J. Environ. Eng. Manage.

, 19(5), 283-289 (2009)

283

ELECTRO-FENTON-BASED TREATMENTS OF REAL EFFLUENTS FROM

TANNING PROCESSES AND LANDFILLS
Birame Boye,1,* Giancarlo Sandon,1 Monica Giomo,2 Anselmo Buso2 and Giuseppe Farnia1
1

Dipartimento di Scienze Chimiche

Universit degli Studi di Padova
Via Marzolo 1, 35131 Padova, Italy
2
Dipartimento di Principi e Impianti di Ingegneria Chimica I. Sorgato
Universit degli Studi di Padova
Via Marzolo 9, 35131 Padova, Italy

Key Words: Electro-Fenton, photoelectro-Fenton, electroprecipitation, electrocoagulation, tanning

wastewater, percolates
ABSTRACT
Leather industry uses high quantities of water, from 50 to 200 m3 d-1 and tanning processes use
large quantities of tannin-based organic compounds, which with all the protein, lipids, greases and
hairs, constitute high amounts of COD (chemical oxygen demand) and BOD (biological oxygen
demand) with many biorefractory compounds in the tanning effluents. Effective treatment with
recycling option of such large quantities of technological waters would: 1) reduce the costs of the
entire tanning process (as for that of water consumption and that of salt expenses), 2) allow to easily
depurate the issuing waters with lower costs, and 3) eliminate progressively the negative
environmental impact of the final effluent discharge into rivers by reducing considerably (or
eliminating) the remaining COD and the quantities of sludge at the end of the treatment process.
Depuration sludges are usually stocked in specially conceived landfills. Leachate from such
landfills contains also high quantities of contaminants, COD from 5000-15000 ppm, and requires
further treatment. Periodical recirculation of the leachate is done, which, in fact, does not always
suffer subsequent treatment.
The main process presented in this work, H2O2-assisted electroprecipitation (AEP) with
sacrificial Fe anode coupled with Ti(Pt) cathode, combines physico-chemical aspects of the
treatment of water effluents with electro-Fenton(EF)-based electrochemical oxidation and partial
coagulation/precipitation of the remaining compounds. The COD removal is 90% in 8 h for the
desalting wastewater and in the range 60-80% in 6 h for the leachate during AEP treatment. EF and
photoelectron-Fenton on boron doped diamond (BDD) anode coupled with O2-diffusion cathode also
allow high degradation efficiency (75-80%), limited by oxalate-complexes formation and the
presence of suspended solids. BDD anodic oxidation achieves 99% destruction of COD in a longer
time, more than 20 h. AEP treatment, alone or in combination with complementary treatment, allows
complete COD removal from the effluents. The AEP-technology is suitable to industrial application
specially for the recycling of tanning effluents and landfill leachate.
INTRODUCTION
Leather industries are large consumers of water
and are, consequently, sources of potential contamination that must be treated before effluent discharge into
rivers or surface waters; there has been progressive
increase of organic compounds in surface and
groundwater [1-5]. Therefore, regulations are adopted
to avoid the critical contamination.
*Corresponding author
Email: [email protected]

When natural vegetal tanning process was traditionally used, the main problem was to ensure the degradation of the organics. In such case, the effluents
have elevated COD (chemical oxygen demand) and
BOD (biological oxygen demand) value, but are relatively easier to treat biologically. The necessary
treatment allowed the biodegradation of the organic
part at relatively low expenses in the normally accepted range of effluents concentration, value less or

J. Environ. Eng. Manage., 19(5), 283-289 (2009)

284

equal 10,000 ppm of COD. High biodegradability is

illustrated by the high BOD/COD ratios. The higher
the value is the better the effluents are treated via biological depuration processes. Later with the expansion
of the chromium-based tannery process, it appears
necessary to eliminate the heavy metals up to their legally authorized and accepted concentrations. Now the
process has a reinforced use of colorants, which are
nevertheless easy to destroy. Unfortunately, the
wastewater from tanning processes has levels of COD
higher than the recommended limits. Usually, before
biological process begins, the wastewater is subjected
to a flocculation/coagulation step, where an important
part of the contaminants is precipitated. The entering
concentration of COD at the head of the depurator
constitutes an important criterion for the payment, by
the manufacturers, of the corresponding treatment
taxes. Sometimes, COD values can easily attain concentrations up to ten times or more than the normally
accepted one. In modern and intensive processes of
depuration, the mixing of the municipal waters with
those of industrial origin (tannery one, for instance)
permits to lower this concentration up to values near
to the recommended before the conventional depuration process begins. It is noteworthy that a meaningful
dilution is sometimes made during and at the end of
the tanning process justified by cleaning proposes,
even if occasionally such cleaning is exaggeratedly
made to ensure lower COD concentrations in the effluents before their arrival to the entrance of the conventional depuration plant.
One other important aspect of the wastewater
from industrial activities and tanning processes is the
accumulation of the sludge (near 300 kt y-1 for the
studied case). The disposal in controlled landfills

yields large quantities of percolates, from 200 to 500

m3 d-1. The leachate shows high and variable COD
(from 2,000 to 15,000 ppm), low biodegradability index and various heavy metals used during the tanning
and treatment processes (see Table 1). This constitutes
an indication that, in fact, during the wastewater
treatment, the main part of the COD of this wastewater is imprisoned in the sludge and not completely destroyed. So with the recirculation of the derived percolates at the top of depuration plant, the result obtained
is not the destruction of the contamination but mainly
a COD and other contaminants recirculation in the
technological scheme, a fact that makes the lately issuing percolates even more concentrated.
Alternative solutions to the classical chemical,
physico-chemical and biological technologies are
needed and are being investigated to achieve the
treatment of toxic and highly loaded wastewater. Appreciable advances are being done for the practical
application of electrochemical methods to the treatment of real wastewater as reported by others [6,7].
These techniques are allowing the treatment of different wastewater with oil and fat emulsion [8-10], from
galvanoplastic and metal electroplating [11-14], textile and derived [15-19], and alimentary [9] sectors.
We have focused our research on the practical
solutions directly applicable to the wastewater and
landfill leachate, and recently, we have presented the
treatment of highly concentrated effluents from vegetal tanning process [20]. In the present paper, we report the part corresponding to the recycling and treatment of tanning and landfills leachate in the case of
the desalting waters and the percolates by mainly using Electro-Fenton (EF) and photoelectron-Fenton
(PEF), single and H2O2-assisted Electro Precipitation

Table 1. Typical composition of the studied percolates

Components
Halogenated organic solvents
Phenols
Ni
Cd
Pb
Cu
Zn
Mn
Fe total
Cr total
Cr(VI)
Sulfates
Chlorides
N-NH4+
Sulfurs
COD
Conductivity
pH

Unit
g L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
mg L-1
S cm-1

Arzignano tanning pool

< 10
< 10
1.3
1.06
0.7
0.67
< 0.01
< 0.01
< 0.2
< 0.2
< 0.05
0.16
0.19
0.39
0.27
0.27
1.08
1.34
5.7
5.4
< 0.1
< 0.1
355
255
3215
2520
8730
7740
27
51
6600
2200
44700
39000
8.30
7.90

Istranno
< 0.05
5.04

< 0.01
< 0.1
0.25
0.5
0.38
2.6
1.6
< 0.01
324
13034
2387
28
4800
40100
7.48

Boye et al.: EF Tretament of Tanning Wastewater and Landfill Leachate

(EP) - an EF-based process with oxidation of the organic compounds and co-precipitation and coagulation
of the solids together with the residual carbon [20].
This paper emphasizes strongly on industrial scalingup for the treatment of the studied effluents.

285

(iron complexes precipitation) before and at the end of

the process. The treated solutions were decanted or filtrated with a 50-m paper filter to simulate the reutilisation step of the obtained water.
RESULTS AND DISCUSSIONS

EXPERIMENTAL
The studied effluents were obtained from the Arzignano tanning pool of Vicenza (Italy) and from Istrana landfill (Treviso, Italy). Two of the effluents
were from the same Arzignano tanning pool: desalting
wastewater and part of the percolates. The desalting
effluents were of vegetal and/or chromium-based tanning processes origin, obtained from Dani Leather
tanning enterprise (Arzignano tanning pool), and the
percolate waters were from the landfill from the corresponding depuration process of the tanning effluents.
The parameters and characteristics of the percolates
are illustrated in Table 1. They present a darkish
brown or black colour with a very repugnant odour.
The desalting waters have fewer odours and are
accompanied with suspended solids, like hairs, for instance. No pre-treatment was applied prior electrochemical step.
Experiments were performed in a batch undivided laboratory cell with solution volumes of 200,
500 and 750 mL, at room temperature, at current densities 30 mA cm-2. There was no need in adding an
electrolyte support to electrochemically treat the industrial effluents since they presented a sufficient and
specific conductivity (ca. 40 mS cm-1 at 20 C), due in
particular to the high contain of sodium chloride. A 10
cm2-area iron (Steel C40) or BDD (Boron Doped
Diamond) sheet or titanium-platinised (Ti(Pt)) grid as
anode and zirconium sheet or O2-Diffusion electrode
as cathode were used. For H2O2-assisted electroprecipitation (HAEP) method, Ti(Pt)/Fe electrolytic system was used, where Ti(Pt) is cathode and Fe is anode.
The same way, for EF and PEF an O2-D/BDD system
was used and for anodic oxidation (AO), Zr/Ti(Pt) and
Zr/BDD systems were used. An 8 W Philips black
light lamp tube was used to irradiate the solution under treatment during PEF. COD measurements were
carried out with a HACH DR2000 spectrophotometer
prior heating of the probe-filled Hach digestive vials
with a thermo-reactor at 150 C for 2 h. The influence
of possible trace of hydrogen peroxide after reaction
was primarily eliminated after verification of its presence in the probe with a Ti(IV) complexation solution
and a spectrophotometer at 420 nm [21]. A calibration
curve allowed determining the contribution of the remaining hydrogen peroxide in the COD value. All the
probes were filtrated with a 0.45-m Whatman paper
before COD determination. A 35% Fluka-made hydrogen peroxide solution was used for HAEP. 96%
H2SO4 and 40% NaOH solutions, all purchased from
Fluka, were used for pH adjustment and neutralization

Tanning macromolecules usually present good

complexing capacity with metals, specially iron-based
one or Fe(II) and (mostly) Fe(III) ions [20,22], as illustrated in reactions (1) and (2). The formed iron
complexes are electro active [20] and the addition/generation in the medium of an oxidant as oxygen
or hydrogen peroxide allows the reaction between the
oxidant and the iron complexes (reactions 3-6). The
result obtained is the partial mineralization of the organic pollution (reactions scheme (7)) accompanied
by coagulation of the remaining carbon under ferrioxalate red precipitate complex, which is mainly Fe(III)
with very low percentiles of carbon [20,23] and can be
accordingly transformed into iron during metallurgical
processes. The series of reactions illustrated hereby
are an extension of the Haber-Weiss mechanism [24]
(reactions (3)-(4)) accompanied with the Fenton and
Fenton-like reactions (reactions (5)-(6)) and the organic part (L) complementary oxidation (Lox) up to
mineralization (CO2 + H2O):
Fe (II) + L Fe (II) L

(1)

Fe (III) + L Fe (III) L

(2)

Fe (II) L + O 2 Fe (III) L + O 2

(3)

Fe (II) L + O 2 + 2H + Fe (III) L + H 2 O 2

(4)

Fe (II) L + H 2 O 2 Fe (III) L + OH + OH

(5)

Fe (III) L + H 2 O 2 Fe (II) L + HO 2 + H +

(6)

L+ OH L OX + OH ... CO 2 + H 2 O

(7)

The desalting waters of initial concentration ca.

15,000 ppm of COD were treated via HAEP at initial
pH 7.5 and also adjusted to 3, to be in the range of the
EF process [25-27], with the addition of ca. 1 vol% of
hydrogen peroxide. The cell used had a volume of 500
mL. As illustrated in Fig. 1, when the desalting waters
are treated at initial pH 7.5, COD removal is high but
the final solution has a yellowish colour. Treatment
under pH values 3-4 permits the complete elimination
of the COD and the remaining solution is transparent
and colourless after neutralisation. It is noteworthy
that the transparent appearance of the solution is obtained early after 1 h of oxidation and decantation.
One other important aspect, which might be taken in
consideration when doing scaling-up projection, is
that electrolysis is accompanied by the presence of
large quantities of foam, from 0.1 to 2.25 times the

J. Environ. Eng. Manage., 19(5), 283-289 (2009)

286

7000

16000

600

1200

14000

10000

800

5000
400

8000
0
0

6000

Time (h)

4000

2000

2000

1000

4
Time (h)

400
200
0

4
6
Time (h)

3000

4000

Vfoam (mL)

COD (ppm)

12000

COD (ppm)

Vfoam (mL)

6000

0
0

10

12

14

Time (h)

Fig. 1. COD decay during HAEP treatment of the

desalting waters in a laboratory cell of 500 mL,
at ambient temperature and current density of 30
mA cm-2; electrolysis was performed at initial pH
7.5 (----) and pH 3 (). Inset gives the foam
evolution during the process.

initial wastewater volume before completing the first

hour of treatment (See insert in Fig. 1). After this,
foam quantity is low. Foam evolution is also noted
immediately when hydrogen peroxide is added to the
basic solution, enhanced by O2-evolution, when, at pH
3, foam evolution is very low. This foaming phenomenon is due to the presence in the initial wastewater of tensioactive compounds and also to oxygen and
CO2 evolution.
The studied percolates have COD values of 2200,
4800 and 6600 ppm and were obtained from Arzignano tanning pool depuration station (first, third) and
from Istrana landfill (Treviso). Their destruction behaviour is represented in Fig. 2. COD is destroyed to
very low values and when the process is ruled at Fenton pH, the solutions are colourless after neutralisation.
Treated at initial pH (ca. 8), the resulting solutions
present a yellow-reddish colour, afforded to the formation of stable iron complexes involving part of the
organic contaminants.
Percolates effluents generated even more foam
than desalting waters during electrolysis [see inset in
Fig. 2], which is destroyed towards the end of the
treatment. Foam formation must be a parameter to
study and monitor when scaling-up HAEP reactor.
AO- and EF-based treatments were also performed on the highly contaminated leachate. Figure 3a
illustrates the COD decay. During AO on Ti(Pt) coupled to a Zr cathode, after 6 h of treatment, just ca.
20% COD removal is attained. Afterwards COD destructions are low and equal to ca. 30 and 40% respectively after 12 and 22 h of treatment. Performed on
BDD anode under the same conditions, these results
are much better with ca. 50 and 70% of COD destruction respectively after 6 and 12 h. Destruction of

Fig. 2. Evolution of the COD of the percolates during

HAEP (----, ----, , , ) and PEF
() treatments in laboratory cells respectively
of 200 and 750 mL, at ambient temperature and
current density of 30 mA cm-2. Electrolysis was
performed at initial (----, ----) and pH 3 (,
, , ). Inset: foam evolution during
the respective degradation processes trials.

contaminants during single AO is directly dependent

on the anode capacity of discharging the water molecules of the aqueous medium and consequently generating oxidants to oxidize the pollutants. The superiority in potential of oxidation of BDD upon Pt and Ti,
and consequently Ti(Pt) is previously studied and
demonstrated [28]. Due to its high discharge potential,
a higher amount of oxidants is generated on its surface
and the oxidation reactions at the interface mediumelectrode improved. As no catalysis accompanies the
reactions, the process is relatively slow.
Anyway, after 22 h, AO on BDD mineralizes the
organic contaminants with more than 99% COD destruction. Other electrocatalytic trials are represented
in the same Fig. 3a. Catalysis is just based on the action of the Fe(II) electrogenerated in the treated medium. In the case where HAEP is performed with a
sacrificial Fe anode and a Ti(Pt) cathode to electrolyse
the percolate, ca. 60 and 75% in COD destruction are
attained respectively after 6 and 12 h of treatment.
AEP shows better performance in COD destruction
with respect to AO performed with the Ti(Pt)/Zr system (Figs. 2 and 3a). AEP process is faster than AO;
however, a threshold is observed after 5-6 h and the
destruction trend becomes lower. EF and PEF with an
O2-D/BDD system show faster rates of COD destruction than both AEP and AO processes. COD destruction during EF is ca. 55 and 60% respectively after 6
and 12 h and is higher than that of AO with Zr/Ti(Pt).
PEF also improves the rate of destruction observed for
EF. COD destruction is ca. 75 and 80% after 6 and 12
h of treatment, respectively. For the last two processes,

Boye et al.: EF Tretament of Tanning Wastewater and Landfill Leachate

7000
(a)

COD (ppm)

6000
5000
4000
3000
2000
1000
0
600
(b)

Vfoam (mL)

400

200

0
0

10

15
Time (h)

20

25

Fig. 3. Evolution (a) and foam evolution (b) of the COD

of the percolate during various anodic oxidation
and Electro-Fenton treatments in a laboratory cell
of 200 mL, at room temperature, at pH 3-4 and
current density of 30 mA cm-2; (a) () and
() represent anodic oxidation respectively
on Ti(Pt) and BDD anodes with a Zr cathode and
(----,,) represent respectively HAEP
with Fe anode, Electro- and photoelectro-Fenton
on BDD anode trials; (b) () and ()
represent anodic oxidation respectively on Ti(Pt)
and BDD anodes with a Zr cathode and (----,
, ) represent respectively H2O2assisted EP, and Electro- and photoelectronFenton on BDD anode trials.

a stationary state is observed where destruction of

COD is so low that it seems the process has stopped.
Two facts explain this phenomenon. The formation of
iron complex and Fe(III) oxalate (typical of EF [2930]) together with the high quantities of suspended
solids contributes to slower rate. As for the synthetic
wastewater [31-33], PEF achieves more than 95% destruction of the contamination, due to the ability of
UV light to break the iron oxalate bonds and to enhance the Fenton reaction by completing its cycle (reactions (5) and (6)) and by generating more hydroxyl
radicals. This high yield was not observed in the case
of this percolate due to the presence of high contents

287

of suspended solids and also to foam evolution that

both do not permit a deep irradiation of the electrolysed medium.
Foam evolution is observed in all processes and
is more intense in the case where hydrogen peroxide is
added in the medium of HAEP (Fig. 3b). This can be
explained by the fact that during AO just the anodes
discharge potential of the water molecules is used to
generate hydroxyl radicals and to destroy the organic
matters. O2 evolution at the anode and CO2 evolution
from the low mineralization of organics slowly enhance the foaming process. When iron catalyst and
oxidation promoters (hydrogen peroxide and oxygen)
are present in the medium, the anodic destruction of
the contaminants is accompanied by bulk reactions (4)
and (7) that favour the evolution of foam. This latter
progressively dissolves back in the medium and is
oxidized again.
With the good performance obtained with the
destruction of the COD during electroprecipitation,
high degree of metal removal is attained; more than
90% for the reported metals in Table 1, even if their
initial concentrations were very low. Nitrogen is also
eliminated with ca. 70% removal. Phenols and halogenated organic solvents are eliminated from the medium with removal higher than 95%. After neutralization and decantation, the obtained waters are colourless, transparent and can be reused in the desalting
process after filtration. Microbial analyses of the
treated waters showed a bacterial destruction of more
than 99.9% and a good appropriation for its reuse in
the tanning sector. For irrigation use, a subsequent
removal of salts, up to electric conductivity lower than
5 mS cm-1, is necessary.
CONCLUSIONS
Fenton-based electrochemical treatments of real
wastewater from tanning processes and landfills percolates were performed under various experimental
conditions and concentrations. The results obtained
show that EP is suitable for the treatment of tanning
solutions, percolates and consequently industrial effluents, specially at initial pH 3-4. For industrial projections, prevision of foam evolution must be done by
using a cell/wastewater volume-ratio of ca. 3:1 or
foam recirculation must be done from an intermediary
liquefaction reservoir and the obtained liquid sent
ahead to treatment with the raw wastewater. The
treated solutions are transparent, colourless and ready
for use in the same process, specifically in tanning industries, or for agricultural purposes after removal of
the sodium chloride salt up to acceptable value. The
obtained precipitate contains principally iron and nontoxic carbon (principally oxalate), with Fe easily recuperated via metallurgical processes. HAEP followed
by sludge/solids and salt separation is a promising
technology for most sustainable use of waters in a

288

J. Environ. Eng. Manage., 19(5), 283-289 (2009)

closed cycle. Such concept of wastewater treatment

provides an integral treatment of industrial effluents
that has very positive impacts on the environment as it
converges to the zero-wastes approach

9.

ACKNOWLEDGMENTS
The authors acknowledge financial support from
the Ministerio dellIstruzione dellUniversit e della
Ricerca and from the Universit degli Studi di Padua under project number 2002095838_003
(COFIN2002). The precious assistance of Prof. Amara
Ndiaye, Harrisburg, is also acknowledged.
This work is dedicated to the loving memory of
Maam Ndeyy Mbogne Ndoye, 1897-1996 (www.
maamndeyy.org).

10.

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Discussions of this paper may appear in the discussion section of a future issue. All discussions should
be submitted to the Editor-in-Chief within six months
of publication.
Manuscript Received: November 4, 2008
Revision Received: February 2, 2009
and Accepted: February 3, 2009