Separation and Purification Technology 252 (2020) 117417

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Separation and Purification Technology

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

Acidification and flocculation of sludge from a water treatment plant: New T

action mechanisms
⁎
Manoel Maraschin , Keila Fernanda Hedlund Ferrari, Elvis Carissimi
Department of Sanitation and Environmental Engineering, Federal University of Santa Maria (UFSM)

A R T I C LE I N FO A B S T R A C T

Keywords: Sludge acidification is an efficient pretreatment method for achieving effective dewatering. In the specific case of
Sludge acidification water treatment plant sludge (WTP), which uses some type of ion-based coagulant (e.g. aluminum and iron),
Recovery of metal ions these ions can be recovered and intended for a purification step, that will enable their reuse in specific treat-
Helical tubular flocculator ments, significantly decreasing waste disposal and chemicals used for water treatment. This study developed a
Static thickener
system in pilot-scale for the treatment of sludge generated in a WTP with the combined application of two
polymers (dual flocculation) and an acidifier, aiming at the thickening and recovery of metal ions from the
coagulant. The sludge used in this study was sampled in settling basins of a conventional WTP and presented the
solids concentration (TS) of 5 g·L−1, due to the dilution with tap water. The first part of the study compared the
addition of polymers (one cationic and one anionic polymer) in natural and acidified conditions by sulfuric acid
(H2SO4) through continuous treatment. The flocculation step was conducted in the helical tubular flocculator
(HTF), also responsible for sulfuric acid mixing. It was observed that the decrease in pH made the aggregation
easier, contributing to the lower volume of polymers added under mixing conditions provided in the (HTF). The
suggested approach for acid solubilization of aluminum ions provided 87% removal results in sludge samples
with an initial concentration of 510 mg·L−1, from a total TS of 5 g·L−1 and pH 2. This recovery rate was obtained
with the flow rate of 3 L·min−1 (G: 507 s−1) and hydraulic detention time (t) of 24 s. Then, in studies of filtration
thickening, in a built static thickener, and by means of sedimentation, we observed the contribution of the pH
reduction in the water release in the flake mass formed. In addition, there was a significant decrease in specific
filtration resistance (SFR) due to the release of aluminum ions present in the sludge, making the material more
easily dehydrable. The study showed that decreasing from pH 6.5 to pH 2 generated a 50% decrease in SFR. This
reduction in pH further provided a thickened with 20% solids sludge (from an initial content of 0,5%) obtained
through filtration of the mass of the flakes through for a static thickener.

1. Introduction
Coagulation and flocculation are essential physicochemical pro-
cesses used to treat water from surface reservoirs. The chemical agents
used by water treatment plants (WTPs) are generally aluminum or iron
salts, especially aluminum sulfate (Al2 (SO4)3·18H2O) and ferric
chloride (FeCl3·6H2O) [1,2]. This chemical conditioning allows for the
destabilization of the surface charges of solid or colloidal particles,
making possible the aggregation of these impurities [3–5]. Thus, the
destabilized particles begin to aggregate, gain mass and are separated
from the clarified water, either by sedimentation, flotation or filtration
[6,7].
Residues generated during clarification are commonly named
sludge. The main physical characteristic of this waste is its high
percentage of water [8] (commonly greater than 98%). This makes the
material highly unstable, making it difficult to dispose or use, and thus
aggravates irregular situations of its disposal in natural watercourses,
which now incorporate large volumes of natural particles removed from
raw water, but also, add to the products, chemicals used for aggregation
as well as other organic or inorganic constituents utilized during the
treatment [9,10].
The required stability to the sludge begins with the removal of the
free water parcel. At this stage, the addition of flocculant polymers
assists rapid aggregation of the suspension [11], giving rise to a mass of
flakes from the energy ingress capable of dispersing the bridging
polymer chains, adsorbing and connecting the colloidal particles of the
waste to form large flakes that can be effectively removed [3,7,12].
Thus, flocculation aggregation of sludge suspensions can be seen as

⁎
Corresponding author at: Federal University of Santa Maria (UFSM), Av. Roraima 1000, CT Lab, Santa Maria, RS 97105-900, Brazil.
E-mail addresses: maraschinmanoel@gmail.com (M. Maraschin), elvis.carissimi@pq.cnpq.br (E. Carissimi).

https://doi.org/10.1016/j.seppur.2020.117417
Received 9 February 2020; Received in revised form 12 July 2020; Accepted 16 July 2020
Available online 24 July 2020
1383-5866/ © 2020 Elsevier B.V. All rights reserved.
M. Maraschin, et al. Separation and Purification Technology 252 (2020) 117417

Fig. 1. Helical tubular flocculator.

Fig. 2. Conventional treatment for coagulants recovery.

the first effective phase in the pre-treatment of these residues, and the electrochemical agents that make it possible to improve its character-
mechanisms and interactions that characterize it tend to influence all istics and performance during treatment [4,25–28]. For WTP sludges,
treatment stages, either thickening or dehydration [13,14]. Thus, the application of acids and alkalis is closely related to coagulant re-
charge characteristics, ionic properties, functional groups, and mole- covery [29–32]. The metal hydroxides used in the coagulation re-
cular weight are the main characteristic elements of the polymers to be present an important portion of the final volumetric composition of the
evaluated in the selection of the best treatment flocculant [5,15]. residue. Thus, there is a possibility of sludge volume reduction, which
However, the selection of the ideal flocculant polymer is closely may reach reductions close to 45% over the final residue [29,33]. Thus,
linked to the type of flocculant and the type of mixture [15,16]. Given there are reductions in costs with the disposal of the material, as occurs
this fact, many studies have aimed to improve the current flocculators with the contracting of space in landfills and transportation, as well as
or even the development of new equipment that can generate savings in the possibility of using the recovered coagulant. The process occurs by
its implementation and operation. In this scenario, the helical tubular dissolving the coagulant present in the sludge, mainly precipitates of Al
flocculators (HTF) has most recently been highlighted. These floccula- (OH)3, which upon addition of acid, generate soluble aluminum species
tors were initially studied by Grohmannet et al. [17], and consist of a [34]. Solubilization of aluminum sludge can be represented by the
flexible tubing wrapped in a rigid structure, giving rise to a helical following reaction: 2Al(OH)3 + 3 H2SO4 ↔ Al2(SO4)3 + 6H2O. How-
tubular system, as shown in Fig. 1. Mixing of the polymers with the ever, there are still few studies that relate certain chemical pre-treat-
effluent occurs taking advantage of the established hydraulic flow, ments, considering the impossibility or difficulty of an effective stabi-
without the need for any complementary stirring device. The degree of lization of the residue when only a certain stage of treatment gets
mixing, as with other flocculation equipment, is given by the velocity performed.
gradient (G) for hydraulic mixing (Equation (1)). In this paper, characteristics resulting from chemical pretreatment
by flocculation and acidification applied together with the sludge
γ ·Hf
G= generated in the WTP decanter are evaluated. The developed system
μ·t (1) operates from flocculation in an HTF, where polymers and acid are
−3 applied to the aggregation system line, a deficiency found in the lit-
where; γ = specific weight of the liquid mass (kgf·m ) and Hf = head
loss (m); μ = absolute viscosity of the liquid mass (kgfs·m−2). The Hf erature, given that the conventional process (Fig. 2) occurs in stages,
readings were performed by means of a digital pressure gauge, through not simultaneously. In addition, most of the studies show results related
the installation of two pressure points, located at the entrance and exit to batch operations, with mechanical agitation of the thickened sludge
of the HTF. samples, shown in Table 1.
Several authors [11,15,18–22] consider HTFs a better flake forma- The conditioning with polymers aims to aggregate the suspensions,
tion with reduced detention time. Thus, there is greater efficiency in the enabling the separation by filtration in a built static thickener, while the
liquid/solid separation step, resulting in a clarified with less turbidity. application of acid aims the recovery of coagulant and aid in floccu-
In addition, the use of hydraulic mixing in the tubular system alleviates lation.
the possibility of dead zones or short circuits common in mechanical
agitation units [15,21,23]. Another advantage of using the Helical Table 1
Tubular Reactor in flocculation aggregation over conventional hy- Results of coagulant recovery studies by sludge acidification using mechanical
draulic systems is the minimization of flake rupture that can occur in mixing.
compartmentalized flocculators, also called chicanes. Due to changes in Type of sludge Acid Solids Time (s) Ion Ref.
the direction of liquid mass passing through the various chambers, local g·L−1 recovery
increases in the velocity gradient tend to occur, which may lead to the Mechanical Settling (%)
mixing
disintegration of the previously formed flakes. In addition, some au-
thors [23,24] point to the reduced cost of installation and operation of Dry sludge H2SO4 10 1800 900 74 [30]
these flocculation units compared to conventional systems, and con- Dry sludge H2SO4 10 1200 73.8 [31]
ventional coagulation and flocculation aggregation can be performed Dry sludge H2SO4 200 7200 7200 100 [39]
Dehydrated H2SO4 20–40 86,400 70 [38]
simultaneously on the same unit.
sludge
Another form of chemical sludge conditioning occurs by the addi- Dry sludge H2SO4 1800 83 [40]
tion of acids, alkalis, oxidizers, surfactants and other chemical or

2
M. Maraschin, et al. Separation and Purification Technology 252 (2020) 117417

In general, the proposed technique investigates the unification of the incorporation of the homogenized sludge at 5 g·L−1 of total solids
steps in the treatment of WTP sludge, which uses some type of coagu- (TS). The raw sludge was fed to the HTF by mechanical pumping, and a
lant, aiming at its volumetric reduction aided by the aggregation, rotameter was installed for flow control. Application of the reagents
thickening and recovery of the coagulant. was initiated with H2SO4, followed by polymers P 2900 and P 22, ac-
cording to a preliminary study that indicated improvement in treatment
2. Material and methods within the presented order of application of the polymers. The reagent
dosages used were performed automatically by peristaltic pumps.
2.1. Characterization of sludge The solids were separated from the clarified water at the end of
flocculation using a built-in static thickener. The separation device had
The sludge used in this study was supplied by WTP São Gabriel a filtering area of 0.11 m2 and a permeability of 0.4 m3·s−1. The use of
Saneamento, located in southern Brazil. The station operates by means the thickener allowed the clarified water and the thickened sludge to be
of the conventional treatment of water collected in a dam installed on collected, in which the recovery of aluminum ions was evaluated. For
the Vacacaí River, which uses polyaluminium chloride (PAC) as a comparison with the results obtained with the filtration thickening,
coagulant agent in its treatment. Removal of most of the waste takes flocculated and acidified sludge have been collected in the HTF and
place in two settling basins. submitted to the sedimentation thickening. Utilized parameters: SRF,
In the experimental development, sludge samples from the settling based on the classical filtration theory [36], and the TS in the thickened
basins of the same batch have been used. During the tests, the TS sludge [37].
concentration was maintained at approximately 5 g·L−1. In this con-
dition, approximately 90% of the solids were in suspension, and the 2.3. Recovery of aluminum ions
inert fraction made up 75% of the total.
Energy dispersive spectroscopy (EDS) analysis demonstrated the Fig. 5 illustrates the coagulant recovery system by the proposed
material elemental composition at the following percentages: O system.
(69.25%); Si (15.14%);Al (10.86%); Fe (3.78%); Mg (0.38%); K The new coagulant recovery system aims to integrate this unitary
(0.35%) Ti (0.24%). Whereas the results of the analysis by X-ray operation with the addition of flocculants polymers. The combination
Fluorescence (XRF), for major oxides, are listed in Table 2. of these processes (acidification and flocculation), in the same mixing
Altogether, the results by EDS and XRF indicate the mineral for- stage, aimed to simplify this interaction in the sludge volumetric re-
mation of the sludge in study with predominance of clay-mineral kao- duction (thickening) and in the recovery of Al ions, which form the
linite, whose chemical composition is expressed by Al4(Si4O10)(OH), coagulant used by WTP.
and its predominant theoretical composition given by Al2O3 (39.50%) The determination of aluminum concentrations in the obtained
and SiO2 (46.54%), where variations could be found [35]. These results samples was performed by an atomic absorption spectrometer (AAS).
are in agreement with the analysis of the micro structure of the solids Total quantification in the 5 g·L−1 of TS sample has been performed
performed by scanning electron microscopy (SEM) (Fig. 3), which after acid digestion and further analysis. The recovery of the Al ions
showed a predominance of hexagonal lamellar plates, common to the occurred in the continuous flocculation and thickening system, and the
kaolinite form. recovery efficiencies have been analyzed in the thickened sludge and
clarified water.
Some studies [30,31,38–40] directed to this theme evaluate the
2.2. Equipment and reagents
recovery of the coagulant-forming ions used by WTPs through acid-
ification of dry or dehydrated sludge. However, this pilot scale proce-
The built HTF featured 12 m of 1.25 cm diameter flexible tubing,
dure, implemented in a sludge treatment unit at the WTP, would offer
wrapped in a 10 cm diameter polyvinyl chloride (PVC) column. The
complex operations, since these residues would need stabilization for
selection of the flocculator occurred after studies with different lengths
acid application. After this procedure, it would require new steps of
of flexible tubing, in addition to other geometric parameters, such as
water removal for use or disposal of solid waste, increasing its final
torsion and curvature. Details of the HTF selection used in this study are
costs.
described by Maraschin et al. [22].
As a result, sludge treatment is simplified when the coagulant re-
The reagents employed were: low charge density Novaflok P 2900
covery step is programmed in parallel with the removal of water, since
cationic polymer, medium charge density anionic Novaflok P 22 and
the same unit used for flocculation aggregation is simultaneously re-
sulfuric acid (H2SO4) at 3.0 N. Polymer applications have been per-
sponsible for acid dispersion, which leads to sludge pH decrease and
formed by means of dual flocculation mechanism when two polymers
thus the solubilization of the ions present in the coagulant.
were applied in a short time [28]. Stoichiometric and alternating ratios
were set at 1:1 at the following concentrations: 2.5 mg·pol. (g·TS)−1;
3. Results and discussion
3.0 mg mg·pol. (g·TS)−1; 4.0 mg·pol. (g·TS)−1; 5.0 mg·pol. (g·TS)−1;
7.5 mg·pol. (g·TS)−1 e 12.5 mg·pol. (g·TS)−1. All applications for
3.1. Flocculation study
polymer dosage selection have been carried out with acidified sludge at
pH 2.
The addition of acid to the sludge facilitated the aggregation of solid
The constructed hydraulic circuit (Fig. 4) consists of a reservoir for
particles at combined dosages of P 2900 and P 22 polymers from 2.5 to
5.0 mg pol. (g·TS) −1, as shown in Fig. 6. The results showed that the
Table 2
Quantitative analysis of oxides by XRF.
lower polymer use was sufficient to reduce clarified water turbidity,
compared to the results obtained in essays without acidification. Thus,
Oxide Measurement (mg·g−1) Oxide Measurement (mg·g−1) the combination of pre-treatments by flocculation and acidification
SiO2 336,934 P2O5 3,582 mutually contribute to improving the sludge treatment.
Al2O3 268,000 CaO 2,873 The HTF used was formed by 32 rings, beginning from the entrance
Fe2o3 75,555 Na2O 1,549 of the polymer and acid conditioned sludge mass, and we observed the
K2O 8,146 MnO 0,608 effective formation of the flake mass at the twelfth ring, as shown in
TiO2 6,528 BaO 0,439
Fig. 8.
MgO 5,948 ZnO 0,184
SO3 4,085 ZrO2 0,153 The increase in turbidity, recorded in Fig. 6, was due to the increase
in the amount of polymers applied to the system. This increase from the

3
M. Maraschin, et al.
Fig. 3. Photomicrographs of solids present in WTP sludge.
Fig. 4. Experimental scheme of sludge treatment and coagulant recovery: (1)
effluent tank; (2) feed pump; (3) rotameter; (4) sulfuric acid metering pump; (5)
polymer metering pumps; (6) HTF; (7) static thickener; (8) clarified water re-
servoir; (9) thickened sludge.
individual dosage of 4.0 mg pol. (g·TS)−1 of polymers P 2900 and P 22
in acid sludge (pH 2) is mainly due to the mechanism that tends to
restore the particles to their suspended state, the “effect of re-
stabilization”. This effect arises from the excess of polymer chains,
which start to act contrary to the aggregation mechanism. As a result,
the suspended particles surface remains covered with flocculant, re-
sulting in the recovery of the stability of the suspension [3,41,42].
Thus, it has been shown that the application of acid leads to a decrease
Fig. 5. Coagulant recovery system by the proposed system.
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Separation and Purification Technology 252 (2020) 117417
Fig. 6. Residual turbidity of clarified water after acidification. Experimental
conditions: Initial turbidity: 1280 NTU; Sludge: 5 g·L−1; Q: 3 L·min−1; T: 25 °C;
P 2900 and P 22 Polymers; pH acidified: 2 ± 0,39 and pH gross: 6.5 ± 0.011.
in the repulsive forces acting between the particles in the suspension,
which tend to be neutralized with the application of the flocculating
agent [5,11,43]. However, the decrease in pH acts similarly to the ac-
tion promoted by a coagulant, leading to a rapid solid/liquid separa-
tion, which leads to the smaller volume of flocculant to be applied.
Fig. 7 exemplifies the action of decreasing and increasing pH in crude
sludge samples without polymer conditioning.
In addition, the hydrodynamic conditions used in the mixture in the
continuous system can be inferred. Thus, the individual and combined
dosing of polymers P 2900 and P 22 at dosages of 3.0 mg pol. (g·TS)−1
proved to be more efficient in reducing turbidity.
We observed, from within the operation performed, the emergence
of a differentiated G during the flow of the sludge mass inside the HTF.
M. Maraschin, et al. Separation and Purification Technology 252 (2020) 117417

Fig. 7. Alteration of the suspended particles equilibrium at different pHs. Experimental conditions: Initial turbidity: 1280 NTU; Sludge: 5 g·L−1; V: 100 mL; T: 25 °C;
pHinitial: 6.65 – Sedimentation time: 10 min.

Fig. 9. Solids content in acidified sludge and added by filtration and sedi-
mentation. Experimental conditions: Initial turbidity: 1280 NTU; Sludge: 5 g/L;
Q: 3 L·min−1; T: 25 °C; Polymer P 2900 and P 22: 3 mg pol. (g·TS)−1 and
pHinitial: 6.5.

Fig. 8. Flocculation in HTF. TS: 5 g·L−1; V: 1.2 L (reactor volume); Q:

3 L·min−1.

In the first few rings the degree of mixing was high, decreasing in in-
tensity alongside the flocculator. According to Jarvis et al. [44] the
hydraulic flow in helical pipes generates large vortices, responsible for
low energy dissipation and consequently an ideal degree of agitation for
aggregation of solid particles present in the effluent. However, there is
also the establishment of smaller vortices that result in greater energy
dissipation, required for effluent and polymer dispersion.
The data shown in Fig. 8 indicate the best energy distribution pro-
vided by the double vortex, that is, smaller vortices at the beginning of
the flow capable of leading the best dispersion between the sludge and
polymers, dissipation energy, and consequently, lower occurrence of
flake rupture.

3.2. Thickening of sludge

The main changes in the thickened sludge TS occurred at extremely
low pHs (Fig. 9), where the TS of 21.8% for pH 1 and 20% for pH 2 have
been recorded, both for filtration thickening. For the other treatments
no significant differences have been found among the means of the TS
at the 5% significance level.
For the sedimentation thickening during 30 min, the pH decrease
also helped to increase the density of the thickened sludge. In the so-
lution at pH 1, the sludge was collected with 8.5% TS, and at pH 2 to
8%, the other treatments maintained levels below 8% for TS.
Essays in order to evaluate the filterability of sludge after acid-
ification (Fig. 10) showed that decreasing pH favors the release of
water, which leads to a material that is more easily dehydrated. De-
creasing the sludge pH from 6.5 to 2 allowed a greater than 50% de-
crease in SRF for both thickening systems. According to Li et al. [34]
Fig. 10. Resistance specifies the filtration of acidified and thickened sludge.
Experimental conditions: Initial turbidity: 1280 NTU; Sludge: 5 g·L−1 (TS:
0.5%); T: 25 °C; Polymer P 2900 and P 22: 3 mg pol. (g·TS)−1 and pHinitial: 6.5.
acidification is the main pretreatment responsible for decreasing the
SRF of aluminum salt conditioned sludge.
3.3. Coagulant recovery
Digestion of the 5 g·L−1 crude sludge sample and analysis by atomic
absorption spectroscopy resulted in a concentration of 510,06 mg·L−1
of Al ions. From within this concentration, the tests have been per-
formed and the results were presented in terms of the recovery effi-
ciency of the coagulant.

5
M. Maraschin, et al.
Fig. 11. Effect of pH and flocculation on Al ions recovery. Experimental con-
ditions: Initial turbidity: 1280 NTU; Sludge: 5 g·L−1; Polymer P 2900 and P 22:
3 mg pol. (g·TS)−1; pHinitial: 6.5 ± 0.083 and Q: 3 L·min−1.
3.3.1. Effect of pH change
The greatest Al recovery occurred at pH 2 (Fig. 11). Hydraulic and
hydrodynamic conditions used in flocculation operation (laminar to
turbulent transition regime - Reynolds number (Re): 5046; G: 507 s−1
and hydraulic holding time (t): 24 s) allowed for an efficient degree of
energy in the mixing of the reagents, however, it was not possible to
achieve high level of coagulant recovery in the clarified water after
filtration in the static thickener.
In all operations, the reduced time (24 s) for contact between solid
particles and acid was not sufficient for solubilization of Al ions in the
clarified water filtered by static thickener. The largest recoveries oc-
curred in the clarified water of the thickened sludge after 30 min of
sedimentation. However, the sum between the percentages of recovery,
aided by flocculation, (clarified water filtered in the thickener and
clarified formed in the thickened sludge) reached satisfactory levels. At
pH 2 these recoveries resulted in approximately 90% of Al ions.
3.3.2. Volumetric reduction of sludge
The high solubilization of Al in acid medium tends to result in vo-
lumetric sludge decrease. Fig. 12 shows the percentages of sludge vo-
lume reduction under three conditions: thickened, flocculated and raw
sludge without polymer addition.
Fig. 12. Volumetric reduction of sludge under acidification. Experimental
conditions: Initial turbidity: 1280 NTU; Sludge: 5 g·L−1; Polymer P 2900 and P
22: 3 mg pol. (g·TS)−1; pHinitial: 6.5 ± 0.083 and Q: 3 L·min−1.
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Separation and Purification Technology 252 (2020) 117417
Fig. 13. Relationship between the reduction of TSS in the clarified water and
the amount of dissolved Al. Experimental conditions: Sludge: 5 g·L−1; Q: 3
L·min−1; TSS: 4440 ± 17.12; pHinitial: 6.5 ± 0,083; without flocculation.
The sludge volume reduction is favored at low pH, in the tests
performed the largest volumetric reductions occurred with the raw
sludge, without addition of polymer, however, the flocculated sludge
presented lower results due to flake formation, requiring a longer time
for flocculated sludge compression. For the thickened sludge the lower
values were justified by the higher solids loading in the samples (ap-
proximately 18%) due to the filtration in the static thickener.
Fig. 13 shows that the dissolution of Al from the clarified sludge
indicates a strong correlation between this variable and the reduction of
Total suspended solids (TSS) in the sample. The results showed that at
pH 2 ± 0.023 there was a reduction greater than 4000 mg·L−1 of
crude sludge TSS, obtaining the highest level of solubilized Al ions
(448 mg·L−1).
3.3.3. Effect of feeding rate
The feed rate, with subsequent change in the degree of mixing,
showed no significant change in the recovery of Al ions (Fig. 14), even
from a transition regime from the rate of 3 L·min−1 to the turbulent
regime in the 6 and 9 L·min−1 flow rates. The hydraulic and hydro-
dynamic parameters involved in this step are presented in Table 3, and
Fig. 14. Effect of feeding rate Experimental conditions: Initial turbidity: 1280
NTU; Sludge: 5 g·L−1; Polymer P 2900 and P 22: 3 mg pol./g TS; pH:
2.0 ± 0.03.
M. Maraschin, et al.
Table 3
Hydraulic parameters involved in the mixture in the HTF.
Parameter Operational Feed Rate (L·min−1)
3.0 6.0 9.0
hf (m) 0.67 2.85 5.89
t (s) 24 12 8
G (s−1) 507 1521 2597
G.t 12,168 18,252 20,776
V (m·s−1) 0.41 0.82 1.22
Re 5046 10,092 15,138
consist of the head loss (hf) measured through a digital pressure gauge
connected to inlet and inlet pressure-taking devices and at HTF output,
Camp number (G.t) and net mass velocity in HTF (V), as well as G, t and
Re.
We observed that the contact time between the reagents and the
effluent had the greatest influence, considering that the clarified water
obtained at the feeding rate of 3 L·min−1 generated a recovery greater
than 50% compared to the obtained at the 9 L min−1 rate, since in the
first condition the holding time of the net mass in the reactor was 16 s
longer.
We can observe from the data obtained and described in Table 1
that the mechanical mixing time between sludge and acid was over
1000 s, with variable resting time. In the developed study the recoveries
were performed with mixing time less than 25 s (Table 3) and a settling
of 1800 s, nevertheless, ideal conditions were reached for the procedure
performed with lower mixing energy costs.
4. Conclusion
The system involving flocculation and acidification pretreatments
applied in the treatment of WTP sludge proved to be efficient. The
application of H2SO4 acid during flocculation allowed a reduction in the
dosage of polymers, coupled with the reduction of turbidity in the
clarified water, with unit dosages of the cationic and anionic polymers
of 3.0 mg pol. (g·TS)−1. The acidifier reduces the dosage of polymers,
and it can be elucidated due the neutralization of the repulsive forces
among the particles of the sludge. Another characteristic benefited by
the developed treatment was the thickening, there were significant
reductions in the SRF of the thickened sludge mass with increase in TS.
Compared to the widely reported flocculation processes, the hy-
draulic mixing in the HTF allowed for the dispersion of sludge reagents
efficiently and with reduced contact time. In addition, we present a
system that contributes to the high cost reduction that involves the
treatment of these sludge waste reagents. The operational condition of
the proposed hydraulic mixture (G: 507 s−1 and t: 24 s), and in an
acidic situation (pH: 2), made it possible to recover approximately 90%
of the Al ions in the raw sludge.
Finally, the recovery of Al ions benefited from the simultaneous
execution of pre-treatments, however, the greater recovery must be
related to a longer time for contact and solubilization of these ions,
given the larger recoveries made in the thickened sludge, zone where
the presence of about 71% of Al ions was verified, compared to ap-
proximately 15% of these ions in the clarified water obtained from the
filtration operation at a contact time of 24 s in the FTH.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
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Separation and Purification Technology 252 (2020) 117417
Acknowledgements
This work was supported by the Coordination for the Improvement
of Higher Education (CAPES, in Portuguese, Coordenação de
Aperfeiçoamento de Pessoal de Nível Superior); and the São Gabriel
Water Treatment Plant/SOLVI for the WTP sludge samples.
References
[1] R.-F. Yu, On-line evaluating the SS removals for chemical coagulation using digital
image analysis and artificial neural networks, Int. J. Environ. Sci. Technol. 11
(2014) 1817–1826, https://doi.org/10.1007/s13762-014-0657-1.
[2] S.R. Teixeira, G.T.A. Santos, A.E. Souza, P. Alessio, S.A. Souza, N.R. Souza, The
effect of incorporation of a Brazilian water treatment plant sludge on the properties
of ceramic materials, Appl. Clay Sci. 53 (2011) 561–565, https://doi.org/10.1016/
j.clay.2011.05.004.
[3] R. Yang, H. Li, M. Huang, H. Yang, A. Li, A review on chitosan-based fl occulants
and their applications in water, Water Res. 95 (2016) 59–89, https://doi.org/10.
1016/j.watres.2016.02.068.
[4] M. Sillanpää, M.C. Ncibi, A. Matilainen, M. Vepsäläinen, Removal of natural organic
matter in drinking water treatment by coagulation: A comprehensive review,
Chemosphere 190 (2018) 54–71, https://doi.org/10.1016/j.chemosphere.2017.09.
113.
[5] C. Oliveira, J. Rubio, A short overview of the formation of aerated flocs and their
applications in solid/liquid separation by flotation, Miner. Eng. 39 (2012) 124–132,
https://doi.org/10.1016/j.mineng.2012.05.024.
[6] S. Byun, J. Kwon, M. Kim, K. Park, S. Lee, Automatic control of polymer dosage
using streaming potential for waterworks sludge conditioning, Sep. Purif. Technol.
57 (2007) 230–236, https://doi.org/10.1016/j.seppur.2007.03.009.
[7] C.S. Lee, J. Robinson, M.F. Chong, A review on application offlocculants in was-
tewater treatment, Process Saf. Environ. Prot. 92 (2014) 489–508, https://doi.org/
10.1016/j.psep.2014.04.010.
[8] M. Anjum, N.H. Al-makishah, M.A. Barakat, Wastewater sludge stabilization using
pre-treatment methods, Process Saf. Environ. Prot. 202 (2016) 615–632, https://
doi.org/10.1016/j.psep.2016.05.022.
[9] R. Clarke, D. Peyton, M.G. Healy, O. Fenton, E. Cummins, A quantitative risk as-
sessment for metals in surface water following the application of biosolids to
grassland, Sci. Total Environ. 566–567 (2016) 102–112, https://doi.org/10.1016/j.
scitotenv.2016.05.092.
[10] M.T. Nalbantcilar, S.Y. Pinarkara, Public health risk assessment of groundwater
contamination in Batman, Turkey, J. Water Health 14 (2016) 650–661, https://doi.
org/10.2166/wh.2016.290.
[11] E. Carissimi, D.G. Sanagiotto, E.B. Cama, Revisiting coiled flocculator performance
for particle aggregation, Water Environ. Res. 90 (2018) 322–328, https://doi.org/
10.2175/106143017X14902968254935.
[12] J. Yang, S. Chen, H. Li, Dewatering sewage sludge by a combination of hydrogen
peroxide, jute fiber wastes and cationic polyacrylamide, Int. Biodeterior. Biodegrad.
(2016) 1–7, https://doi.org/10.1016/j.ibiod.2016.10.027.
[13] W. Zhang, P. Xiao, Y. Liu, S. Xu, F. Xiao, Understanding the impact of chemical
conditioning with inorganic polymer flocculants on soluble extracellular polymeric
substances in relation to the sludge dewaterability, Sep. Purif. Technol. (2014),
https://doi.org/10.1016/j.seppur.2014.05.034.
[14] L. Jin, P.-Y. Zhang, G. Zhang, J. Li, Study of sludge moisture distribution and de-
watering characteristic after cationic polyacrylamide (C-PAM) conditioning,
Desalin. Water Treat. 57 (2016) 29377–29383, https://doi.org/10.1080/
19443994.2016.1144085.
[15] E. Carissimi, J. Rubio, Polymer-bridging flocculation performance using turbulent
pipe flow, Miner. Eng. 70 (2015) 20–25, https://doi.org/10.1016/j.mineng.2014.
08.019.
[16] E. Carissimi, J. Rubio, The flocs generator reactor-FGR: a new basis for flocculation
and solid – liquid separation, Int. J. Miner. Process. 75 (2005) 237–247, https://doi.
org/10.1016/j.minpro.2004.08.021.
[17] A. Grohmann, M. Reiter, U. Wiesmann, New flocculation units with high efficiency,
in: Water Sci. Technol., Water Science Tecnology, 1981, pp. 567–573.
[18] S. Vigneswaran, T. Setiadi, Flocculation study on spiral flocculator, Water Air Soil
Pollut. 29 (1986) 165–188, https://doi.org/10.1007/BF00208407.
[19] K. Yamamoto, S. Yanase, R. Jiang, Stability of the flow in a helical tube, Fluid Dyn.
Res. 22 (1998) 153–170, https://doi.org/10.1016/S0169-5983(97)00032-4.
[20] K. Yamamoto, A. Aribowo, Y. Hayamizu, T. Hirose, K. Kawahara, Visualization of
the flow in a helical pipe, Fluid Dyn. Res. 30 (2002) 251–267, https://doi.org/10.
1016/S0169-5983(02)00043-6.
[21] J. Gregory, Polymer adsorption and flocculation in sheared suspensions, Colloids
Surf. 31 (1988) 231–253, https://doi.org/10.1016/0166-6622(88)80196-3.
[22] M. Maraschin, K.F. Soares Hedlund Ferrari, A. Paolla Hubner da Silva, E. Carissimi,
Aluminum Sludge thickening: Novel helical pipes for aggregation by dual floccu-
lation and thickening by filtration applied to water treatment plants, Sep. Purif.
Technol. (2020), https://doi.org/10.1016/j.seppur.2020.116560.
[23] E. Carissimi, J.D. Miller, J. Rubio, Characterization of the high kinetic energy dis-
sipation of the Flocs Generator Reactor (FGR), Int. J. Miner. Process. 85 (2007)
41–49, https://doi.org/10.1016/j.minpro.2007.08.001.
[24] J. Luo, Y. Luo, G. Chu, M. Arowo, Y. Xiang, Micromixing ef fi ciency of a novel
helical tube reactor: CFD prediction and experimental characterization, Chem. Eng.
Sci. 155 (2016) 386–396, https://doi.org/10.1016/j.ces.2016.08.010.
M. Maraschin, et al.
[25] Y. Chen, H. Yang, G. Gu, Effect of acid and surfactant treatment on activated sludge
dewatering and settling, Water Res. 35 (2001) 2615–2620, https://doi.org/10.
1016/S0043-1354(00)00565-0.
[26] J. Guo, J. Ma, Bioflocculant from pre-treated sludge and its applications in sludge
dewatering and swine wastewater pretreatment, Bioresour. Technol. 2 (2015) 3–7,
https://doi.org/10.1016/j.biortech.2015.07.113.
[27] R. Guan, X. Yuan, Z. Wu, H. Wang, L. Jiang, Functionality of surfactants in waste-
activated sludge treatment: A review, Sci. Total Environ. 609 (2017) 1433–1442,
https://doi.org/10.1016/j.scitotenv.2017.07.189.
[28] H. Wei, P. Hu, A. Li, H. Yang, Evaluation of acidification and oxidation of sludge to
improve the effect of a starch-based flocculant on the dewaterability of sewage
sludge, J. Environ. Manage. 231 (2019) 405–412, https://doi.org/10.1016/j.
jenvman.2018.10.058.
[29] J. Keeley, P. Jarvis, A.D. Smith, S.J. Judd, Coagulant recovery and reuse for
drinking water treatment, Water Res. 88 (2016) 502–509, https://doi.org/10.1016/
j.watres.2015.10.038.
[30] A.T. Nair, M.M. Ahammed, Influence of sludge characteristics on coagulant re-
covery from water treatment sludge: a preliminary study, J. Mater. Cycles Waste
Manag. 19 (2017) 1228–1234, https://doi.org/10.1007/s10163-016-0513-0.
[31] M.M. Fouad, T.M.A. Razek, A.S. Elgendy, Utilization of drinking water treatment
slurry to produce aluminum sulfate coagulant, Water Res. 89 (2017) 186–191,
https://doi.org/10.2175/106143016X14504669769056.
[32] Y. Lu, G. Zheng, W. Wu, C. Cui, L. Zhou, Significances of deflocculated sludge flocs
as well as extracellular polymeric substances in influencing the compression de-
watering of chemically acidified sludge, Sep. Purif. Technol. 176 (2017) 243–251,
https://doi.org/10.1016/j.seppur.2016.12.016.
[33] M.M. Bishop, A.T. Rolan, T.L. Bailey, D.A. Cornwell, Testing of alum recovery for
solids reduction and reuse, J. Am. Water Works Assn. 79 (1987) 76–83, https://doi.
org/10.1002/j.1551-8833.1987.tb02860.x.
[34] C. Li, J. Lin, S. Kang, C. Liang, Acidification and alkalization of textile chemical
sludge: volume/solid reduction, dewaterability, and Al (III) recovery, Sep. Purif.
Technol. 42 (2005) 31–37, https://doi.org/10.1016/j.seppur.2004.06.001.
Separation and Purification Technology 252 (2020) 117417
[35] A.B. Luz, F.A.F. Lins, Rochas e Minerais Industriais: usos e especificações, second
ed., CETEM/MCT, Rio de Janeiro, 2008.
[36] U. Yukseler, H. Tosun, I. Yetis, A new approach in assessing slurry filterability, J.
Membr. Sci. 303 (2007) 72–79, https://doi.org/10.1016/j.memsci.2007.06.053.
[37] American Public Health Association, AmericanWaterWorks Association,Water
Environment Federation, Standard Methods for the Examination of Water and
Wastewater, 22th ed., American Public Health Association, Washington, D.C, 2012.
[38] P. Prakash, A.K. Sengupta, Selective coagulant recovery from water treatment plant
residuals using donnan membrane process, Environ. Sci. Technol. 37 (2003)
4468–4474, https://doi.org/10.1021/es030371q.
[39] Y.-J. Chen, W.-M. Wang, M.-J. Wei, J.-L. Chen, J.-L. He, K.-Y. Chiang, C.-C. Wu,
Effects of Al-coagulant sludge characteristics on the efficiency of coagulants re-
covery by acidification, Environ. Technol. 33 (2012) 2525–2530, https://doi.org/
10.1080/09593330.2012.679696.
[40] L. Yang, Y. Han, D. Wang, High efficiency aluminum coagulant recovery from
drinking water treatment plant sludge by using ultrasound assisted acidification,
Adv. Mater. Res. 777 (2013) 60–64, https://doi.org/10.4028/www.scientific.net/
AMR.777.60.
[41] V.K. La Mer, Filtration of colloidal dispersions flocculated by anionic and cationic
polyelectrolytes, Discuss. Faraday Soc. 42 (1966) 248, https://doi.org/10.1039/
df9664200248.
[42] Q. Lin, H. Peng, S. Zhong, J. Xiang, Synthesis, characterization, and secondary
sludge dewatering performance of a novel combined silicon – aluminum – iron –
starch flocculant, J. Hazard. Mater. 285 (2015) 199–206, https://doi.org/10.1016/
j.jhazmat.2014.12.005.
[43] J. Ma, K. Fu, L. Jiang, L. Ding, Q. Guan, S. Zhang, H. Zhang, Flocculation perfor-
mance of cationic polyacrylamide with high cationic degree in humic acid synthetic
water treatment and effect of kaolin particles, Sep. Purif. Technol. 181 (2017)
201–212, https://doi.org/10.1016/j.seppur.2017.03.027.
[44] P. Jarvis, B. Jefferson, J. Gregory, S.A. Parsons, A review of floc strength and
breakage, Water Res. 39 (2005) 3121–3137, https://doi.org/10.1016/j.watres.
2005.05.022.