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Archives of Environmental Protection
Vol. 47 no. 1 pp. 3–9
PL ISSN 2083-4772
DOI 10.24425/aep.2021.136442
© 2021. The Author(s). This is an open-access article distributed under the terms of the Creative Commons Attribution-ShareAlike
4.0 International Public License (CC BY SA 4.0, https://creativecommons.org/licenses/by-sa/4.0/legalcode), which permits
use, distribution, and reproduction in any medium, provided that the article is properly cited, the use is non-commercial, and no
modifications or adaptations are made
Phosphorus removal by microelectrolysis
and sedimentation in the integrated devices
Bartosz Libecki, Tomasz Mikołajczyk*
Department of Chemistry, Faculty of Environmental Management and Agriculture,
University of Warmia and Mazury in Olsztyn, Poland
* Corresponding author’s e-mail: tomasz.mikolajczyk@uwm.edu.pl
Keywords: ZVI, phosphorus removal, microelectrolysis, coagulator
Abstract: This paper presents the results of tests performed on an installation with an aerated microelectrolytic
bed (MEL-bed) and sludge sedimentation. The systems were designed in two versions, differing in the aeration
method, i.e., a mechanically aerated coagulator (MAC) and an automatically aerated coagulator (AAC).
The experiment demonstrated a high (approx. 84%) efficiency of phosphorus removal from a model solution
for both versions. The corroding bed was the source of iron in the solution. In the initial phase aeration method
affected the phosphorus removal rate, flocculation and sedimentation processes. Physical and chemical changes
in the MEL-bed packing were observed.
Introduction
Phosphorus (apart from nitrogen) is the main agent limiting
the eutrophication of water bodies (Sterner 2008; Tarkowska-
-Kukuryk 2013). Restrictive standards concerning the quality
of wastewater discharged into natural water bodies are being
imposed (Gromiec and Gromiec 2010). It is possible to obtain
the assumed permissible concentrations for phosphorus in
wastewater discharged from wastewater treatment plant
after applying either biological dephosphatation or chemical
precipitation methods using coagulants, i.e., aluminium or
iron(III) salts (Gu et al. 2011; Zou and Wang 2017). Chemical
coagulation is also initiated by the dissolution of metals in the
electrocoagulation process after an electric current was applied
to the electrodes (Smoczyński et al. 2014). A source of metals
in the solution may also be a galvanic cell built of electrodes
of steel (anode) and carbon (cathode), immersed in an
electrolyte (Yuan et al. 2009). As a result of microelectrolysis
processes, during the contact of the bed with electrolyte, i.e.,
wastewater, steel corrosion takes place. The high degree of
steel fragmentation guarantees a large specific surface area
of the bed and, thus, a countless number of corrosion spots,
i.e., micro-cells in which cathodic and anodic processes take
place. In the anodic zone, oxidation and the release of electrons
and metal cations take place, while a reduction occurs on the
cathode (Yang 2009). Fe2+ cations released as a result of the
steel bed disintegration are a substrate for further processes
with the production of hydrolysis products, i.e., iron(III)
hydroxycations that are capable of destabilizing colloids
with an opposite charge, and hydroxides that are capable of
adsorbing contaminants (Deng et al. 2013).
The effect of corrosive dissolution of iron in the form of
chips or filings as Fe0 (zero-valent iron – ZVI) for wastewater
treatment has been presented in numerous studies (Sun et al.
2016),which indicate that the most important factors affecting
the rate of corrosion processes include the type and surface
of the steel, the presence of dissolved oxygen, electrolytic
conductivity, the pH and the electrolyte composition.
There are many examples of new wastewater treatment
installations using a microelectrolytic bed to streamline this
process. The ZVI method with a bed in the form of immersed
steel chip packs with the addition of 0.1% Cu was applied for
a full-scale municipal wastewater treatment (Ma and Zhang
2008) to enhance the process. The above was obtained thanks
to higher standard potential of copper compered to iron.
Constant wastewater flow through the steel bed and infiltration
ensured continuous microelectrolysis process and contact with
the electrolyte. The process can be intensified under aerobic
conditions, e.g., as a result of forced aeration of wastewater
with a fine bubble aerator placed below the bed pack (Qin et
al. 2011; Yanhe et al. 2016).
The advantages of this treatment method over the
traditional chemical coagulation may be due to the following:
G Availability of raw materials – the opportunity to utilize
waste materials (steel scrap);
G Elimination of secondary contamination – chemical
coagulation leads to an increase in salinity and a decrease
in the pH value;
G Minimization of the environmental impact – a reduction
in energy and environmental hazards associated with
the production of acidic coagulants (chemical processes
associated with the emission of chemicals into the
4 B. Libecki, T. Mikołajczyk
environment) as well as the storage and transport of
hazardous cargo.
The study aimed to test phosphate removal using
a microelectrolytic bed operating under aerobic conditions
with sludge separation by the sedimentation method at a new
integrated wastewater treatment installation.
Experimental
Description of the devices tested
For the study, two versions of self-made based on a patent
application (Libecki 2018) wastewater treatment coagulators
were tested, one with mechanical aeration (Fig. 1, MAC)
and the other one with automatic aeration (Fig. 2, AAC).
The treatment process was initiated in the reaction tank, at
the bottom of which the microelectrolytic bed (MEL-bed)
was packed in the form of steel chips < 2 mm in size from
unalloyed carbon steel with a weight of 3 g. Steel chips were
initially degreased in 0.1 M NaOH, then rinsed with distilled
water and dried.
The experiment was carried out on a laboratory scale for
a model solution with characteristics provided in Table 1.
150 cm3 of the solution was placed in the outer tank |1| of the
coagulator (Fig. 1 and Fig. 2) and forced with a pump |7| with
a flow rate of 5 cm3/min through a suction flange |8| and the
conduit terminated with a nozzle |9| in the reaction tank |3|
with a capacity of 5 cm3. The aerated solution under pressure
penetrated through the steel bed and, along with the reaction
products, escaped via the holes in the upper part of the reaction
tank into the inner tank |2|. In the inner tank, the first separation
of the post-coagulation sludge suspensions took place, and the
solution overflowed through the upper edge of the tank into
the outer tank |1|. For the MAC coagulator, the solution was
aerated using an aerator |6| with a constant capacity of 5 cm3
air/min. On the other hand, the AAC coagulator was equipped
with a system of perforated PE flanges through which the
solution was cascading.
The arangment of reactors – the total volume of tank (Vt) and
retention time (Tr)
Outer tank |1| (glass cylinder) Vt – 400 cm3, Tr – 21 min;
Inner tank |2| (polyethylene cylinder) Vt – 45 cm3, Tr – 8 min.;
Reaction tank |3| (polyethylene container) 5 cm3, Tr – 60 s;
MEL-bed |4| V – 1,5 cm3, Tr – 18 s.
Analytical methods
Tests of MEL-bed coagulators were carried out using solutions
with and without phosphates (Table 1). During the experiment
without PO4
3- added, the corrosion performance of the steel
bed was analysed by testing for the Fe3+ concentration, pH and
electrolytic conductivity in the solution from the outer tank.
After the completion of the experiment with a phosphate-free
solution, the precipitated sludge was drained (on cellulose
filter paper with pore size 12 mm) and dried at 100°C to
a constant weight. During the test with phosphates added,
the PO4
3- concentration was analysed in the solution from
the outer tank. At 30 min intervals, a sample of the solution
was taken for tests and supplemented with the initial solution.
For the measurements, a pH-meter and a conductometer with
a conductivity probe (HANNA Instruments) were used. The
concentration of Fe3+ was determined using the thiocyanate
colorimetry (quantification limit of this method was on the
level of 0.2 mg Fe3+/dm3), while PO4
3- concentration by the
molybdate method (quantification limit of this technique was
on the level of 0.3 mg) (HACH). Additionally, spectroscopic
characterization and elemental composition of the bed filling
surface were performed by means of Quanta FEG 250 Scanning
Electron Microscope (SEM), equipped with an Energy-
Dispersive X-ray Spectroscopy (EDX) supplement (Bruker
XFlash 5010). EDX tests were carried out at an acceleration
voltage of 12 kV.
Fig. 1. Mechanically aerated coagulator (MAC)
1 – Outer tank, 2 – inner tank, 3 – reaction tank, 4 – MEL-bed,
5 – drain holes, 6 – aerator, 7 – circulating pump, 8 – pump
suction fl ange, 9 – conduit terminated with a nozzle
Fig. 2. Automatically aerated coagulator (AAC)
1 – Outer tank, 2 – inner tank, 3 – reaction tank, 4 – MEL-bed,
5 – drain holes, 6 – aerating rings, 7 – circulating pump,
8 – pump suction fl ange, 9 – conduit terminated with a nozzle
Phosphorus removal by microelectrolysis and sedimentation in integrated devices 5
Results and discussion
Figures 3a and 3b show changes in the solution parameters
during the experiment. In both cases, similar changes, such as
an increase in the pH value and a decrease in conductivity were
observed.
The coagulators were operating in aerobic conditions.
Within the volume of the corrosive bed, the electrolysis process
took place, which can be divided into anodic and cathodic
parts. As a result of the anodic oxidation, Fe2+ ions are released
from the steel. During the cathodic reduction under aerobic
conditions and in a neutral pH, alkalization of the environment
takes place in the carbon inclusion sites:
2Fe − 4e- → 2Fe2+
O2 + 2H2O + 4 e- → 4OH− (Yang et al. 2009).
At the same time, the conductivity decreases probably
due to reactions of the solution components, i.e., hydrolysis
and precipitation, the visible effect of which is the formation
of sediment at the bottom of the inner tank. The inhibition of
conductivity changes after 120 minutes is associated with the
alkalization and the establishment of the chemical equilibrium
of the occurring processes of steel bed dissolution and iron(II)
ion hydrolysis (Sarin et al. 2004; Yang et al. 2017). In a weak
alkaline environment, phosphates are bound by Fe oligomeric
species (El Samrani et al. 2004).
Changes in the iron(III) ions concentration in the
solution in Figs. 4a and 4b indicate the progress of corrosion
processes. An effect of the operation of the system was
the Fe(III) concentration at a level of 2–2.5 mg Fe3+/l for
the MAC system, and 1.5–2 mg Fe3+/l for the AAC. The
mechanical aeration method probably more efficiently
intensifies the electrode processes involving oxygen
reduction by accelerating the bed corrosion and the ferrous
oxidation to ferric hydroxides and oxides (Wei et al. 2011;
Lakshmanan et al. 2009).
After the contact with the corrosion bed, wastewater along
with the iron hydrolysis products was flowing out through
the holes in the upper part of the reaction tank into the inner
container, where the further stage of floccule growth, separation
of easily-settling suspensions and sedimentation took place.
The total weight of sludge in the installation, determined after
6 h of the experiment with no phosphates, came to 4 and 8 mg
for the MAC and AAC, respectively. These results indicate
a high content of a large amount of suspended matter in the
system. Heavy aeration may adversely affect the processes
of floccule growth and fragmentation and problems with the
sedimentation. As a final result, the treatment efficiency may
be limited. Therefore, the technology using a microelectrolytic
bed with aeration should assume the final filtration process.
At the same time, a reduction in phosphate concentration
(Fig. 4) was observed and after 300 minutes of the experiment
reached a value of 4.80 mg PO4
3-/l in both tested systems.
The phosphate removal rate (Vr) changed throughout the
investigations (Fig. 5). In both cases, the value of Vr parameter
was increasing with time till 30th min of the experiment when it
reached its maximum value of 0.40 mg PO4
3-/min for the MAC,
compared to only 0.26 mg PO4
3-/min for the AAC. After 30 min,
the Vr parameter value was progressively decreasing at a different
rate. Consequently, the final effectiveness after 300 minutes of
the experiment was the same for both coagulators. The effect
of aeration may be of fundamental importance to the course of
phosphorus removal kinetics in the initial phase of the process.
The process can proceed as a result of phosphate precipitation in
accordance with the following reaction:
3Fe2+ + 2PO4
3- + 8H2O → Fe3(PO4)2↓,
with the minimum solubility of the precipitated products at pH
of 7–8 (Priambodo et al. 2018). After 30 minutes, the phosphate
Table 1. Characteristics of the model solution
pH Conductivity
mS/cm
HCO3
-
mg/L
Cl-
mg/L
SO4
2-
mg/L
PO4
3-
mg/L
Na+
mg/L
K+
mg/L
Ca2+
mg/L
123456789
7.6 640 122 71 48 30 69 12 40
Fig. 3. Changes in the solution pH and conductivity during the experiment: a – MAC, b – AAC
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6 B. Libecki, T. Mikołajczyk
removal efficiency decreases rapidly at pH of already above 8.
This is associated with the substrate depletion, but also with
the change in process conditions, i.e., an increase in pH and
oxygenation. Under the influence of oxygen, the reactions of
Fe(II) oxidation → Fe(III) and the hydrolysis with Fe(OH)3↓
precipitation are intensified. OH- ions compete with PO4
3- for
Fe3+ ions and, at the same time, sorption processes can proceed
(Li et al. 2009). Smoczyński et al. (2014) found that the
main mechanism of phosphorus removal in the chemical and
electrochemical coagulation processes is the chemical sorption
process (chemisorption); as a result, covalent bonds are formed
between the adsorbate particles and the adsorbent – hydrolysed
metal species surface.
Comparing the bed structure from the SEM/EDX image
before the experiment (Fig. 6a) and after 6 hours of the process
(Fig. 6b), a significant increase in the surface roughness
can be observed. These changes are the effect of the steel
bed dissolution and adsorption of dissolved compounds and
hydrolysis products in the form of incrustation on the surface.
An elementary analysis of the surface granule layer of the bed
before electrolysis (Fig. 7 and Table 2) revealed a composition
typical to carbon steel with a Fe content of approx. 70% and
carbon content of 20% along with the additions of Al and Mn,
and traces of Si and Cu. After the electrolysis process (Fig. 8
and Table 3), the total share of iron and carbon decreased by
approx. 10% and 6%, correspondingly, while the percentage
of oxygen increased by 10%; moreover, trace amounts of
phosphorus, sulphur and calcium appeared.
These results indicate the process of bed oxidation and
dissolution as well as the sorption of solution components,
including phosphorus. Sleiman et al. (2016) demonstrated that
a sand bed with ZVI in its fragmented form was able to adsorb
152 mg P/g Fe during a several-day experiment. It is not clear
how the adsorbed components affect the process efficiency. It
can be assumed that both the blocking of electrolytic sites and
the passivation of the material surface with the production of
Fe oxides could have occurred (Mak et al. 2009). The adsorbed
phosphate ions exhibit anti-corrosion properties and can inhibit
the microelectrolysis process in the bed over a longer period
(Wan et al. 2011; Lai et al. 2012).
Fig. 4. Changes in the phosphate and total iron levels during the tests on reactors: 4a – MAC, 4b – AAC
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Fig. 5. Changes in the phosphate removal rate in reactors during the experiment
Phosphorus removal by microelectrolysis and sedimentation in integrated devices 7
Fig. 7. Elementary analysis of the MEL-bed surface granule before electrolysis process
Fig. 8. Elementary analysis of the MEL-bed surface granule after electrolysis process
Fig. 6. Image of the MEL-bed fi lling surface: a – before, b – after action
Table 2. The elementary composition of the surface granule layer of the bed before electrolysis
Spectrum C O Al Si Mn Fe Cu
12345678
Content % 20.2
± 0.08
5.85
±1.09
0.22
±0.06
0.18
±0.03
7.13
±0.34
69.09
±4.73
0.22
±0.00
Table 3. The elementary composition of the surface granule layer of the bed after six hours of operation
Spectrum C O Al Si P S Ca Mn Fe Cu
12345678912
Content
%
14.01
±4.79
15.5
±7.24
0.22
±0.15
0.15
±0.07
0.88
±1.11
0.12
±0.03
2.23
±1.99
6.6
±1.2
60.22
±11.63
0.11
±0.14
8 B. Libecki, T. Mikołajczyk
Conclusions
The six-hour experiment demonstrated the efficiency of the
microelectrolytic bed in the removal of phosphorus at a level
of approx. 84% for both tested versions of the installation.
The mechanical aeration method accelerated the treatment
process in the initial phase, which lasted for up to 1 hour. In
the first phase of the experiment in the MAC reactor, a higher
Fe3+ concentration and the P removal rate were obtained.
The maximum rate of phosphorus removal was noted in the
30th minute of the experiment and amounted to 0.40 mg
PO4
3-/min for the MAC and 0.26 mg PO4
3-/min for the AAC.
In the following minutes, the process effectiveness decreased
almost to zero at the end of the test. Despite the differences in
the course of phosphate removal kinetics in the initial phase of
tests on both versions of the installation, the final effects of the
treatment were comparable. The total weight of sludge after the
experiment was greater for the AAC, which may indicate that
the intense aeration in the MAC disturbs the aggregation and
sedimentation processes. Based on the analyses performed, it
can be concluded that phosphorus removal occurs due to the
interaction with products of the corroding bed reactions in the
solution and in the bed itself. The results suggest that the new
installation is suitable for supporting wastewater treatment. The
tested technology proved promising, although the experimental
data need to be verified in terms of bed passivation during
a long-term test and tested on a larger technical scale.
Acknowledgments
The results presented in this paper were obtained as part of
a comprehensive study financed by the
University of Warmia and Mazury in Olsztyn, Faculty
of Agriculture and Forestry, Department of Chemistry (grant
No. 30.610.001-110).
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Usuwanie fosforu przez mikroelektrolizę i sedymentację
w zintegrowanych urządzeniach
Streszczenie: W pracy zaprezentowano wyniki testów urządzenia z napowietrzanym złożem mikroelektrolitycznym
(MEL-bed) i sedymentacją osadu. Urządzenie zaprojektowano w dwóch wersjach, różniących się sposobem
napowietrzania. tj.: mechanical aerated coagulator (MAC) oraz automatically aerated coagulator (AAC).
Eksperyment wykazał wysoką ok. 84% skuteczność usuwania fosforu z roztworu modelowego dla obydwu wersji.
Korodujące złoże było źródłem żelaza w roztworze. Sposób napowietrzania miał wpływ na szybkość usuwania
fosforu w początkowej fazie trwającej do 1 h oraz na procesy flokulacji i sedymentacji. Zaobserwowano zmiany
fizyczne i chemiczne wypełnienia złoża MEL-bed.
