Applied Clay Science 53 (2011) 561–565

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Applied Clay Science

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / c l a y

Research Paper

The effect of incorporation of a Brazilian water treatment plant sludge on the

properties of ceramic materials
S.R. Teixeira ⁎, G.T.A. Santos, A.E. Souza, P. Alessio, S.A. Souza, N.R. Souza
Department of Physics Chemistry and Biology, Univ. Estadual Paulista, UNESP, Rua Roberto Simonsen, 305, P.O. Box 266, 19060-080, Presidente Prudente, SP, Brazil

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

Article history: We evaluated the feasibility of incorporating sludge from decantation ponds of a water treatment plant (WTP)
Received 14 September 2010 into a ceramic body used in ceramic brick manufacturing. The sludge grain-size distribution (silt, sand and
Received in revised form 2 May 2011 clay) and the effects of its incorporation on the properties of the ceramic body were studied. Samples were
Accepted 4 May 2011
collected during a period of ten months. The chemical and mineralogical compositions of the WTP sludge
Available online 8 June 2011
varied according to the month of sludge production, but the compositions are similar to those of the natural
Keywords:
raw material used by the red ceramic industry. Technological tests of ceramic probes showed that this residue
Water treatment sludge can be incorporated into clays used to produce ceramic bricks. The concentration of sludge to be incorporated
Clay depends on its properties (grain-size distribution and chemical and mineral composition), but mainly on the
Texture properties of the raw material (matrix) used.
Red ceramic © 2011 Elsevier B.V. All rights reserved.
Physical properties

1. Introduction amount of sludge released into waterways is still substantial

(Monteiro et al., 2008). A comprehensive study about biosolids was
Conventional water treatment plants (WTPs) transform crude published by Andreoli (2006) where he presented the state of the art
water into potable water utilizing a series of processes: coagulation, in alternatives for recycling of sanitation waste in the manufacture of
flocculation, decantation and filtration. The process of coagulation red ceramics.
involves the use of Fe or Al salts that form floccules with impurities in The sludge generated in WTPs is a solid residue that should be
water, which sediment (or float) and are later filtered out. This properly treated and disposed without causing harm to the environ-
treatment produces a solid residue (alum or ferric sludge) with a high ment. One of the techniques used to prepare sludge for disposal is
water content, whose composition depends on the origin of the crude dehydration, resulting in a cake with a concentration of solids of 60 to
water collected (surface water or groundwater through wells), the 70%. This cake can be used as fertilizer, incinerated, disposed in landfills
type of soil of the region, the material discharged into the river, for urban waste, and composted with urban waste, among other
chemical products present, the process of treatment employed, etc. alternatives. More recently, the alternatives in which the residue is
The main components of the sludge from WTPs are (sometimes utilized or transformed into products that are useful to society
known as water treatment residues): clay minerals, very fine-grained have been studied. An important one of them is the utilization of
minerals (mainly oxides and hydroxides of aluminum and iron), residues in making cement and ceramic bodies. Its incorporation
organic matter and contaminants from the discharge of urban and into ceramic bodies for the production of bricks and roof tiles is a
industrial effluents and other human activities. viable practice, and could be of interest to ceramic manufacturers
In general, this sludge is dumped directly into rivers and streams (Andreoli, 2006; El-Mahllawy and El-Sokkary, 2008; Huang et al., 2001,
or into the drain system, causing a significant environmental impact, 2005; Jordan et al., 2005; Kayaci et al., 2010; Li et al., 2005, 2006;
which compromises the quality of drinking water and the health of Menezes et al., 2002; Monteiro et al., 2008; Oliveira et al., 2006; Teixeira,
the public and animals that utilize it. The growing concern of 2006; Teixeira et al., 2002, 2006; Ueno and Leite, 2007; Vieira et al.,
environmental organizations, due to the risks to health and to the 2008; Weng et al., 2003; Zou et al., 2009).
environment, has led to the restriction or prohibition of discharging The recycling of residues can reduce environmental impacts,
this residue into the environment (streams, landfills, soil, etc.). increase the useful life of the mineral raw materials used, and lower
Currently, there are more than 7500 complete cycle (or conventional) final production costs. The ceramic industry is a very important sector
WTPs in Brazil, and even though there is legislation prohibiting it, the in Brazil and is widespread. Brazilian consumption of clay has
surpassed 150 million tons/year since 2005 (MME, 2009). Sludge
from WTPs, mainly from the treatment of surface water, can be
⁎ Corresponding author. Tel.: + 55 18 322953 55; fax: + 55 18 3221 5682. incorporated into ceramic bodies; sludge contains minerals that are
E-mail address: [email protected] (S.R. Teixeira). common in clays, and therefore, its composition facilitates the clay/

0169-1317/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.clay.2011.05.004
562 S.R. Teixeira et al. / Applied Clay Science 53 (2011) 561–565

sludge mixture (Monteiro et al., 2008). One of the main contaminants bending test using a universal machine (EMIC, model DL 2000)
of sludge is associated with the type of flocculants used for its (Santos, 1989; Teixeira, 2006).
precipitation. In previous work, we observed that the sludge obtained
with aluminum-based chemical is more deleterious to ceramic 3. Results and discussion
properties than those obtained with iron compounds (Teixeira et al.,
2002, 2006). 3.1. Grain-size distribution
This paper presents the results of a study conducted over ten
months with the aim of evaluating the variation of grain-size Texture analysis showed that the fractions of clay, silt and sand of
distribution (texture) in sludge from water treatment. Also, we the sludge varied monthly. The percentages of these fractions differ
assessed the technological properties of ceramic bricks obtained with according to the time of the year in which the sludge was produced.
the addition of sludge to clayey material used by ceramic industry. Fig. 1 shows the variation of the fractions and of organic matter, in the
ten sampling months and, the variation of the water level measured
using a fixed ruler in the river where water was drawn for the WTP.
2. Materials and methods The changes in river levels were associated with the amount of rainfall
in the region. The concentration of organic matter showed no
From 2001 to 2004, samples were collected on the washing dates apparent variation. On the other hand, sand showed a tendency to
of the first decanter of the WTP of the state sanitation company vary inversely with the level of the river, while clay decreased at the
SABESP (Companhia de Saneamento Básico do Estado de São Paulo) in lowest river level. During the sampling period (10 months), clay
Presidente Prudente County, located 558 km west of São Paulo, the concentration varied from 30 to 60 wt.%. As shown by the lowest river
capital city of the state of São Paulo. This company uses the levels (Fig. 1), the months of June to September had the lowest rainfall
conventional coagulation–flocculation–sedimentation pretreatments in the region, which is normal at this time (winter) in the southern
in its water purification system. During this period, three different hemisphere.
coagulants were utilized (aluminum sulfate, ferric chloride and The ideal grain-size distribution for each type of product for the
aluminum polychloride), and samples were collected monthly over red ceramic industry is represented in the classical Winkler diagram
ten months. The aluminum polychloride coagulant was adopted by (Monteiro and Vieira, 2004). It consists of a triaxial scheme where
SABESP due to its higher efficiency in the coagulation of solid particles each axis represents the sand, silt and clay fractions and, it can be
in treated water. Therefore, the sludge incorporated in the ceramic organized in regions in which each component may have a variable
material for technological tests was obtained with this chemical and composition as shown in Table 1. According to these ranges, the
called sludge-Al. The tank was divided into six parts, and two liters of sludge had a concentration of clay that gave it an ideal plasticity for
sludge were obtained from each one, totaling twelve liters per making roof tiles and ridge caps. It was also evident that the
sampling. The samples were mixed and dried in an oven at 110 °C, concentrations of clay greater than 40% conferred high plasticity to
broken up and pulverized in a blade mill, and the resultant material the ceramic body, causing problems in the drying and firing of ceramic
was then passed through a # 40 sieve (0.42 mm). pieces. In some cases, the concentration of sand (non-plastic material)
Concentrations of organic matter (OM) were determined by the was also very high, which can worsen the properties of the ceramic
Walkley–Black method (EMBRAPA, 1998) and the concentrations of material. Therefore, the sludge to be used for mixing with the ceramic
the sand, silt and clay fractions by the pipette method, in the samples raw material should have concentrations of clay and non-plastic
of sludge and clay, with prior oxidation of the organic matter using materials compatible with those ranges shown in the Winkler
hydrogen peroxide (Dixon and White, 1996; Klute, 1986). The main diagram. As the raw material used in this paper has high plasticity,
minerals in the clay were determined in a previous study (Teixeira et we used the sludge with the highest concentration of sand.
al., 2001). The sludge minerals were identified using a D/MAX-2100/
PC, Rigaku X-ray diffractometer (copper radiation, Ni filter and 0.02° 3.2. X-ray diffraction and chemical analysis
step). These samples were K or Mg saturated and oriented (spread) on
glass plates (Dixon and White, 1996; Moore and Reynolds, 1997). X-ray diffraction analysis (Fig. 2) of the clay material and of
Chemical analysis of a sample of sludge, to test for the presence of oriented clay plates showed kaolinite (0.723 and 0.359 nm) as the
heavy metals, was carried out in a laboratory certified for chemical predominant clay mineral, along with the presence of mica (1.068 and
analysis using atomic absorption spectrophotometry (AAS), in
accordance with established standards. A thermogravimetric system
(TG-209, NETZSCH Instruments) and a differential scanning calorimetry
apparatus (DSC 291A, TA Instruments) were used to characterize the
samples, at 10 °C/min in air (50 ml/min).
Ceramic probes (CPs) were pressed uniaxially (19 MPa, 60 ×
20 × ~5 mm 3) in triplicate, using clay from the floodplains of the
Paraná River (on the Bauru Sandstone), which is also used to produce
bricks by the ceramic industry located in the Presidente Prudente
region, São Paulo state, Brazil. This raw material has 57 wt.% clay,
37 wt.% silt, 6 wt.% sand, a high plasticity limit (40.6%) and low
concentration of organic matter (5.57 wt.%) (Teixeira et al., 2001). The
sludge concentration added to the clay ranged from 0 to 30 wt.%. After
firing in a laboratory kiln at five temperatures varying from 850 to
1200 °C, the CPs were submitted to technological tests according to
Brazilian norms for the evaluation of ceramic properties. Water
absorption (WA), apparent porosity (AP) and apparent specific mass
(ASM) were determined using an analytical balance and the
Archimedes method. Linear shrinkage was determined by measuring
the length of the samples before and after firing using a caliper. The Fig. 1. Variation of the grain-size fractions and of organic matter in the sampling
flexural rupture strength (FS) was determined by the three-point months and, the variation of the river water level at the point of water collection.
 S.R. Teixeira et al. / Applied Clay Science 53 (2011) 561–565 563

Table 1
Ideal grain-size distribution for ceramic masses according to the Winkler diagram
(Monteiro and Vieira, 2004).

Type Clay ≤ 2 μm Silt 2–20 μm Sand ≥ 20 μm

I. Plasticity very high 40 to 50 20 to 40 20 to 30

(difficult workability)
II. Roof tiles and ridge caps 30 to 40 20 to 50 20 to 40
III. Perforated bricks 20 to 30 20 to 55 20 to 50
IV. Heavy bricks 15 to 20 20 to 55 25 to 55

0.500 nm), goethite (0.415 nm) and quartz (0.333 nm). This clay also
contained, at lower concentrations, other iron oxides, titanium oxides,
gibbsite and other 2:1 type minerals such as smectites (Dixon and
White, 1996; Moore and Reynolds, 1997). The ceramics factories of
the region use floodplain clays which have a similar mineralogical
composition, as observed in a previous work (Teixeira et al., 2001).
Considering the major minerals and texture of the sludge used, we
Fig. 3. X-ray diffraction pattern of oriented clay minerals in the WTP sludge.
observed that this material has a composition similar to that
characteristic of non-plastic material (high concentration of sand
and silt) used to mix with raw material (predominantly kaolinitic
3.3. Thermal analysis
clays) with high plasticity (high concentration of clay minerals). The
sludge collected during the rainy season (October to May) has a
Fig. 4 shows the thermograms (TG/DTG) for two samples of sludge
particle size distribution (high plastic clay concentration and low
with iron and one with aluminum, collected in different periods. The
concentration of non-plastic material) close to that observed for
thermogravimetric analysis data showed that there was a loss of
kaolinitic clays used in brick production (Monteiro et al., 2008;
moisture of approximately 9% (near 65 °C), loss of water due to
Teixeira et al., 2001). Fig. 3 shows the diffractogram of the oriented
decomposition of hydroxides (aluminum and iron) and burning of
clay slide of the sludge sample, collected in the month of August,
organic matter on the order of 7% (close to 265 and 315 °C), and loss of
obtained using aluminum polychloride as coagulant. Here, the main
structural water from kaolinite of 7% (around 500 °C) (Monteiro et al.,
clay minerals noted above can be identified.
2008; Teixeira et al., 2008).
Chemical analysis (X-ray fluorescence — XRF) of a sample of
Fig. 5 shows the data for differential scanning calorimetry (DSC) of
sludge showed that iron, silicon, aluminum and titanium were the
WTP sludge with two different coagulants used (Fe and Al), clay used
main components of the sample, with a small concentration of
for the production of bricks, and kaolin from Georgia (USA).
calcium. Quantitative analysis by atomic absorption spectropho-
Comparing the diagrams, it can be seen that all three samples showed
tometry (AAS) showed that the concentrations of the heavy metals
kaolinite as the main clay mineral. Besides the loss of free water
Pb (0.42 ppm), Cr (4.60), Zn (31), Mn (121), Al (0.43) and Cu (15)
(~70 °C), there was an exothermic band (200–450 °C) that was
were below the limits recommended for agricultural recycling of
greater in the samples with WTP sludge, characteristic of organic
sewage sludge (Mota, 2003). This result was expected since this is
matter oxidation and also to the crystallization of amorphous phases
a farming region with little industry. The concentration of Fe
of iron and aluminum (gels) (Gastuche et al., 1964), formed during
(130,800 ppm) was high due to the coagulant used, which has an
the chemical treatment of the water to precipitate the sludge. The
iron base. The presence of heavy metals in the sludge does not
narrow peak observed at 573 °C is characteristic of the α ↔ β phase
prohibit its incorporation into ceramic materials, considering that
transition of quartz, present in the clay sample. The book edited by
these metals can be incorporated and made inert in the crystalline
Dixon and Weed discusses the possible transformations of iron
structure of vitreous phases formed during the sintering process of
(Schwertmann and Taylor, 1989) and aluminum (Hsu, 1989)
ceramics.
hydroxides into oxides and polymorphic transformations of silica.

Fig. 2. X-ray diffraction pattern of clay material used by ceramic industry (Enclosed Fig. 4. Thermogravimetric data TG and DTG (Derivative TG curve) of WTP sludge (using
XRDP of saturated (K and Na) and oriented clay slides). iron chloride and aluminum sulfate).
564 S.R. Teixeira et al. / Applied Clay Science 53 (2011) 561–565

Fig. 5. Differential scanning calorimetry (DSC) data of clay material, kaolin and sludge Fig. 7. Three-point flexural strength (FS) for ceramic probes with (0, 10, 15 and 20 wt.%)
using different coagulants. incorporated sludge.

3.4. Technological tests due to the high concentration (29%) of organic matter in sludge,
which increases the porosity of the sample during firing.
The results with sludge obtained using the coagulant aluminum The behavior of the properties (WA, ASM, LS) of ceramic bodies
sulfate (sludge-Al) were always poorer than those with ferric chloride with sludge were similar to those of pure clay material (Teixeira et al.,
(sludge-Fe) as observed in a previous work. In general, the aluminum 2004), showing that it determines the final properties of the material.
increased the refractivity and the friability of ceramic material, while All the properties of clay with sludge showed little variation below
the iron improved the properties of material resulting from the 1000 °C. At this temperature up to 1100 °C, the variation was abrupt,
reaction with mica in the formation of a glassy phase (Teixeira et al., and then for the greater concentrations of sludge the properties
2006). tended to stabilize. This effect, of the improvement of ceramic
In general, the results of the technological tests showed that the properties with increase in temperature, was already expected since
incorporation of sludge from WTP consistently worsened the a liquid phase occurs above 1000 °C, with greater densification of the
technological properties of the ceramic materials, as also observed ceramic probe. However, the slowdown of the reaction between 1100
in other studies (Jordan et al., 2005; Monteiro et al., 2008; Teixeira and 1150 °C was not expected, indicating that with sludge the
et al., 2006; Weng et al., 2003). However, research results show that it densification reactions occurred at temperatures lower than those for
is possible to produce materials within the limits specified by the pure clay, and crystallization of new phases could have occurred with
regulations of each country, controlling the amount of sludge to be the production of microfissures. The highest concentration of quartz
added to the ceramic material and the sintering temperature. due to the sludge may contribute to an increase in porosity and
Figs. 6 to 8 show the results of technological tests for clay with microcracks generated by its alpha-beta transition (573 °C) during
sludge-Al (10, 15 and 20%) collected in the month of August, which cooling of the ceramic bodies. These microfissures tend to increase
had a greater concentration of sand. In general, the variation in the water absorption and decrease apparent specific mass and mechanical
properties of the samples was approximately equal for the additions resistance.
of 15 and 20% sludge. The graphs show that the incorporation of Linear firing shrinkage (Fig. 8) changed little at low temperatures
sludge increased water absorption and decreased apparent specific (up to 900 °C) due to the high concentration of sand (non-plastic
mass (Fig. 6) and flexural strength (Fig. 7). These effects are mainly material) in sludge. Above this temperature there was a substantial

Fig. 6. Water absorption (WA) and apparent specific mass (ASM) of ceramic probes Fig. 8. Linear firing shrinkage of ceramic probes with (0, 10, 15 and 20 wt.%)
with (0, 10, 15 and 20 wt.%) incorporated sludge. incorporated sludge.
 S.R. Teixeira et al. / Applied Clay Science 53 (2011) 561–565 565

increase in linear shrinkage due to the formation of a liquid phase, up to Jordan, M.M., Almendro-Candel, M.B., Romero, M., Rincón, J.Ma., 2005. Application of
sewage sludge in the manufacturing of ceramic tile bodies. Appl. Clay Sci. 30,
1100 °C. At this temperature range, LS was more evident for CPs with 219–224.
added sludge due the presence of fluxing material (mica and goethite) Kayaci, B., Kara, A., Kayaci, K., Samet, Küçüker A., 2010. Re-use of mud from process
in sludge (Fig. 3). Again, there was a change in behavior at 1150 °C for waste water purification plant in ceramic tile production. Ind. Ceram. 30, 195–207.
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Acknowledgements used in the structural ceramic industry in west of S. Paulo State, Brazil. Cerâmica 47,
204–207http://www.scielo.br/pdf/ce/v47n304/7813.pdf.
Teixeira, S.R., Souza, S.A., Souza, N.R., Job, A.E., Gomes, H.M., Heitzmann Neto, J.F., 2002.
The authors thank SABESP of Presidente Prudente for their Caracterização de resíduos de estação de tratamento de água (ETA) e de esgoto
collaboration, FAPESP for fellowships and grant support (PROC. (ETE) e o estudo da viabilidade de seu uso pela indústria cerâmica (Characteri-
zation of waste water treatment plants (WTP) and sewage (WTS) and study of
2008/04368-4), and the CNPq/PIBIC program for the Student Scientific
feasibility of its use by the ceramic industry). XXVII Congresso Interamericano de
Initiation grants. Dr. A. Leyva helped with the English editing of the Ingeniería Sanitaria y Ambiental, Cancun-Mexico.
manuscript. Teixeira, S.R., Souza, S.A., Nobre, M.A.L., 2004. Physical and mechanical properties of
ceramics from clays of the west of S. Paulo State, Brazil. Cerâmica 50,
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