Separation and Purification Technology 248 (2020) 117152

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Separation and Purification Technology

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

Vinasse treatment using hybrid tannin-based Coagulation-Microfiltration- T

Nanofiltration processes: Potential energy recovery, technical and economic
feasibility assessment
Yuri A.R. Lebrona, Victor R. Moreiraa, Tatiane P.B. Furtadoa, Selma C. da Silvab, Lisete C. Langea,
⁎
Miriam C.S. Amarala,
a
Department of Sanitary and Environmental Engineering, School of Engineering, Federal University of Minas Gerais, Antônio Carlos Avenue, 6627, Campus Pampulha, MG
31.270-901, Brazil
b
Exact and Technological Science Center, Federal University of Recôncavo da Bahia, Rui Barbosa Street, 710, Center, BA 44.380-000, Brazil

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

Keywords: The sugarcane industry has a relevant contribution in the Brazilian economy. However, the inadequate disposal
Coagulation of vinasse in the fertigation practices has led to environmental issues. Therefore, the current research in-
Economic analysis vestigated the applicability of microfiltration (MF) and nanofiltration (NF), with and without the use of tannin as
Microfiltration an organic coagulant, to treat vinasse. Among the different coagulant concentrations used, 8.0 mg/L was selected
Nanofiltration
as optimum dosage due to greater removal efficiencies. Removal efficiencies for COD, color and ions by MF-NF
Vinasse
and C-MF-NF routes were similar and higher than 90.6%. As floc sizes increased with the coagulant addition, the
Water reclamation
cake layer became more porous and compressible, reducing fouling resistance in MF process. In that sense, back
transport velocity of particles became an important mechanism affecting the membrane fouling. Overall, the NF
permeate quality allows its various uses, such as washing water and cooling water. The combined concentrate
from MF and NF was considered for energy production and fertigation, presenting higher potential for methane
production compared to raw vinasse. MF-NF route was chosen after an economic analysis due to the high
chemical expenditures related to tannin acquisition in the C-MF-NF process. Considering the prices currently
practiced for industrial water acquisition (2.8 US$·m−3), a 3 year would be required for the investment to be
recouped. Moreover, an internal rate of return of 52.3% was obtained, which was higher than the market at-
tractiveness considered. Hence, the economic analysis reassures the MF-NF rout feasibility for vinasse treatment.

1. Introduction demand (COD: 11.925–22.788 mg·L−1), biochemical oxygen demand

Brazil is the world's largest producer of sugarcane, the largest pro-
ducer and exporter of sugar and the second largest producer of ethanol
in the world. The sugarcane industries have a relevant participation in
the Brazilian economy, since they had the second largest GDP among
the agribusiness industries in 2019, generating an income around US$
26.31 billion [1]. However, to obtain ethanol and distilled alcoholic
beverages, liquid waste is generated and the vinasse represents the
largest fraction. For example, in a distillation column operating at
85–90 °C, for each liter of ethanol, approximately 10 to 15 L of vinasse
is produced [2].
The vinasse pollution capacity is about one hundred times greater
than domestic sewage due to its high concentration of chemical oxygen
(BOD: 9.310–19.300 mg·L−1), color, nutrients (N: 598–1,243 mg·L−1,
P: 33.33–111.52 mg·L−1, K: 2,720–4,175 mg·L−1) acidity (pH:
3.90–5.93), corrosivity and toxicity [3,4]. However, the same effluent
that presents a polluting risk has an enormous potential for generating
income and wealth, if properly treated and used.
In Brazil, the most common destination for this effluent is the ap-
plication in soils as fertilizer for sugarcane plantations, due to the high
content of organic matter and nutrients (mainly potassium, but also
magnesium, nitrogen and phosphorus). This application represents the
least expensive and simplest solution to dispose this effluent according
to Brazilian environmental legislation [5]. Moreover, the practice
avoids the use of synthetic fertilizers and water for irrigation. However,
when applied in an unplanned manner, i.e. without pretreatments,

⁎
Corresponding author at: Miriam Cristina Santos Amaral, Department of Sanitary and Environmental Engineering, Federal University of Minas Gerais, Belo
Horizonte, Brazil.
E-mail address: miriam@desa.ufmg.br (M.C.S. Amaral).

https://doi.org/10.1016/j.seppur.2020.117152
Received 2 April 2020; Received in revised form 19 May 2020; Accepted 21 May 2020
Available online 23 May 2020
1383-5866/ © 2020 Elsevier B.V. All rights reserved.
Y.A.R. Lebron, et al. Separation and Purification Technology 248 (2020) 117152

proper caution, supervision, or calculations, it can cause negative im- Table 1

pacts to soil and groundwater mainly due to its high content of K+ and Vinasse physicochemical characterization.
Na+. Parameters Raw vinasse
Sugarcane vinasse concentration is an alternative for the use of this
−1
residue, since it is not possible to dispose all volume of vinasse pro- COD (mg·L ) 29,510 ± 1,126
BOD (mg·L−1) 5,758 ± 523
duced in fertigation practices. The vinasse volume may be reduced by
Color (uH) 4,657 ± 3,458
evaporation or membrane separation processes (MSP), in such way that pH 3.9 ± 0.3
the substances which account for its fertilizing effects will remain in the Conductivity (µS·cm−1) 4,389 ± 890
concentrate. The concentrate obtained in this process may be used as Total solids (mg·L−1) 12,548 ± 1,025
input to produce feedstuff, as fuel to generate energy or as a fertilizer. Total volatile solids (mg·L−1) 9,874 ± 1,102
Total fixed solids (mg·L−1) 2,436 ± 85
Moreover, the vinasse concentration may reduce the transportation
Total nitrogen (mg·L−1) 98 ± 9
costs and broaden the scope of vinasse use. Total phosphorus (mg·L−1) 250 ± 27
MSPs such as microfiltration have been used in many different in- Chloride (mg·L−1) 663 ± 82
dustrial sectors and have also been shown to effectively remove sus- Phosphate (mg·L−1) 108 ± 9
Sulfate (mg·L−1) 588 ± 52
pended solids from vinasse [6,7] offering an alternative to evaporation
Sodium (mg·L−1) 118 ± 37
[7–9]. Microfiltration (MF) is a less energy-intensive process Potassium (mg·L−1) 2660 ± 108
(7–9 kJ·kg−1 H2O removed) compared to the triple-effect evaporation, Magnesium (mg·L−1) 156 ± 208
that requires about 1,300 kJ·kg−1 H2O removed [10]. In a previous Calcium (mg·L−1) 388 ± 89
article [7] the authors evaluated the use of submerged MF module to
concentrate vinasse. Besides the volume reduction, the low potassium
retention combined with a high organic material retention improves the 2. Methodology
potential use of vinasse as an organic fertilizer. The concentrate may
also be used as an organic matter supplement for contaminated soil 2.1. Vinasse sampling
bioremediation or to produce microbial biomass or substrate for bio-
surfactant production. Furthermore, MF permeate has physical–chem- Vinasse samples were collected from a distillery located in the state
ical quality enough to be used as reuse water in cases in which the of São Paulo, Brazil, which produces ethanol from fermentation of su-
water quality standard is less demanding or may be later treated to garcane juice. Collected samples were stored at 4 °C and brought to
supply purified water demands. room temperature before use. The vinasse physicochemical composi-
Nanofiltration (NF) process is a widespread technology to treat the tion is shown in Table 1.
MF permeate towards water reclamation and zero liquid discharge. The
NF membrane was relatively recently introduced for wastewater 2.2. Experimental setup and procedure
treatment and can replace reverse osmosis (RO) in many applications
due to lower energy consumption and higher flux values (20 to 200 The schematic diagram for the laboratory-scale C-MF-NF hybrid
L·m−2·h−1) [11]. MF permeate treatment by NF may allow a permeate system is shown in the Fig. 1.
production with physical chemical quality to meet different water de- The MF module was installed in a 4 L-coagulation/MF tank
mands of the sugar and alcohol industry. equipped with a flat stirrer for mixing condition control. Tannin-based
Coagulation can be integrated to MF-NF processes in order to im- coagulant (KURIFLOCK CL-33) was dosed at concentration of 0.5, 1, 2,
prove MF retention and mitigate membrane fouling. Although dissolved 4, 6 and 8 mg·L−1 under constant stirring of 100 rpm (2 min) followed
organic matter retention by coagulation alone might not be effective, by 40 rpm (10 min) and 10 rpm (10 min) after which microfiltration
the cake layer induced by flocs accumulated on the membrane surface was started. MF was conducted on a commercial submerged membrane
would have positive contribution in soluble organic matter retention module (PAM Membranas LTDA), polyetherimide-based polymer
[12]. Furthermore, the coagulants ability to aggregate organic matter composition with average pore diameter of 0.45 µm, and a filtration
accumulated on the membrane surface contribute to a more porous area of 0.04 m2. In all experiments, the pressure was measured by a
cake layer formation that can be easily removed by physical cleaning manometer and was adjusted by a diaphragm pump equipped with a
[12]. Here it is important to note that better quality MF permeate speed controller. MF was performed at concentrated mode filtration,
contributes to fouling mitigation on the NF process. constant pressure of 0.2 bar, and up to a recovery rate of 60%.
Tannins are mostly vegetal water-soluble polyphenolic compounds Nanofiltration was carried out with the membrane NF90 (Dow Filmtec),
with a molecular weight higher than 500 Daltons. Tannins have ex- which has a molar weight cut-off of 100 Da, average membrane hy-
tensively been used in drinking water and industrial wastewater draulic resistance of 5.8 × 1013 m−1, and rejection of NaCl (2,000 mg/
treatment applications [13–16]. Furthermore, because tannin-based L) and MgSO4 (2,000 mg/L) of 85–95% and 97%, respectively (DOW-
coagulant are biodegradable [17], its application in the vinasse MF FILMTEC™). A needle-type valve was used to adjust the feed flow rate
process offers a greater advantage related to the safe disposal of MF and the trans-membrane pressure. The pressure was measured by a
concentrate in soil. manometer. NF was conducted in a stainless-steel membrane cell with
In this context, the aim of this paper was to evaluate the feasibility 9 cm diameter and filtration area of 63.6 cm2. The flat-sheet commer-
of hybrid tannin-based coagulation-MF-NF (C-MF-NF) process for the cial membranes were properly cut to fit the membrane cell, and a feed
vinasse treatment. Different doses of tannin-based coagulant were as- spacer of 28 mil (25.4 µm) was placed over the membrane to promote
sessed aiming at MF rejection improvement, membrane fouling miti- flow distribution. NF was performed at concentrated mode filtration,
gation and the propose of a sustainable vinasse treatment that allows its constant pressure of 10 bar, feed flow of 144 L h−1 and up to a recovery
reuse. Furthermore, an assessment of the potential energy recovery rate of 60%. The feed temperature was maintained at 20 ± 5 °C using
from raw and treated vinasse and a technical and economic feasibility a chiller.
of vinasse treatment was carried out.
2.3. Analytical methods

The following parameters were measured: COD (5220B), TOC

(5310B – Shimadzu TOC-VCPH analyzer), color (2120B – Hach DR
3900), electrical conductivity (Hanna Conductivity meter HI 9835) and

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Y.A.R. Lebron, et al. Separation and Purification Technology 248 (2020) 117152

Fig. 1. Schematic of the MF-NF bench scale units.

pH (Hanna pH meter) based on the Standard Methods for Examination national environmental company (Eq. (6)).
of Water and Wastewater recommendations [18]. The particle sizer
distribution of raw and coagulated vinasse was measured using Laser (0.05. CEC − Ks ). 3, 744 + 185
VARmax =
Scattering Particle Size Distribution Analyzer (HORIBA - LA-950V2). Kv (6)

2.4. Calculations where CEC (cmolc·dm−3), Ks (cmolc·dm−3) and Kv (kg-K2O·m−3) cor-

respond to the cation exchange capacity, the potassium concentration
The permeate flux ( J , L/h·m2) was calculated according to Eq. (1), in the soil at a depth of up to 0.8 m and the potassium concentration in
in which A (m2) corresponds to the membrane area and QP (L·h−1) to sugarcane vinasse respectively. Considering a dystrophic red latosol,
the feed flowrate. the Ks and CEC values adopted were 0.05 cmolc·dm−3 and 3.23
cmolc·dm−3 respectively [22]. The constant value 3,744 is a correction
J = QP / A (1) factor to convert the potassium concentrations from cmolc·dm−3 to kg
Membrane resistance (Rm ) was calculated as in Eq. (2), in which K per a volume of 8000 m3 (1 ha × 0.8 m). The constant value 185
(m3/m2·s·Pa) is the membrane water permeability and μ (Pa·s) the corresponds to the mass of K2O extracted by the crop per hectare during
water dynamic viscosity at 25 °C. Resistance due to fouling was cal- the harvest.
culated using a resistance in series model as described in a previous The inputs of organic matter into the soil were estimated through
study [4] and Hermia filtration models were fitted to the experimental the applied organic load ( AOL ) according to Eq. (7), where εCOD (0.607;
data to assess fouling mechanism [19,20]. [23]) is the expected COD removal in a anaerobic biodigester and CODv
is the COD (kg·m−3) of vinasse.
1
Rm =
K . μ (25°C) (2) AOL = VARmax . (1 − εCOD ). CODv (7)
Flux total decay (TD ) was estimated after a comparison of the
AOL values were further used to estimate the populations with a pol-
permeate flux at the end of the experiment (Jsd ) and water permeate
luting potential equivalent to sugarcane vinasse (PE ), as indicated by
flux ( Jw ) as in Eq. (3).
Eq. (8).
Jw −Jsd
TD = AOL
Jw (3) PE =
PCCCOD. HP (8)
The rejection or retention efficiency (R%) is an important parameter
in membrane filtration operation processes. It corresponds to the solute where PCCCOD is the sewage average daily per capita contribution of
fraction retained by the membrane and is calculated according to Eq. COD (0.054 kg-BOD·inhab−1·day−1) and HP is the harvesting period
(4), in which Cf (mg·L−1) and Cp (mg·L−1) corresponds to the solute (210 days).
concentration in both feed and permeate stream, respectively. Potential sulfide and carbon dioxide emissions were also estimated
Cf − Cp ⎞ considering the reduction of sulfate into sulfide under anaerobic con-
R (\%) = ⎜⎛ ⎟ × 100 ditions (Reaction (1) and Eq. (9)) and the anaerobic degradation of the
⎝ Cf ⎠ (4) vinasse organic matter into the soil (Reaction (2) and Eq. (10)).
−3
The specific energy consumption SEC (kWh·m of permeate) was
calculated according to Eq. (5). SO42 − + C2 H3 O2− → HS − + 2HCO3− (Reaction 1)

ΔP. QF
SEC = MHS−
3.6 × 106. QP (5) SE = VARmax . SO42 −.
MSO42 − (9)
where W (kWh·s−1) is the rate of work done by the pump, ΔP (N·m−2)
is the pressure difference between the feed pressure and the permeate, where SO42 − (kg·m−3), MHS− , and MSO42 − are the concentrations of sulfate
and QF (m3·s−1) and QP (m3·s−1) are the feed and permeate flow rates, in the vinasse, the molar mass of sulfide and the molar mass of sulfate
respectively. respectively.
The potential use of vinasse in fertigation was also assessed. The
microorganisms
maximum vinasse application into soils rate (VARmax ) was calculated Cx Hy Oz + O2 → CO2 + H2 O + new cells (Reaction 2)
considering the recommendation proposed by CETESB (2015), a

3
Y.A.R. Lebron, et al. Separation and Purification Technology 248 (2020) 117152

MCO2 where ic is the investment rate (equal to 14% in 2018 in Brazil) and DL
CO2 E = VARmax . (1 − β ). BOD . = VAR . (εCOD − β ). CODv .
MO2 max is the design life of the plant (15 years).
MCO2 To calculate Opex the variables capital cost amortization, mem-
MO2 (10) brane replacement, cleaning agent, chemicals, energy requirement and
maintenance were considered. The tannin coagulant cost was con-
where β , MCO2 and MO2 are the COD fraction that is converted into sidered 630.25 US$·ton−1 of tannin. Chemical cleaning and main-
microbial biomass, CO2 and O2 molar mass respectively. tenance costs were estimated at 2 and 5% per year of the initial in-
The production of biomethane can be estimated from the organic vestment cost respectively. Membrane replacement was calculated
load of the substrate and the efficiency of the anaerobic process through considering a membrane lifespan of 3 years. MF and NF membrane
the COD balance, considering sulfate interference as a potential in- costs were considered as 40 and 21 US$·m−2 respectively, price pro-
hibitor of methanogenic archaea activity due to the growth of sulfate vided by a large commercial membrane supplier in Brazil. Energy re-
reducing bacteria (SRB). Then the methane generation can be de- quirement cost was estimated considering the energy tariff currently
termined according to Eq. (11). paid by industries in Brazil, which is 0.04 US$/kW·h (considering an
MO2 2− exchange rate of US$1 = R$4.00). Additional expenses considered in
VCH4 = εCH4. (εCOD − β ). (CODv − SO ) Opex and Capex calculations were presented in Table S1 (supplemen-
MSO42 − (11)
4 tary material).
where VCH4 (Nm3·m−3) is the volume of methane produced per volume The cost of vinasse pumping for use as a fertigation is 0.675 US
of vinasse and εCH4 is the theoretical CH4 production per COD removed $·m−3 considering a Brazilian experience [27]. The price of treated
(0.35 NL·g−1; [24]). water was obtained on the website from the Companhia de Saneamento
The energetic potential (EP) of the biogas streams considering the de Minas Gerais (Sanitation Company of Minas Gerais) for the water
application of internal combustion engines was calculated according to industrial consumption > 200 m3 daily (US$ 2.8 (US$1 = R$4); [28]).
Eq. (12). Since the revenue from the savings in water purchase was more sig-
nificant, a sensitivity analysis was completed for the rate of treated
VCH4. LHV . ω water, aiming to confirm how changes in these variables would affect
EP =
3600 (12) the economic evaluation of the system. For this, rates range from 1 to
where LHV and ω correspond to the lower heating value of methane 3.3 US$ per m3 of water were considered.
(35.72 MJ·Nm−3; [25]) and the electric conversion factor (0.43; J620
GS-F12 GE Jenbacher GmbH & Co). 3. Results and discussions

2.5. Evaluation of the economic feasibility of vinasse treatment 3.1. Hybrid-coagulation-MF of vinasse: membrane retention and fouling

The preliminary economic analysis conducted intended to evaluate
the replacement of this traditional form of water management (ferti-
gation) by the combined MF and NF wastewater treatment system
considering a vinasse flow of 560 m3·h−1. This combined system gen-
erates two streams: one of treated water for industrial reuse (NF
permeate) and another from MF and NF concentrate that can be used
for fertigation. Thus, revenue is obtained from the reduction in costs
associated with water consumption and fertigation operations.
The net present value (NPV), the internal rate of return (IRR), and
the payback period for the investment were calculated considering a
period of 15 years. The NPV was calculated using Eq. (13) [26], in
which S is the profit or loss in the year (cash flow), i is the interest rate
considered, t is the number of the year.
n s
NPV = ∑t=1 (1 + i)t
(13)
The IRR was also calculated using Eq. (13). This parameter is equal
the interest rate, i, when NPV is equal zero. To calculate the payback,
corresponding to the year in which the overall result becomes a positive
value, the capital cost was divided by the annual cash inflow, which
considers both the profit or loss of the period is added to that of the
previous year.
The MF-NF membrane unit capital cost was based on a price pro-
vided by a major supplier of commercial membranes in Brazil and
corresponds to 8750.00 U$·m−3·h−1 of effluent. The capital cost (Ccap )
was calculated per cubic meter of effluent (Ccap / m3 ), from Eq. (14).
Ccap. AF
Ccap / m3 =
Qsys (14)
where Qsys is the capacity of the designed system and AF is the amor-
tization factor. AF is calculated by annualizing the capital cost, as
shown in Eq. (15).
ic ∙ (1 + ic ) DL
AF =
(1 + ic ) DL − 1 (15)
The coagulation assays were performed, and the removal efficiency
of different parameters are represented in Fig. 2. The pH measured after
coagulation, at different coagulant dosages, remained practically con-
stant, with a final value of 4.2 ± 0.3. According to other authors
[29,30], natural coagulants such as tannins does not consume or sig-
nificantly alter the alkalinity of the medium.
Coagulants adjust the solids surface charge properties so that ex-
isting particles in the effluent can be agglomerated or embedded into a
flocculated precipitate. Thus, significantly higher floc diameter was
found when increasing the coagulant dose, which facilitate the removal
by MF. An increase in COD removal and, specially, color removal can be
attributed to adsorption onto flocs surface or coprecipitation by inclu-
sion/occlusion during floc formation [31,32]. Furthermore, given the
increase in floc size, consequently higher surface area, the adsorption
removal mechanism is favored, ultimately justifying the increase in
removal given the increase in surface area. Besides the COD and color
removal by the floc’s formation, the main rejection mechanism is at-
tributed to the MF size exclusion and electrostatic interactions. The
vinasse residual color may be related to the presence of melanoidins
and phenolic compound with low molecular weight [7].
An increase in coagulant dose ensured an almost linear increase in
microfiltration permeate flux (Fig. 3). It is important to notice that the
resistance due to fouling (Rf) also decreases at initial coagulant dose
(0.5 mg/L) and remained relatively stable for further increases. The
specific fouling resistance presents an inverse relationship with cake
layer porosity; therefore, as floc sizes increase with the coagulant ad-
dition, the cake layer becomes more porous and compressible, reducing
fouling resistance [33]. In that sense, back transport velocity of parti-
cles becomes an important mechanism affecting the membrane fouling.
Particles ≤ 2 µm would promptly settle over membrane surface,
therefore responsible for cake layer formation, while larger particles
obtained after tannin was added (> 3 µm) would have negligible effect
in permeate flux [34]. Pore blocking presented a minor contribution for
total fouling resistance in this case, since most particles were bigger
than the membrane pore (0.45 µm). The overall results in terms of

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Y.A.R. Lebron, et al. Separation and Purification Technology 248 (2020) 117152

COD Color Floc size

80 40
71

COD and Color removal (%)

70 36
64 66
68 32
60 64 66 66 64 64
63 28

Floc size (μm)

50 53 24
40 48 20
30 16
31 12
26
20
8
10 4
0 0
0 0.5 1 2 4 6 8
Coagulant dose (mg/L)
Fig. 2. Floc size and removal of COD and Color for different coagulant doses.

membrane fouling reassures the advantages of using tannin as a coa-
gulant agent since other conventional additives, such as polyaluminum
chloride (PACl), is conventionally associated with an increase in fouling
resistance [35,36] and limits the vinasse application in fertigation due
to the presence of aluminum.
The higher cake porosity and compressibility would also explain the
lower flux decay (J/J0) when the coagulant was added to the process. In
terms of process stability, and based on the values of J/J0, 0.5 mg/L of
tannin would correspond to lower interruptions for membrane
cleaning. However, higher permeate flux was obtained at higher tannin
concentration, which should also be taken into consideration while
deciding for a proper dosage. Since higher settling rates were observed
at higher coagulant dosages (observed in Fig. 2 in terms of higher COD
and color removal), higher permeate flux was achieved at a given re-
covery rate when tannin was dosed at 8 mg/L. In despite of the coa-
gulant dosage, a similar pattern of permeate flux decay was observed in
all tests, being more pronounced when no coagulant agent was added.
A rapid decrease in permeate flux was perceived within the first re-
covery rates due to concentration polarization. Thereafter, a gradual
reduction was noticed and associated with the cake layer formation.
After the cake layer became the main fouling mechanism, the rate in
which permeate flux decay is relatively slow. Hence, based on permeate
flux, COD and color removal, a coagulant concentration of 8 mg/L was
chosen for subsequent analysis.
3.2. Integration of coagulation-MF and NF
Although microfiltration process showed considerable removal for
both COD and color, it was not enough to guarantee the physico-
chemical quality required for further water reuse. For that reason, an
additional NF process was employed. As a pre-treatment, MF presented
itself as an effective process and allowed for a better nanofiltration
performance. The process stability was observed until a recovery rate of
60% (Fig. 4), in which no significant flux decay was perceived (J/J0, C-
MF-NF = 0.88 and J/J0, MF-NF = 0.87). A positive effect over nanofil-
tration was also observed when it was preceded by the coagulation-
microfiltration. Although the flux decay presented a similar trend in
either case, a higher average permeate flux was obtained for the na-
nofiltration preceded by the hybrid pre-treatment process (33.45
L·m−2·h−1 for C-MF-NF compared to 29.96 L·m−2·h−1 for MF-NF).
The flocs formed after coagulation may deposit onto the membrane
surface, form a cake filter or cause membrane pore blockage. These
phenomena were briefly mentioned previously and is now investigated
in depth by the Hermia membrane fouling models. These models fit and
parameters are presented in Table 2. In most cases, intermediate
blocking filtration and cake filtration fitted well to the experimental
results, specially cake filtration. Whereas complete blocking filtration
and standard blocking filtration showed the poorest fitting among the
four fouling mechanisms. This result indicates that the flocs formed did
not precipitate on the inner walls or the entrance of the membrane
pores. The dominant fouling mechanism was the cake filtration model,

0% 10% 20% 40% 60% J/Jo Rf

90 0.7
80
0.6
Permeate flux (L m-2 h-1 )

70
0.5
Rf x 10 13(m-1)

60
0.4
J/Jo

50
40 0.3
30
0.2
20
10 0.1

0 0
0 0.5 1 2 4 6 8
Coagulant dose (mg/L)
Fig. 3. Permeate flux, flux total decay and fouling resistance at different recovery rates and coagulant doses.

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Y.A.R. Lebron, et al. Separation and Purification Technology 248 (2020) 117152

MF C-MF MF-NF C-MF-NF

80 40
70 35

MF permeate flux (L m-2h-1)

NF permeate flux (L m -2h -1)

60 30
50 25
40 20

30 15
20 10
10 5
0 0
0 5 10 15 20 25 30 35 40 45 50 55 60
Permeate recovery rate (%)
Fig. 4. Permeate flux comparison between MF and NF and their respective hybrid system for a coagulant concentration of 8 mg/L.

which means that a permeable layer was formed on the membrane The high organic compounds and nutrients concentration obtained
surface. In the MF case, this is corroborated by the fact that the flocs for both microfiltration and nanofiltration concentrate allows its further
formed, due to their size (≥7.14 µm), are unable to penetrate the usage in fertigation and energy obtainment (biodigestion/biogas).
membrane pores (0.45 µm), so they accumulate in the membrane sur- Although it seems to be consensus that wastewaters containing high
face and form a cake layer. The phenomenological constant k from the salinity may have an impact on the methanogenesis, and consequently
cake filtration Hermia model can be associated with the flux decline reduction on methane production, a previous study [39] showed that
severity [37]. As denoted by Table 2, the k values decrease when the high salinity concentration in molasses may inhibits anaerobic diges-
coagulation is applied, corroborating with the results shown previously. tion as the high K+ levels exert multiple negative effects on microbial
Furthermore, because MF is applied after coagulation, the k values are metabolism (particularly on methanogenesis) thereby favoring car-
larger than the k values from the NF, showing that the flux decline boxylate accumulation. One promising alternative could rely on sali-
severity in MF is higher than NF. nity-acclimated inocula (e.g., marine sediment) coupled with anaerobic
Table 3 presents both permeate and concentrate physicochemical digestion, which has been showing positive results on methanogenesis
parameters. Most COD and color content derive from natural con- [40,41]. Additionally, the opportunity of working with a lower vinasse
densation products of sugar and amino acids, commonly referred to volume overcomes one of the main disadvantages in fertigation appli-
melanoidins [38]. These are macromolecules, therefore more easily cations, the expenses related to its transportation [42].
retained by MF membranes, justifying the higher removal efficiencies
for both COD and color. However, due to steric hindrance, it was not
3.3. Raw and treated vinasse use in fertigation: Potential and impact
expected from MF a high retention of divalent and monovalent ions.
prediction
Hence, the values observed comes from an additional contribution of
the cake layer formed over membrane surface, which acted as an extra
The potential application and the impact prediction for the use of
filtration medium. It is noteworthy the contribution of a simultaneous
raw and treated vinasse in fertigation is presented in Table 4. The dif-
coagulation process for color and phosphorus removal. A slightly in-
ferent routes assessed (with or without coagulation) did not affect the
crease in conductivity is also noticed, however derived from the coa-
VARmax of the generated streams, mainly because coagulation is not
gulant addition.
able to influence or effectively remove potassium from the raw vinasse.
The subsequent nanofiltration process presented high removal rates
With a considerable reduction of potassium concentration from raw
without a significant difference in terms of removal percentages be-
vinasse with respect to NF permeate, the maximum vinasse application
tween the permeate obtained from MF-NF and C-MF-NF routes. The
rate (VARmax ) increases about 10 times. This means that if a combined
result points out to the robustness of nanofiltration, capable of pro-
stream containing the concentrates from NF and MF is used, it can lead
viding a high-quality permeate regardless of the feed composition. As
to a reduction in the total transportation cost associated with vinasse
expected, monovalent ions as potassium and chloride presented the
disposal on agricultural soil. This application should be carried out with
lowest retention values compared to the others, but still higher than
care due to the presence of other components in this stream such as
90%.
other ions and high BOD levels.

Table 2
Hermia fit and parameters obtained for microfiltration (MF), nanofiltration preceded by microfiltration (MF-NF), microfiltration preceded by coagulation (C-MF),
and nanofiltration preceded by coagulation-microfiltration (C-MF-NF).
Pressure (bar) Model

Complete blocking filtration Standard blocking filtration Intermediate blocking filtration Cake filtration

−2 −1 −2 −1 −2 −1
J0 (L·m ·h ) k (h −1
) R 2
J0 (L·m ·h ) k (m·L −1/2
·h −1/2
) R 2
J0 (L·m ·h ) 2
k (m ·L −1
) R 2
J0 (L·m−2·h−1) k (m4·L−2·h) R2

MF 23.2 0.004 0.91 24.1 0.0006 0.94 25.9 0.00031 0.95 45.6 0.000048 0.96
C-MF 55.3 0.011 0.76 55.5 0.0009 0.83 56.3 0.00031 0.90 61.6 0.000019 0.98
MF-NF 31.7 0.001 0.96 31.7 0.0001 0.96 31.7 0.00004 0.95 31.8 0.000003 0.96
C-MF-NF 35.7 0.001 0.80 35.7 0.0001 0.81 35.7 0.00003 0.81 35.7 0.000002 0.89

6
Y.A.R. Lebron, et al. Separation and Purification Technology 248 (2020) 117152

Table 3
Removal efficiency and physicochemical parameters for the microfiltration (MF) and nanofiltration (NF) permeate and concentrate streams.
Treatment COD Color (uH) Conductivity Phosphorus Sulfate Chloride Potassium Calcium Magnesium
route (mg·L−1) (mS·cm−1) (mg·L−1) (mg·L−1) (mg·L−1) (mg·L−1) (mg·L−1) (mg·L−1)

Raw vinasse 29,510 4657 4.3 250 588 663 2660 388 156

MF-NF MFPermeate 11,179 3410 3.4 248 484 570 2578 374 152
MFConcentrate 57,006 6527 5.65 253 744 802.5 2783 409 162
Removal (%) 62.1% 26.8% 20.9% 0.8% 17.7% 14.0% 3.1% 3.6% 2.6%
NFPermeate 168 6 0.28 2.09 3.44 39 251 3.1 2.6
NFConcentrate 24,637 7570 7.22 548 1071 1219 5422 827 334
Removal (%) 99.4% 99.9% 93.5% 99.2% 99.4% 94.1% 90.6% 99.2% 98.3%
C-MF-NF MFPermeate 8609 1763 5.3 206 508 608 2595 380 149
MFConcentrate 63,612 – 5.5 316 708 745 2757 400 166.5
Removal (%) 70.8% 62.1% −23.3% 17.6% 13.6% 8.3% 2.4% 2.1% 4.5%
NFPermeate 137 4 0.38 1.98 2.78 26 249 3 2.2
NFConcentrate 18,965 3912 11.75 455 1125 1319 5462 841 328
Removal (%) 99.5% 99.9% 91.2% 99.2% 99.5% 96.1% 90.6% 99.2% 98.6%

Regarding the estimated AOL the coagulation route induced a
concentration reduction in the concentrates due to removal of organic
matter by coagulation as discussed in Section 3.1. The input of organic
matter in the soil has several advantages such as increase in the soil's
potential to retain water, improvement in the physical structure of the
soil aggregates, increase in the soil's cation-exchange capacity and en-
hancement in the microbial activity [43]. Nevertheless, a large amount
of easily degradable organic matter in the soil could lead to numerous
biological processes, especially the uncontrolled release of greenhouse
gases [3]. Furthermore, the uncontrolled application of large amounts
of organic matter could overstimulate the microbial activity, which
promptly depletes oxygen levels and generates conditions of anaero-
biosis [3,43]. Lastly, the PE associated with the AOL , specially in the
MF concentrate reached a considerable value, 8.6–8.9 times greater
than the population densities of various countries such as São Paulo and
Belo Horizonte.
As expected, given the membrane retention efficiency for COD,
greater pollution potential is found for the membranes concentrates.
Furthermore, we can note that the coagulation route doesn’t sig-
nificantly affect the potential pollution. The concentrate use for ferti-
gation is once again here highlighted due to the attenuation in pollution
and beneficial aspects involved in this practice. Another option to at-
tenuate this scenario is the biodigestion of this concentrate to avoid
sulfide and CO2 simultaneously generating energy and cutting down
costs.
Because the NF permeate has low nutrients content this stream is
not ideally be used for fertigation. Other uses, within the manufactory,
are preferred such as cooling water and equipment cleaning.
3.4. Potential of energy recovery from raw and treated vinasse
The higher volumetric flow rate for raw vinasse contributed to a
higher energetic potential and overcame its lower potential for methane
production (Fig. 5). The energetic potential values observed were
equivalent to the values obtained when both microfiltration and
nanofiltration concentrate were combined in a single stream. However,
in addition to the advantages previously mentioned concerning the use
of a combined concentrate stream, it still presented a higher potential
for methane production (fold increase: 2.8 times) for a lower volumetric
flow rate.
Considering the microfiltration concentrate only, an average me-
thane production of 12.9 Nm3 per cubic meter of treated vinasse was
achieved, which increased by 35.6% (17.5 Nm3 per cubic meter of
treated vinasse) when the microfiltration and nanofiltration con-
centrate were combined. The values observed were higher than ob-
tained by other anaerobic systems devoted for vinasse treatment (6.3
Nm3·m−3 [44]; and 9.8 Nm3·m−3 [45]), reinforcing the advantages of
considering the concentrate stream for energy production.
In addition to the lower volumetric flow rate related to the nano-
filtration concentrate, regardless of the route, the lower COD/SO4−2
ratio notably contributed to lower yields of CH4 production and en-
ergetic potential. Compared to the microfiltration concentrate, it has a
higher and lower SO4−2 and COD concentration (see Table 3), re-
spectively, and would favor the sulfidogenesis in an anaerobic biodi-
gestion processes [4]. Under the mentioned conditions, sulfate reducing
bacteria would be competing with other microorganisms for carbon
sources leading to lower biogas production. Moreover, higher salts
concentration, although not considered while estimating the potential
of methane production, would be an additional contributor for in-
hibitory effects over biogas production as they cause bacterial cell de-
hydration as well as deleterious effects on the enzymatic catalytic rate
[4,46]. Conversely, higher COD/SO4−2 ratio achieved for the combined
concentrate would favor the methanogenesis process, therefore yielding
in higher methane production.
Although generated at higher volumetric flowrates, microfiltration
permeate would result in the lowest values of methane production and
energetic potential, therefore not considered as a practical option for
energy production. Instead, industrial reuse water could be obtained as
nanofiltration permeate, which has a higher economic value as dis-
cussed in the following sections.

Table 4
Potential and impact prediction of the use of raw and treated vinasse in fertigation. VARmax maximum vinasse application rate, AOL applied organic load, PE
polluting potential equivalent.
Parameters Raw vinasse MF-NF route C-MF-NF route

MFP MFC NFP NFC MFP MFC NFP NFC

3 −1
VARmax (m ·ha ) 189 195 180 2000 92 193 182 2016 92
AOL (kg·ha−1) 3342 1266 7204 19.0 2789 975 6456 15.5 2148
PE (inhab·ha−1) 295 112 635 1.7 246 86 569 1.4 189
Potential sulfide emissions (kg·ha−1) 38.2 31.4 48.3 0.2 69.6 33.0 46.0 0.2 73.1
Potential CO2 emissions (Mg·ha−1) 3.8 1.7 8.9 0.03 3.8 1.3 9.9 0.02 2.9

7
Y.A.R. Lebron, et al. Separation and Purification Technology 248 (2020) 117152

Potential CH4 production Energetic potential (MW) AD Feed flow

20 600

Potential CH4 production (Nm 3 m-3)

18
500

Energetic potential (MW)

16

AD feed flow (m 3 h-1)

14
400
12
10 300

8
200
6

4
100
2

0 0
PMF

PMF
CMF

CMF
CMF +CNF

CMF +CNF
CNF

CNF
Raw vinasse

MF-NF route C-MF-NF route

Fig. 5. Potential energy recovery from raw and treated vinasse. PMF: microfiltration permeate; CMF: microfiltration concentrate; PNF: nanofiltration permeate; CNF:
nanofiltration concentrate.

3.5. Technical and economic feasibility of vinasse treatment
Given the previously discussion, a route for vinasse treatment and
valorization, along with the stream’s main characteristics, is presented
in Fig. 6. In this route the membranes concentrates are combined for
later anaerobic biodigestion to reduce the pollution potential and allow
the vinasse valorization by means of a fuel gas production. The esti-
mated CH4 production for this concentrate stream (17.5 Nm3·m−3) is
2.7 times higher than the raw vinasse. The electricity production from
biogas streams could be enhanced with combined cycle power plants,
for example, gas turbines coupled to steam turbines.
Several works have indicated that there is a close relationship be-
tween increase in stalk production and accumulation of N and K, which
suggests that these two elements play a major role in the nutrition and
fertilization of the sugarcane plant. The maximum rate of uptake of
macronutrients by sugar cane was reported by NETAFIM (2020). The
sum of potassium, phosphorus, sulfate and chloride (KPSC) in the
generated streams does not exceed the maximum nutrients uptake rate
by sugar cane.
Furthermore, the NF permeate, with high physical chemical quality,
can be used as a reuse water, which consequently reduces costs and
pollution potential. The NF permeate can even be used as cooling water
given its low hardness value and chloride concentration. On the other
hand, for applications that demands better physical chemical char-
acteristics, this permeate should undergo a polishing step, especially for
Na+ and K+ removal. A possible choice for this polishing step would be
the use of electrodialysis or reverse osmosis.
The overall process presented a capital expenditure of 0.37 US
$·m−3. In terms of Opex, no difference was observed from amortization
and maintenance costs when considering the hybrid route, as shown in

Fig. 6. Technical and economic feasibility of vinasse treatment.

8
Y.A.R. Lebron, et al.
Fig. 7. (a) Operational costs related of the proposed route for vinasse treatment and (b) Payback and IRR as a function of treated water costs.
Fig. 7(a). The requirement of an additional stirring process for coagu-
lation implied in a higher energy requirement by the hybrid route, and
therefore, higher costs and contribution to Opex. Conversely, the lower
propensity to fouling for the C-MF-NF route resulted in a 47% reduction
in the membrane replacement contribution to the operational ex-
penditures. The savings represented by membrane replacement, how-
ever, were not enough to overcome the chemical requirement. These
costs were mainly due to the requisite of tannin-coagulant, which re-
presented 87% of the total operational expenditure for the C-MF-NF
route. For that reason, the route without coagulation presented the
lower Opex (0.37 US$·m−3) and, therefore, was chosen for subsequent
economic analysis.
Hence, the period elapsed before the investment is recouped and the
initial rate of return were evaluated, both based on possible variations
of treated water costs according to the location and availability. An
increase in acquisition costs for treated water corroborates to its ob-
tainment by the route proposed as it reduces the payback time. For the
prices currently practiced for industrial water acquisition (2.8 US
$·m−3), a payback would be achieved in three years after the process
implementation. For lower prices, a payback of ten years was observed
when treated water acquisition costs were close to 1.0 US$·m−3.
Because the NF permeate can be used as reuse water in the industry,
the demand for water from the local water supplier can be reduced or
even be totally replace by the NF permeate. Considering the water cost
from a local water supplier (2.8 US$·m−3), savings from the use of NF
permeate as reuse water would be 0.91 US$·m−3, in a year it would
total to US$ 10,333,794.24. A reduction in vinasse disposal costs was
also observed, in lower rates (0.01 US$·m−3) but still representing an
annually savings of US$ 123,561.59.
Finally, the internal rate of return was assessed, and the annual
percentage values reported in Fig. 7(b). It is then possible to decide
whether the proposal would be advantageous from the economical
point of view. For an average market attractiveness of 10%, the in-
vestment made would become interesting for water acquisition costs
higher than 1.3 US$·m−3 (IRR: 18.3% a/a). For the values currently
practiced, an internal rate of return of 52.3% as obtained and reassures
the MF-NF rout feasibility for vinasse treatment.
4. Concluding remarks
Microfiltration (MF), conjugated or not with coagulation, and na-
nofiltration (NF) separation process were compared for vinasse treat-
ment and valorization. At higher coagulants dosages, lower fouling
9
Separation and Purification Technology 248 (2020) 117152
rates were observed over MF membrane surface and, therefore, higher
permeate flux were obtained. Industrial reuse water was obtained as NF
permeate, and the concentrate from both processes presented a higher
energetic potential compared to raw vinasse. However, the costs related
with the coagulant acquisition suppressed the advantages of lower
membrane replacement when operational expenditures were taken into
consideration, thus, MF-NF route was elected. A 3 year would be re-
quired for the investment to be recouped considering the prices cur-
rently practiced for industrial water acquisition and an internal rate of
return of 52.3%.
CRediT authorship contribution statement
Yuri A.R. Lebron: Formal analysis, Visualization, Writing - original
draft. Victor R. Moreira: Formal analysis, Visualization, Writing -
original draft. Tatiane P.B. Furtado: Investigation. Selma C. da Silva:
Writing - original draft. Lisete C. Lange: Conceptualization, Resources,
Supervision. Miriam C.S. Amaral: Conceptualization, Methodology,
Validation, Resources, Supervision, Writing - review & editing.
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.
Acknowledgments
This research was funded by Coordination of Superior Level Staff
Improvement (CAPES); National Council for Scientific and
Technological Development (CNPq); Foundation for Research Support
of the State of Minas Gerais (FAPEMIG).
Appendix A. Supplementary material
Supplementary data to this article can be found online at https://
doi.org/10.1016/j.seppur.2020.117152.
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