Applied Clay Science 118 (2015) 171177

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Applied Clay Science

journal homepage: www.elsevier.com/locate/clay

Research Paper

Utilization of water treatment plant sludge in structural ceramics bricks

A. Benlalla a, M. Elmoussaouiti a,, M. Dahhou a, M. Assa b
a
Department of Chemistry, Laboratory for Materials, Nanomaterials and environment, Faculty of Science University Mohamed V., Rabat, Morocco
b
National Ofce of Electricity and Drinking Water, International Water and Sanitation Institute Rabat, Morocco

a r t i c l e i n f o a b s t r a c t

Article history: The main aim of this study is to assess the effect of incorporating water treatment sludges (WTS) of plant
Received 13 May 2015 Bouregreg on the properties and microstructure of clay used for raw material.
Received in revised form 14 September 2015 This work proposes to test the clays used in the manufacture of a ceramic that could incorporate alumina sludge.
Accepted 15 September 2015
The raw materials, alumina sludge and clay, were mixed together in different proportions, were prepared by
Available online 6 October 2015
incorporating from 5 to 30%. Specimens of these mixtures were then red at 800, 900, and 1000 C. In order to
Keywords:
determine the technological properties, such as bulk density, linear shrinkage, water absorption, compressive
Drinking water sludges strength, X-Diffraction, and Scanning Electron Microscopy. The results obtained showed that the samples tested
Terracotta are dense and have high mechanical resistance, without deformation or defects.
Technological properties These clay materials may be used for the production of terracotta products and also for the formulation of low
Low porosity porosity raw material.
2015 Elsevier B.V. All rights reserved.

1. Introduction
A water treatment plant produces large quantities of sludge as a
result of treatment processes of raw water such as occulation, ltration
and coagulation. According to regulations, drinking water sludges are
classied as non-hazardous waste also known as banal industrial
waste (BIW). That implies that they are not submitted to the heavy
constraints of hazardous waste (Miroslav, 2008). This sludge can be
dewatered further by thickening, centrifugation and ltration opera-
tions in order to recover water and minimize the volume of the waste
stream is commonly to dewater the sludge up to about 30% dry
matter(DM) and then pay to send it to a commercial landll (Benlalla
et al., 2015).
However, this practice is becoming more and more expensive.
Consequently, National Ofce of electricity and drinking water of
Bouregreg initiated a research project on alternative methods for utili-
zation of mill sludges. Questions have been raised in regard to the
potential environmental impacts of the sludge when used.
The recycling of such waste to fabricate structural ceramics can be
technologically, economically, and environmentally attractive because
it produces materials with greater exural strengths and provides
for adequate treatment of the water treatment plant (WTP) sludge.
Therefore this technological innovation for manufacturing news
products was able to minimize the impacts of WTP residues and can
be seen as an environmental performance of industrial solid waste
from WTP.
Corresponding author.
E-mail address: m.elmoussaouiti@gmail.com (M. Elmoussaouiti).
The sludge produced by WTP can be used like additive to produce
high-alumina refractory ceramics, lightweight aggregate (LWA), Glass-
ceramics, and nally as a prime material for clinker manufacture
(Ferreira and Olhero, 2002; Huang and Wang, 2013; Toya et al., 2007;
Husillos Rodrguez et al., 2011).
The sludge produced by WTP can also be a potential substitute for
brick clay because its chemical composition is very close to that of
brick clay (Hegazy et al., 2012). In addition, the use of sludge in the con-
struction industry is considered to be an economic and environmentally
sound option (Ramadan et al., 2008). The concentration of sludge that
can be incorporated into clays in order to produce bricks depends partly
on the sludge properties (grain-size distribution and chemical and min-
eral composition) but even more so on the properties of the raw mate-
rials used (Teixeira et al., 2011). Using bench-scale experimentation,
(Alleman and Berman, 1984), showed that conventional clay and
shale ingredients for bricks could be partially supplemented with
sludge. They called this clay product biobrick. Bricks manufactured
from dried sludge collected from an industrial wastewater treatment
plant were investigated by (Lin and Weng, 2001; Weng et al., 2003b).
These reports showed that the sludge proportion and the ring
temperature were the two key factors determining brick quality (Liew
et al., 2004). In accordance with a previous study, bricks produced
from sewage sludge of different compositions were investigated by in-
corporating WTP sludges with different proportions that can reduce
the cost due to the utilization of waste and, at the same time, it can
help to solve an environmental problem (Pereira et al., 2000). The utili-
zation of WTP sludge in brickmaking eliminates an environmental prob-
lem, several economies related to the replacement of a natural raw
material are generated, leading to environmentally friendly practices
(Beretka, 1975).

http://dx.doi.org/10.1016/j.clay.2015.09.012
0169-1317/ 2015 Elsevier B.V. All rights reserved.
172 A. Benlalla et al. / Applied Clay Science 118 (2015) 171177

Table 1
Chemical compositions of raw materials determined by XRF.

Raw materials SiO2 Al2O3 Fe2O3 TiO2 CaO MgO Na2O K2O P2O5 LoI Total

WTP sludge 27.12 62.66 1.16 0.16 1.25 0.37 0.24 0.83 0.19 5.11 99.09
Clay 54.17 15.27 6.81 0.91 10.88 7,74 0.76 2.85 0.12 10.29 99.51

LoI: loss Ignition.

Utilization of water treatment sludge in the industry of construction
products is promising and economically reasonable, and the products
produced are not contaminated with hazardous impurities (Liew
et al., 2004). Therefore, the objective of the research is to determine
the inuence of drinking water treatment sludge, which is composed
from a large amount of Al2O3, on physical and mechanical properties,
structural parameters, mineralogical composition of the ceramic body
burned at 800 to 1000 C temperatures. In addition, the possibility to
utilize this additive in the production of ceramic products was studied.
2. Experimental
This section describes the materials and methods used to investigate
the feasibility of using WTS for brick production and characterize the
structural properties of the resulting bricks.
(20 L capacity) and mixed for 60 min while water was added after
10% moistening by weight. The plastic mixtures prepared in this way
were stored in plastic bags for one day to achieve a homogenous distri-
bution of moisture.
The plastic mixtures were molded in a pilot scale screw mold of
size 80 30 20 mm. the shaped samples were held for one day and
then dried in an oven at 105 C until constant weight was achieved.
The dried samples were then red in an electric furnace at three
different test temperatures; 800 C, 900 C and 1000 C at an average
heating rate of 5 C/min with a 2 h soaking time at the respective
peak temperatures. The samples were furnace cooled for further
experiments. Fig. 1 shows aspect of raw samples and red at 800 to
1000 C.
2.4. Brick testing method

2.1. Sludge and clay samples
The sludge used in this work was collected from the water treatment
plant of Bouregreg located in the city of Rabat (Morocco). In this indus-
try, the water is treated with aluminum sulfates, and cationic polyelec-
trolytes. The sludge was collected from thecoagulation/occulation tank
once a week during 12 months. The material was sun-dried during 72 h
and stocked after each collection. All the collected materials were ho-
mogenized. The dried materials were then milled and passed through
a 0.6 mm sieve before use. The used clays were supplied by a local bricks
industry (Rabat. Morocco). The samples of clay were also sun-dried
during 72 h and sieved to 0.6 mm particles. In order to get a uniform
particle size. Both sludge and clay were dried with an electric heater
during 48 h at 105 C in order to remove moisture, to get a representa-
tive samples for a number of chemicalphysical analyses.
2.2. Characterization of raw materials
Tables 1 and 2 show the chemical composition by XRF and a range of
metals including Pb, Cd, Cu, Cr, Zn and Ni analyzed using ICP. All of these
metals and their concentration in the sludge is an important indicator
for the quality for sludge. It can be seen that Alumina is the most abun-
dant element in the sludge, which also contains a signicant amounts of
Silica, as well as minor amounts of Fe2O3, CaO, MgO, Na2O and K2O.
Environmental safety testing based on heavy metals concentration in
WTS tested shows the satisfactory in comparison to the permitted
standards (TCVN 59452005: Fe b 5, Ni b 0.5, and Cr6 + b 0.1 ppm)
(Degirmenci, 2008).
Because water content is an important factor affecting the quality of
the brick, tests compaction, and Atterberg limits were conducted, to ob-
tain the plastic nature of the sludgeclay mixtures and to determine the
optimum moisture content (OMC) in the brick manufacturing process.
Using this OMC, the mixtures with various proportions of sludge and
clay were prepared in batches. The methylene blue value (BV) reects
the activity of the clay fraction, thus, it gives an indication of the miner-
alogy of this fraction and the cation exchange capacity (CEC) of clay
minerals. Methylene blue tests performed in this study are based on
the French standard Norme Franaise NF P 94068 AFNOR (1993).
This procedure is continued by adding further 5 mL portions of the
methylene blue solution to the clay suspension until a halo of light
blue dye surrounds the dark blue spot on the lter paper (Trkz and
Tosun, 2011).
The produced bricks then underwent a series of tests including ring
shrinkage, weight loss on ignition, water absorption, bulk density, and
open porosity were conducted according to ASTM C373-88 (ASTM
C373-88, 2006a; ASTM C674-88, 2006; ASTM C326-03, 2006), and
compressive strength to determine the quality of bricks. As the major
properties of the ceramics materials are intimately connected to their
mineralogical composition, the samples were nely crushed and analyzed
by X-ray diffraction. The different phases formed after ring at 1000 C
were identied using the XPERT DATA COLLECTER software. The samples
microstructure was evaluated using scanning electron (SEM).
3. Results and discussion
3.1. Atterberg limits of claysludge mixtures

2.3. Preparation blocks sludge bricks Atterberg limits are an important indicator for several properties of
clayey soils: plasticity, sensitivity, consistency and shrinkage/swelling
Bricks containing 5 to 30% WTS by weight were produced in accor- potential. Their determination gives a rst insight for the mineralogical
dance with the mix compositions as shown in Table 3. The mixture of composition of clays. The liquid and the plastic limits are highly and
brick clay and WTS slurry was placed in a commercial kitchen mixer
Table 3
Samples of bricks masses with WTP sludge (wt.%).
Table 2
Concentrations of main heavy metals of WTP sludge determined by ICP (ppm on dry Firing temperature Formulations of mixtures containing WTP sludge
material).
5% 10% 15% 20% 25% 30%
Element Cd Cr Cu Ni Pb Zn
800 C S1 S2 S3 S4 S5 S6
Sludge 5 31 17 15 36 35 900 C SA SB SC SD SE SF
1000 C SG SH SI SJ SK SL
ppm: parts per million.
 A. Benlalla et al. / Applied Clay Science 118 (2015) 171177 173

Fig. 2. Compaction proctor test curve.

sludgeclay mixtures show that incorporating the sludge with different

concentration did not inuence the value of placticit. It can be noted
that claysludge mixtures are highly plastic clays with a very soft
consistency. The plastic limit values shown in Table 4 indicate that up
to 30% of sludge can be applied into brick without losing its plastic
behavior.

3.2. Proctor compaction test

A standard compaction test was used to determine the OMC which is

Fig. 1. Aspect of raw samples (A) and red (B) at 800 C to 1000 C.
mainly inuenced by the ability of clay minerals to interact with liquids
(Schmitz et al., 2004). Several studies had determined a direct link
between the mineralogy of clays and geotechnical properties (Mitchell,
1993; Kaya, 2009).
Table 4 gives the results of the determination of Atterberg limits of
sludgeclay mixtures. According to these results, the effect of moisture
on the pulverized material's plastic behavior is demonstrated in accor-
dance with the Atterberg Limits test. The results of Atterberg's tests of
Table 4
Values of plasticity parameters of sludgeclay mixtures.
an important factor affecting the properties of brick. The OMC of a
mixture was based on the moisture requirement in which maximum
bonding among the mixture particles is retained. The test results show
that the OMC is 23% for clay mixture. Increasing the sludge proportions
in the mixture resulted in an increase of OMC (Fig. 2).
3.3. Methylene blue value
The methylene blue value (MBV) represents the amount of MB
sorbed by 100 g of sludge sample. The MBV is calculated according to
Eq (1), where Vcc represents the volume of methylene blue solution
(ml) consumed by the sludge suspension and f is the dry weight of
the sludge sample (g).

S1 5% S 2 10% S3 15% S4 20% S5 25% S6 30% Table 5

Liquid limit (WL) 63.6 62.9 65.4 60.9 52.5 61.7 Methylene blue value (MBV) for sludge and clay minerals.
Plastic limit (WP) 39.1 31.6 32.3 31 28.9 31.3
Sludge Kaolinite Chlorite Illite Smectite
Plasticity index (IP) 25 31 33 30 24 30
BV (g100 g1) 0.32 1 3 31
*S: Sample.
174 A. Benlalla et al. / Applied Clay Science 118 (2015) 171177
Fig. 3. The weight loss on ignition of bricks.
Table 5. shows the results of the methylene blue test which are com-
pared to values assigned to clay minerals (Tran, 1980) presented in the
same table.
g
  Vccml  0:01
g
MBV =100g ml  100
0
f g
This test is based on the interaction of the MB dye cation (MB +)
with either exchangeable interlayer cations present in a clay mineral
(e.g. in smectites) and/or surface adsorbed cations. Clay minerals
possessing exchangeable interlayer cations, a highly negative charge
and a large specic surface area exhibit the highest capacity for cation
exchange (Trkz and Tosun, 2011; Teresa et al., 2001; Hang and
Brindley, 1970).
According to the data above, the Methylene blue value of WTS
(0.32 g) is lower than those of values assigned to clay minerals (Tran,
1980; Eslinger and Peaver, 1988) presented in the Table 5. WTS are of
low and/or medium electrochemical activity and cation exchange
capacity because of the absence of exchangeable interlayer cations.
These clay minerals can interact with MB only via surface adsorption.
Finally, according to the Atterberg limits, the methylene blue values
WTS are silty sands characterized by a highly plastic clay fraction, has
low to medium shrink swell capacity and cation capacity exchange
linked to clay group.
Fig. 4. The brick ring shrinkage.
Fig. 5. The density and porosity of bricks.
3.4. Brick weight loss on ignition
Fig. 3 shows that increasing the sludge proportion and temperature
resulted in increases in brick weight loss on ignition. The weight loss on
ignition criterion for a normal clay brick is 15%, (AASHTO, AASHTO T-99,
1 1982). With 5% to 15% sludge addition, the produced bricks all meet the
criteria. Visual observation showed that an uneven surface was found
for the sludge brick. It is speculated that the formation of this
unwanted surface was mainly due to the organic component burnt off
during the ring process.
The brick weight loss on ignition is not only attributed to the organic
matter content in the clay, but it also depends on the organic content in
the clay and sludge being burnt off during the ring process. In order to
avoid the uneven surface texture of bricks, both sludge and clay was
oven dried at 105 C for about 24 h. Upon drying these samples were
crushed into powder and then mixed well in required proportion by
weight.
3.5. Brick ring shrinkage
The quality of brick can be further assured according to the degree of
ring shrinkage. Normally, a good quality of brick exhibits a shrinkage
below 8%. As shown in Fig. 4, the percentage of shrinkage increases
with the increasing sludge addition. For a clay 30% sludge brick, the
shrinkage is: 1.9, 2.4 and 2.9% at ring temperatures of 800, 900 and
Fig. 6. The water absorption of bricks.
 A. Benlalla et al. / Applied Clay Science 118 (2015) 171177
Fig. 7. Compressive strength of bricks.
1000 C, respectively. The produced bricks all meet the criteria. However,
the ring temperature is another important parameter affecting the de-
gree of shrinkage. In general, increasing the temperature results in an in-
crease of shrinkage. Thus, the proportion of sludge in the mixture and
the ring temperature are the two key factors to be controlled to mini-
mize the shrinkage in the ring process.
Fig. 8. XRD Spectra of samples red at 800 C to 1000 C.
175
3.6. Bulk density and apparent porosity of bricks
The bricks made with clay normally have a bulk density of 1.8 to
2.0 kg/cm3. The measurements of bulk density for different proportions
of sludge red at three temperatures are demonstrated in Fig. 5. As
shown, the bulk density of the bricks is inversely proportional to the
quantity of sludge added in the mixture. A linear relationship between
the bulk density and sludge proportion in the mixture for all three tem-
peratures is observed. The results obtained from the determination of
total porosity as a function of ring temperature (Fig. 5). Apparent
porosity increases as decreases bulk density. In addition this property
decreases with temperature.
This nding is closely related to the quantity of water absorbed
as demonstrated in Fig. 6. When bricks absorb more water, it ex-
hibits a large pore size than the one with less water absorption.
As a result, the bulk density becomes smaller. The ring tempera-
ture can also affect the bulk density of the bricks. The results show
that increasing the temperature results in an increase in bulk
density.
3.7. Brick water absorption
Water absorption is a key factor affecting the durability of brick.
The less water inltrates into brick, the more durability of the brick
and resistance to the natural environment are expected. Fig. 6
shows the results of the water absorption tests for various sludge
176 A. Benlalla et al. / Applied Clay Science 118 (2015) 171177
clay mixtures red at three different temperatures. As shown in
Fig. 6, the value of water absorption is directly proportional to the
quantity of sludge added. Increasing the ring temperature result-
ed in a decrease of water absorption, thereby increasing the
weathering resistance. According to the criterion of water absorp-
tion of bricks in ASTM C373-88, ASTM (2006a); ASTM (2006b),
the ratio is below 15% for rst- class brick and 15 to 20% for
second-class brick. According to this guideline bricks with 5 wt.%
red at 900 C and 510 wt.% red at 800 C to 1000 C are rst
class category, and bricks with 515 wt.% red at 800 C,
520 wt.% red at 900 C and 525 wt.% red at 1000 C are within
second-class category.
The curves for water absorption and linear shrinkage are realized.
This type of curves is also known as gresication diagram, which is
associated with the efciency of the sintering process. The sintering of
a material usually causes many changes in its properties (Edemarino
Araujo Hildebrando et al., 2013).
Gresication diagrams were plotted for the temperature range of
800 C to 1000 C for each mixture. The corresponding curves exhibit
an increase in water absorption and a decrease in linear shrinkage up
to 930 C, it can be observed that above 930 C a sharp change occurs
in the trend of the curves. It is observed that the specication for bricks
was achieved in the studied temperature range (910930 C) for
samples with up to 20% sludge while the sample above 25% sludge
attained only 890 C.
Fig. 9. SEM images of the ceramic bricks red at 1000 C.
3.8. Compressive strength of bricks
The compression test is the most important test for assuring the
engineering quality of a building material. The results of the compressive
strength test on the bricks made from clay and sludge mixtures are
shown in Fig. 7. The results indicate that the strength is greatly dependent
on the amount of sludge in the brick and the ring temperature. Com-
pressive strength of bricks decreases with increase of sludge mix in the
bricks but increases with the increase of ring temperature. As shown,
with up to 30% sludge in the bricks at 1000 C, the strength is even higher
than that of normal clay bricks. When a 5 to 10% sludge is added in the
brick, the achieved brick strength at 900 C and 1000 C lies in the
scope of the 1st-class category. With up to 20% sludge added to the bricks,
the strength measured at temperatures of 800 to 1000 C, met the
requirements of a 2nd class brick standard (Weng et al., 2003a). It is con-
cluded that alumina sludge can be blended with clay in different propor-
tions to produce a good quality brick under a certain temperature.
3.9. Micro-structure and phase analysis
To further investigate the crystalline composition and microstruc-
ture of samples. XRD and SEM analyses were carried out, and the results
are shown in Figs. 8 and 9, respectively. The results revealed the
co-presence of several phases in each one.
 A. Benlalla et al. / Applied Clay Science 118 (2015) 171177
The crystalline phases of thermal treatment of the drinking water
sludge are muscovite KAl2 [(OH, F) 2 | AlSi3O10] and quartz and
common lines between muscovite and quartz. These phases seem
more reactive to thermal treatment, only quartz is stable during this
treatment.
The higher the temperature the more we witness the crystallization of
solid phases that contain calcium, iron, aluminum, potassium, aluminum
silicate, forsterite Mg2SiO4. In turn, the clay is constituted mostly by the
mineral phases such as hematite, quartz.
It can be not observed a trend or, alternatively, the presence of a typ-
ical phase in a group of samples. XRD Fig. 8 analysis shows predominant
peaks of quartz at 27.78 and 20.89, and illite peaks at 19.76 and 50.1302.
In addition, the diopside peaks at 27.90, 31.17 and 70.01 and anorthite
peaks at 31.26 and 35.81 have also been observed.
The sintered specimens produced dense matrix material with good
surface characteristics. It can be seen from scanning electron micro-
graph Fig. 9. that the samples are mainly composed of rounded and
rhombic shaped quartz crystals along with the lath and cubic crystals
of clay.
4. Conclusion
The present study was conducted to develop and to characterize a
clay product with the addition of alumina sludge as a clay substitute.
The feasibility in the use of this material was demonstrated. There is a
good correlation between all the properties tested. Ceramics materials
could be prepared by using clay and sludges waters as source of alumina.
The combination of techniques XRD, SEM, and the characterization of
the technological parameters allowed a better analysis of the structural
and mineralogical evolution after sintering at 1000 C. The environmen-
tal characterization of the product indicates that a material containing
alumina sludge can be used safely. The technological properties are
compatible with those specied for ceramic bricks.
The proportion of sludge in the mixture and the ring temperature
are the two key factors affecting the quality of brick. In all, the recom-
mended proportion of sludge in brick is 20%, with a 30% optimum mois-
ture content, prepared in the molded mixtures and red between 900 C
and 930 C to produce a good quality brick.
Acknowledgments
This study was conducted in the laboratory of quality control (DCE-
ONEEP). The authors acknowledge support from National Ofce of
Hydrocarbons and Mines (ONHYM). Authors would like to thank
National Ofce of electricity and drinking water (ONEEP) for supplying
the drinking water sludge.
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