 0.8 applied. These results are given in Tables 3 and 4 and
Residue on 90 m (%) 11.3 10.3
Figs. 1–5.
 1132 M. ÖZDEMİR AND A. UǦURLU

Table 3.—The results of compressive and flexural strength tests for mortar
mixtures.

Compressive Flexural
strength (MPa) strength (MPa)
Code CW (%, w/w) CW1 CW2 CW1 CW2

CW0 0.0 52 52 7.2 7.2

CW1 1.0 56 53 8.1 7.8
CW15 1.5 57 54 8.4 8.0
CW25 2.5 51 53 7.2 7.9
CW5 5.0 50 52 7.0 7.3
CW75 7.5 39 46 6.4 6.9
CW10 10 21 38 4.4 6.4
CW15 15 17 36 2.1 5.7
CW20 20 14 30 – 4.6

Table 4.—The results of setting time and volume expansion for mortar
mixtures.
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Volume
Setting time (h min) expansion (mm)

Code CW (%, w/w) CW1 CW2 CW1 CW2 Figure 2.—Variation of flexural strength of mortar with CW.

initial final initial final

CW0 0.0 2.30 3.25 2.30 3.25 3 3

CW1 1.0 3.10 4.30 2.40 3.05 3 3
CW15 1.5 3.14 4.40 2.50 3.25 3 3
CW25 2.5 3.20 4.55 3.05 3.44 4 3
CW5 5.0 3.25 4.59 3.18 3.55 4 3
CW75 7.5 3.30 5.05 3.25 4.00 4 3
CW10 10 3.40 5.19 3.35 4.15 4 3
CW15 15 4.00 5.25 3.40 4.30 3 2
CW20 20 4.15 5.40 3.55 4.55 2 2

Figure 3.—Variation of ultrasonic pulse transmitting time of mortar with CW.

mortar of cement obtained by adding CW1 up to 1.5% and

Figure 1.—Variation of compressive strength of mortar with CW.
Compressive Strength
The compressive strength values of mortar samples at 28
days are given in Table 3 and Fig. 1. It is observed that the
CW2 up to 5.0% to OPC had higher compressive strength
than that of control sample. In the case of higher ratios, the
mortar had lower compressive strength with respect to the
control sample. This is the result of the small pozzolanic
contribution of CW due to the lower total SiO2  Al2 O3 , and
Fe2 O3 contents than 70%, which is the value given in ASTM
C 618 [12]. This also results from the mortar’s lower cement
content. As seen from the results, it is possible for CW1
to be used in 2.5% ratio since the result obtained from this
additive quantity is nearly equal to that of control sample. It
is suitable to increase this ratio up to 5% by using CW2 with
a lower boron content. The loss encountered in compressive
 EVALUATION OF BORON CONTAINING CLAY WASTES
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Figure 4.—Variation of weight loss mortar with CW.
Figure 5.—Variation of weight loss mortar with CW.
strength by increasing CW1 ratio is higher than that in the
case of increasing the CW2. This result indicates that the
increase in the amount of boron contained in CW affected
the strength negatively [5, 8]. This may be explained by the
reduction in the pozzolanic activity of CW with increasing
boron content. The C3 S and C2 S react with water in cement
to form a calcium silicate hydrate (C− S− H) by releasing
lime as Ca
OH2 . These are the two principal solid phases
in the hydrated cement paste. The C− S− H occupies 50
to 60% of the volume of solids in completely hydrated
Portland cement paste. The Ca
OH2 constitutes 20 to 25%
of the solid volume in the hydrated paste. The strength-
contributing potential of calcium hydroxide is limited in
compared with C− S− H, due to a considerably lower surface
area. When pozzolanic materials are added to cement, they
1133
react with calcium hydroxide in the presence of moisture to
form secondary calcium silicate hydrate [3, 18].
Flexural Strength
Table 3 and Fig. 2 show the flexural strength values
of samples at 28 days. The flexural strength increased by
increasing CW ratio. The flexural strength had a maximum
value with the addition of CW1 and CW2 in the ratio of
1.5%. However, the flexural strength value became less than
that of the control sample in the case of more than 2.5%
CW1 addition, while it became less than that of the control
sample when more than 5.0% CW2 was added. The decrease
in flexural strength can be explained in a way similar to the
compressive strength decrease in mortar samples as reported
above.
Ultrasonic Pulse Transmitting Time
The ultrasonic pulse transmitting time test consists of
measuring the travel time of a pulse of longitudinal
ultrasonic waves passing through the concrete. Longitudinal
waves with frequencies in the range of 20 to 150 kHz
are normally used. The travel times between the initial
onset and reception pulse are measured. This test gives
considerable information about the interior of the concrete.
Nondestructive test results of mortar containing CW are
presented in Fig. 3. According to the ultrasonic pulse test
results, transmitting time is in the range of 36–78 s. As
the ratio of CW increases, ultrasonic pulse transmitting time
increases. This result is related to the detection of some
negative points such as voids and cracking (not parallel
to the direction of the pulse) in the internal structure
by increasing CW content in mortar samples. The results
obtained from ultrasonic transmitting time experiments are
convenient to those of compressive strength and flexural
strength experiments. There is no significant difference
between CW1 and CW2 in means of ultrasonic pulse
transmitting time.
Setting Time
The term setting refers to the solidification of the
plastic cement paste. The initial set is the beginning of
solidification. The time taken for complete solidification
determines the final set. The setting time is very important
for cement, mortar, and concrete mixtures. The results of
setting time tests are given in Table 4. The initial and
final setting times of mortar samples were considerably
increased by increasing CW ratio. Also, the setting time
of mortar produced with CW1 was longer than that of
CW2. This result shows that boron increased the setting
time. In spite of the delayed setting time with respect to
the control sample, the setting times obtained were within
the limits indicated in TS 19 even in the case of 20% CW
level [10]. Borates were reported to be strong retarders of
cement setting and hardening. Setting time may retard due
to the surface adsorption, the formation of protective layers
over cement grains by precipitation with calcium, and the
increasing of calcium hydroxide solubility [13–16].
 1134
Volume Change
It is essential that a cement paste, once it has set, does
undergo a large change in volume. In particular, there
must be no appreciable expansion, at the conditions under
which restraint could result in a disruption of the hardened
cement paste. The volume changes of the mortar samples
are presented in Table 4.
As seen in Table 4, it was observed that the replacement
of CW by OPC had no remarkable effect on the expansion
of mortar. It can be said that the volume expansion obtained
in the studies carried out using CW2 was lower than that of
CW1. Furthermore, the volume expansion values are in the
limits accepted by TS 19 [10].
Durability
Durability experiments were performed with NaCl and
MgSO4 solutions in order to test the durabilities of the
samples prepared by using CW and cured for 28 days.
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The weight losses of the samples were measured after they
had been put into these solutions for 60 days. The results
are given in Figs. 4 and 5. As known, NaCl and MgSO4
compounds are salts having an explosive effect on concrete,
mortar, and cement. Both salts used in the experiments
react with lime
Ca
OH2  in cement to form CaCl2
and CaSO4 releasing Na+ , Mg2+ , and OH− , respectively,
by the following reactions:
2NaCl + Ca(OH)2 → CaCl2 + NaOH (1)
MgSO4 + Ca(OH)2 + 2H2 O
→ CaSO4 · 2H2 O + Mg(OH)2  (2)
Subsequently, CaCl2 and CaSO4 react with tricalcium
aluminate (C3 A) in the cement to form calcium
chloroaluminate hydrate (Friedel’s salt: 3CaO · Al2 O3 ·
CaCl2 · 10H2 O) and oxychlorides (3CaO · CaCl2 ·
15H2 O CaO · CaCl2 · 2H2 O), and tricalcium sulfoaluminate
or ettringite (Candlot’s salt: 3CaO · Al2 O3 · 3CaSO4 ·
32H2 O), respectively, causing crystal growth, as follows:
CaCl2 + 3CaO · Al2 O3 + 10H2 O
→ 3CaO · Al2 O3 · CaCl2 · 10H2 O (3)
3
CaSO4 · 2H2 O + 3CaO · Al2 O3 + 26H2 O
→ 3CaO · Al2 O3 · 3CaSO4 · 32H2 O (4)
Therefore, a great volume increase appears during the
formation of salt, and the concrete may be cracked due to
the internal tension occurring in the course of this volume
expansion [16–19].
With the examination of Figs. 4 and 5, it is seen that there
is a small weight loss in samples subjected to two different
chemical solutions even in the case of using CW in the high
ratios. Any breakage or cracking was not observed on the
surfaces of the samples since this weight loss remained in
a low level in spite of the high concentration of solutions.
However, in comparison with the control samples, there was
an almost linear increase in weight losses with increasing
M. ÖZDEMİR AND A. UǦURLU
CW ratio. This may result from the fact that the CW has
a small pozzolanic activity, and thus Ca(OH)2 which was
necessary for the formations of CaCl2 and CaSO4 . 2H2 O
(gypsum) is not reduced by pozzolanic reactions.
In the samples prepared with both CW, the weight
losses of the samples subjected to the MgSO4 solution
were generally higher than those of subjected to the NaCl
solution. In other words, the durability performance of the
mortars in the NaCl solution was better. The cementitious
hydration product C− S− H is stable since the formation of
sodium hydroxide, which is a by-product of the reaction,
ensures the continuation of high alkalinity in the system.
In the case of magnesium sulfate attack, the formed
magnesium hydroxide is insoluble and reduces the alkalinity
of the system. In the absence of hydroxide ions in the
solution, C− S− H is no longer stable and is also attacked
by the sulfate solution. So, the magnesium sulfate attack
is more serious on the mortar [18]. These results reveal
that the durability of mortar depended on the type of the
chemical solution as well as the performance of mortar.
Under the light of all these information, it is possible to say
at least that CW affected the durability negatively in a low
level for both of the chemicals. In some studies concerning
the long term behaviors of the Portland limestone cement
mortars exposed to sodium sulfate or magnesium sulfate
attacks, it was reported that the mortars containing limestone
were affected slightly by sulfate attack at 20
C and damage
was not observed at 25
C [20–22]. Similar results were
also obtained in this study since CW consisted mainly of
CaCO3 .
Conclusions
In this study, the use of CW containing boron as cement
additive in mortar was investigated by using the fresh
and hardened concrete tests. From the test results, it was
found that clay waste can be used in cement, mortar, or
concrete as an additive up to 5% of cement with comparable
performance or better performance to that of ordinary
Portland cement. However, CW1 and CW2 can be used as
an additive up to 7.5% and 15% of cement, respectively,
according to the requirement of 32.5 MPa for the 28-day
strength for grade 32.5 cement. As the ratio of clay waste
increases, the alkali content of cement increase. It is known
that a high alkali content also reduces the long term strength.
Therefore, the long term performance of cement should be
investigated. Furthermore, for a more economical use of the
clay waste, the studies should especially be directed towards
the use of the clay waste with other additives having a high
pozzolanic activities. By this way, the usage ratio of the
clay waste in the cement may be increased. This will enable
to reduce the OPC consumption, and thus energy cost and
CO2 emission will decrease, and this will contribute to the
production of environmentally friendly cement.
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