Separation and Purification Technology 126 (2014) 21–29

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Separation and Purification Technology

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

Nanofiltration as tertiary treatment for the reuse of dairy wastewater

treated by membrane bioreactor
L.H. Andrade ⇑, F.D.S. Mendes, J.C. Espindola, M.C.S. Amaral
Department of Sanitary and Environmental Engineering, Federal University of Minas Gerais, Av. Antônio Carlos, no. 6627, Pampulha, Belo Horizonte, Minas Gerais, Brazil

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

Article history: Due to the growth in the costs of collecting and treating water, and with the treatment and discharge of
Received 5 July 2013 effluents, reuse has become an increasingly viable option for industries. This study aimed at evaluating
Received in revised form 30 January 2014 the application of membrane bioreactor (MBR) as secondary and nanofiltration (NF) as tertiary treatment
Accepted 31 January 2014
for the reuse of dairy wastewater, focusing on determining the best NF operating conditions. MBR
Available online 13 February 2014
showed high removal efficiency for COD (mean of 98%) and nutrients (86% total nitrogen and 89%
phosphorus). However, the concentration of dissolved solids in the permeate still prevented its reuse.
Keywords:
In order to remove these solids, the MBR permeate was nanofiltrated, and three different cross-flow
Nanofiltration (NF)
Operating conditions
velocities were evaluated. Due to lower external fouling and better quality of the permeate, the velocity
Wastewater reuse of 7.8 m/s was selected as the most suitable for the NF system. The optimum permeate recovery rate was
Dairy wastewater determined to be 45% since, at values higher than this, the quality of the permeate dropped. The proposed
Membrane bioreactor (MBR) treatment system (MBR + NF) showed overall efficiencies of 99.9% for COD and 93.1% for total solids. The
final treated wastewater could be reused as water for cooling, steam generation, or washing of external
areas and trucks.
Ó 2014 Elsevier B.V. All rights reserved.

1. Introduction restrictive parameters for wastewater discharge, imposition of

The dairy industry is considered, among the food industries, to
be the most polluting due to the high water consumption and the
generation of large amounts of liquid waste which, in turn, consti-
tute the main source of pollution of this type of industry [1]. These
wastewaters are characterized by high concentrations of organic
matter and nutrients, and are composed mainly of carbohydrates,
proteins and fats originated from milk, and of residual cleaning
agents [2].
Conventional treatment systems for these wastewaters include
the use of primary treatment to remove solids, oils and fats;
secondary biological treatment to remove organic matter and
nutrients; and, in some cases, tertiary treatment such as polishing.
However, several problems have been reported, such as high
production of scum, poor sludge settleability, low resistance to
organic shock load, difficulties in removing nutrients (nitrogen
and phosphorus) and problems in the degradation of fats, oils
and other specific types of pollutants [3,4].
Currently, the reuse of wastewater has become an environmen-
tal and economically viable option for industry, due to increasingly
⇑ Corresponding author. Tel.: +55 (31) 34093669; fax: +55 (31) 34091879.
E-mail address: lauraha@ymail.com (L.H. Andrade).
charges both for the collection of water as well as for the discharge
of effluents, and to the reduced availability and quality of water re-
sources. In the case of the dairy industry, on the one hand, the use
of treated wastewater should be avoided for washing equipment
that receives products or for operations where there is a possibility
of direct contact with raw material, because there may be a risk of
contamination; on the other hand, the reuse of water is encouraged
as replacement in cooling or heating systems and for good manu-
facturing practices, such as washing floors and trucks and rinsing
external areas [5,6]. In this scenario, one of the most promising
technologies for wastewater treatment and reuse are membrane
separation systems and the combining of these systems with other
technologies [7].
Membrane bioreactors (MBR) consist of biological reactors
associated with membrane separation processes, usually with
micro or ultrafiltration. Among the advantages of MBRs, it is
notable that they are compact and modular systems, with low
sludge production, that show total removal of suspended solids
independently of the characteristics of sedimentability of the
biomass, and that generate high quality treated wastewater [8].
The wastewaters from MBRs may be reused directly for unre-
stricted irrigation [7] or for recreational purposes after removal
of the residual color [9]. However, if the water use requires a

http://dx.doi.org/10.1016/j.seppur.2014.01.056
1383-5866/Ó 2014 Elsevier B.V. All rights reserved.
22 L.H. Andrade et al. / Separation and Purification Technology 126 (2014) 21–29
higher quality, such as for indirect reusable drinking water or for
industrial reuse, a tertiary treatment with nanofiltration or reverse
osmosis, for example, may be necessary [10,11].
Nanofiltration (NF) is an intermediate process of ultrafiltration
and reverse osmosis which carries advantages such as the efficient
removal of dissolved solutes, including multivalent ions and organ-
ic compounds of high molar mass; however, with lower pressure
requirements and higher flows than reverse osmosis [12]. Studies
show that NF is an efficient system for the secondary or tertiary
treatment of wastewaters, aiming at generating water for indus-
trial, agricultural and/or indirect drinking reuse [11,13–15]. How-
ever, the evaluation of the optimum operating conditions for
each specific NF system allows improvement of the overall perfor-
mance of the process, both in terms of quality of the permeate and
fouling control.
The use of NF for the treatment of several types of wastewaters
is reported in the literature, e.g. tannery [16], textile [17,18], refin-
ery [19] and municipal [20]. The application of NF for dairy waste-
waters is also found. However most papers focus on the treatment
of real used cleaning-in-place (CIP) solutions [21–23], model CIP
wastewater [24], flash cooler condensates from ultra high temper-
ature treatments [25], milk whey [26], model dairy effluent
prepared from commercial milk [1,27–29] or dairy chemical–bio-
logical treatment plant effluent [30]. We found no references to
the treatment of real effluents from large dairy industries making
use of MBR and NF.
Therefore, the aim of this study was to evaluate the application
of MBR as secondary treatment and NF as tertiary treatment for the
reuse of dairy wastewater. Emphasis was placed on evaluating the
best NF operating conditions that would generate a better quality
permeate and provide less membrane fouling.
2. Materials and methods
2.1. Wastewater from the dairy industry
The wastewater that was fed into the MBR came from a large
dairy industry located in the state of Minas Gerais, Brazil, whose
manufactured products are UHT milk, yogurt, cheese, cottage
cheese and petit suisse. The wastewater was collected from the
industry wastewater treatment station, following the stages of
sieving and flotation with compressed air.
2.2. Experimental unit of the membrane bioreactor
The bench scale membrane bioreactor used to conduct the tests
was built by PAM Membranas Seletivas Ltda (Rio de Janeiro Brazil).
The MBR had one module of hollow fiber, submerged microfiltra-
tion membranes (polyetherimide, average pore size of 0.5 lm,
membrane area of 0.044 m2, packing density of 500 m2/m3). The
MBR system consisted of three acrylic tanks (a 40-liter feed storage
tank, a 4.4-liter working volume biological tank, into which the
membrane was inserted, and a 5-liter tank for permeate storing),
a diaphragm pump, solenoid and needle valves, and flow and pres-
sure gauges.
The MBR was initially inoculated with sludge coming from the
activated sludge reactor of the effluent’s supplier. After an initial
phase of acclimatization of the microorganisms to the conditions
of the MBR and the effluent, which lasted 28 days and in which
the hydraulic retention time (HRT) was set to 8 h and there was
no sludge discharge, the system operated continuously for 40 days.
The operating conditions were: HRT of 6 h and sludge retention
time of 60 days (the defined values were based on existing litera-
ture and previous tests as explained elsewhere [31,32]. The flow
rate was 0.80 L/h, and the permeate flux was 18.2 L/(h m2). The
air flow rates of the two aeration systems used for oxygenation
and mixing of the biological tank and for membrane fouling control
were both 0.5 Nm3/h. The backwash flow rate was adjusted to
2.0 L/h and it was triggered automatically for 45 s, for every
15 min of permeation.
The feed and permeate of the MBR were characterized daily as
to COD and color (Hach DR2800 Spectrophotometer), and weekly
as to BOD, total nitrogen (Shimadzu TNM-1) and ammonia nitro-
gen, phosphorus and total solids. Three times per week the concen-
tration of mixed liquor volatile suspended solids of the sludge was
also ascertained. All analyses were done according to the recom-
mendations of the Standard Methods for the Examination of Water
and Wastewater [33].
2.3. Experimental unit for nanofiltration
The MBR permeate was nanofiltrated in order to generate final
treated wastewater with quality for reuse. For NF testing, an NF90
commercial membrane from Dow–Filmtec was used. The mem-
brane was cut properly and inserted into an 8.9 cm diameter stain-
less steel cell, providing a 62 cm2 filtration area, which simulated a
procedure with a flat membrane. The water permeability of the
membrane used showed a mean value of 2.3 L/(h m2 bar), indicat-
ing that this NF membrane had characteristics similar to those of
reverse osmosis.
The NF system comprised an feed tank (FT) where the MBR per-
meate was stored, a pump connected to a speed controller, flow-
meter for reading the feed flow rate, a pressure adjustment
valve, a manometer and temperature gauge. Fig. 1 shows a sche-
matic of this unit.
2.4. Determination of the best NF operating conditions
Initially, the best condition for the feed cross-flow velocity was
determined and next, the optimum permeate recovery rate of NF.
To determine the best flow regime, tests were conducted at
three different feed velocities, 4.4, 6.1, and 7.8 m/s, which corre-
spond to the feed flow rates of 4.0, 5.6, and 7.2 L/min. These values
are close to those applied by other authors, as Trägardh and
Johansson [21], who studied the nanofiltration of dairy discharged
alkaline cleaning solutions at a cross flow velocity of 7.0 m/s, and
László et al. [27], who treated model dairy wastewaters with ozone
P T
Retentate
FT
Permeate
SC
Legend
Pump
Flowmeter
Needle valve P
Manometer
SC Speed controller T
Thermometer
FT Feed Tank
Fig. 1. Schematic of the NF system.
 L.H. Andrade et al. / Separation and Purification Technology 126 (2014) 21–29 23

and nanofiltration at 4.6 m/s. Each test included measurements of
permeability, evaluation of pollutant retention efficiency, and
determination of resistance to filtration. To keep the conditions
constant during these tests, all permeate and retentate were fed
back into the feed tank, which was kept between 25 and 35 °C
by using an ice bath. At the end of each intermediate step, the
membrane was chemically cleaned using a sodium percarbonate
solution at a concentration of 0.5 g/L in an ultrasonic bath for
20 min.
Membrane permeabilities were calculated by measuring the
permeate flow at pressures of 10.0, 7.5, 5.0 and 2.5 bar. The perme-
abilities with wastewater were compared to the permeabilities
with distilled water for the clean membrane, previously measured.
To evaluate the retention capacity of the membrane, feed
samples (MBR permeate) and NF permeate were collected and ana-
lyzed for conductivity (Hach 44600 Conductivimeter), color, total
carbon (TC) and total organic carbon (TOC) (TOC Analyzer, Shima-
dzu TOC-V CNP), and total solids (TS) [22].
Resistances to filtration were determined according to the ser-
ies resistance model. Similar to the methodology used by László
et al. [27], the total resistance (Rt) was divided into membrane
resistance (Rm), external resistance (Re) and internal resistance
to fouling (Ri). To calculate these resistances, the flows Jw (flow
of the clean membrane filtrating pure water), Ji (flow of the fouled
membrane filtrating pure water) and Jt (flow of the membrane fil-
trating effluent) were determined at a fixed pressure of 10 bar. The
Jw flow was determined by the permeation of distilled water
through the clean membrane. Following this step, the wastewater
was nanofiltered for 30 min and the stabilization flow (Jt) was
measured. Subsequently, water was recirculated in the system at
a flow rate of 3.2 L/min for 30 min and, following this procedure,
the flow of permeation of distilled water was measured again,
corresponding to Ji. The resistances were calculated according to
the following equations, considering the dynamic viscosity of the
permeate to be equal to that of the water:
P occurred due to the reduction in the oxygen transfer efficiency
Rm ¼
g  Jw
P
Ri ¼  Rm
g  Ji
P denitrifiers, can lead to an anoxic microzone in the biofilm, result-
Re ¼  Rm  Ri
g  Je
in which P corresponds to the difference between the applied trans-
membrane pressure and the osmotic pressure of the feed, and g to
the dynamic viscosity of the water at 25 °C.
To determine the optimum permeate recovery rate (RR), nano-
filtration of the effluent was conducted with return of the concen-
trate to the feed tank and continuous withdrawal of the permeate,
using the optimum cross-flow velocity previously determined. The
permeate flow was monitored and samples of the permeate were
collected periodically for TC, TS and conductivity analysis [33].
The optimum RR was determined based on the results of permeate
were compared with standards for both cooling and boiler water
found in literature Asano et al. [5].
3. Results and discussion
3.1. Membrane bioreactor
The MBR operated with a mean MLVSS concentration of
19,500 mg/L. This value, which may be considered high given that
the mean MLVSS concentration in an MBR with a submerged mem-
brane module fluctuates between 10,000 and 15,000 mg/L [34], is
justified by the fact of the wastewater having a high concentration
of organic matter which is highly biodegradable [35]. Therefore,
there was sufficient substrate available for the microorganisms
for both the catabolism and the synthesis of new cells.
Table 1 shows the mean results of the concentration of
pollutants of the feed and the permeate of the MBR, and of the
respective removal.
It can be observed that the MBR showed increased capacity for
the removal of organic matter, both in terms of COD and BOD,
which may be justified by the high biodegradability of the waste-
water, high concentration of biomass in the reactor and the
presence of the membrane in the system [32].
High removal of nutrients and color is also noted. The high
sludge ages usually applied in MBRs contribute to the nitrification
that occurs in these systems, since nitrifying bacteria, responsible
for the conversion of ammonia to nitrate, are notoriously slow-
growing microorganisms [8]. In addition, the tropical climate and
high temperatures of the country also contribute to the nitrifica-
tion that occurs systematically in biological treatment systems
implemented in Brazil [36]. Thus, the high removal efficiencies of
ammonia nitrogen were predictable. However, since the reactor
is totally aerated and has no anoxic zones, the significant removal
of NT, which indicates the occurrence of denitrification, was not
expected initially. Nonetheless, this phenomenon might have
ð1Þ stemming from the sludge’s high viscosity. In this way, internal re-
gions of the biological flocs possibly did not receive oxygen and
transformed themselves into anoxic zones, thus providing favor-
ð2Þ able denitrification conditions [37].
According to Guadie et al. [38] incomplete air circulation in the
reactor and/or the presence of biofilms, which create a shield for
ð3Þ
ing in simultaneous nitrification and denitrification (SND) in the
reactor even during aeration. In such cases, nitrification occurs
on the surface of the biofilm, whereas denitrification occurs in
the inner layers due to a dissolved oxygen gradient [39,40].
Moreover, since sludge growth was high, part of the total nitro-
gen removal may result from a higher nutrient uptake. According
to Wang et al. [40], during the steady state, the mass of discharged
Table 1
Mean values of the main physicochemical parameters of feed and permeate and the
removal efficiencies of the MBR.

quality and flux decay. Parameters Raw wastewater MBR permeate Removal %
COD (mg/L) 2937.6 57.3 97.9
2.5. Evaluation of the viability of reusing final treated wastewater BOD (mg/L) 1120 6 99.5
Color (units Pt-Co) 2316.6 27.35 98.7
TN (mg/L) 49.8 6.9 86.1
To evaluate the viability of reusing the effluent from the NF, the N-NH3 (mg/L) 43.1 1.4 96.0
permeate, collected with the RR and cross-flow velocity conditions Phosphorus (mg/L) 36.3 1.4 89.0
considered as the most appropriate for the system, was analyzed TS (mg/L) 3.366 1.647 45.7
for pH, alkalinity, total dissolved solids, COD and metals (Ca, Mg, TFS (mg/L) 1.527 1.473 0.7
TVS (mg/L) 1.838 174 84.3
Cu, Zn and Fe) according to Standard Methods for the Examination
of Water and Wastewater [33]. Metals were analyzed by an atomic TN – total nitrogen; N-NH3 – ammonia nitrogen, TS – total solids, TFS – total fixed
absorption spectrophotometer (Perkin Elmer 3300). The results solids, TVS – total volatile solids.
24 L.H. Andrade et al. / Separation and Purification Technology 126 (2014) 21–29
sludge is equal to the mass of microorganism growth and forma-
tion; and nitrogen consumption due to cell assimilation can be cal-
culated with the cell formula (C5H7NO2), in which N accounted for
12% of the total mass. Mean total nitrogen load removal was calcu-
lated by the difference between feed and permeate TN concentra-
tions multiplied by flow rate; and nitrogen removal for
assimilation was estimated by emission of sludge, considering
sludge retention time of 60 days. The comparison of nitrogen re-
moval for assimilation (171 mg N/day) and TN removal
(719 mg N/day) shows that nitrogen loss in the system was larger
than nitrogen loss for assimilation. Thus, simultaneous nitrification
and denitrification must have occurred in the reactor.
The mean phosphorus removal was 86%. Traditionally, systems
projected to remove phosphorus should contain aerobic and anaer-
obic reactors in series for the selection and growth of phosphate
accumulating microorganisms (PAO) [36]. In the case of conven-
tional biological treatment systems, the partial removal of phos-
phorus takes place through its assimilation by the biomass for
cellular synthesis. In this case, the discarding of excess sludge
can result in phosphorus removal that varies between 10% and
30%, depending on the organic load of the effluent and on the oper-
ation conditions [41].
Farizoglu et al. [42] evaluated the removal of nutrients in a
membrane jet loop reactor treating whey and obtained total phos-
phorus removal efficiencies between 65% and 85%, similar to those
in the present study and greater than those expected for systems
that do not have specific configurations for advanced phosphorus
removal. For the authors, these elevated values result from consid-
erable phosphorus assimilation for cellular synthesis, as the bio-
mass concentration in the reactor was high (between 6000 and
14,500 mg/L), which was also true for both MBRs in this study.
Moreover, the authors assumed that part of the phosphorous re-
moval was related to the precipitation of phosphates with Ca2+
and Na+ ions, present in great quantities in the effluent in question.
The effluent used as feed in this work presented relatively high
Ca2+ concentration (near to 85 mg/L [31]). Given the low Kps value
for calcium phosphate (1.3  1032) the hypothesis of phosphorus
precipitation is quite plausible. Therefore, both justifications pre-
sented by Farizoglu et al. [42] are applicable to the present work.
Moreover, although PAOs thrive under anaerobic/aerobic condi-
tions, they do not necessarily require these operational conditions
in order to survive, persisting in bioreactors operated under strict
aerobic conditions as well as other aquatic habitats [43]. In that
way, MBRs present a potentially suitable environment for PAO pro-
liferation because they are slow growing organisms and the mem-
brane may completely retain them, since their size is typically
larger than microfiltration membrane pores [44 apud 38]. Addi-
tionally, as discussed before, the high biomass concentrations nor-
mally found in MBRs might lead to areas of anoxic or anaerobic
micro-niches within the sludge flocs, potentially providing PAOs
a selective advantage [43].
Silva et al. [43] characterized the microbial diversity of the acti-
vated sludge in a group of eight MBR plants fed with municipal
wastewater, located in different regions of Europe. They found that
PAOs were presented in similar levels (10% ± 6%) in all studied
MBRs, even those without a defined anaerobic zone. The results
from this study suggest that a defined anaerobic zone is not neces-
sarily required for putative PAO growth in MBRs, since polyphos-
phate storage may provide a selective advantage in fulfilling cell
maintenance requirements in substrate-limited conditions (low
F/M).
Thus, it is possible that a part of phosphorous removal found in
the presented study was related to biological assimilation by PAOs.
In relation to the solids, the highest removal was for volatile sol-
ids, which are made of biodegradable organic matter. The removal
of fixed solids may be related to the precipitation of salts and/or
the retention of inorganic particulate material by the membrane.
It is important to note that MBRs show complete retention of sus-
pended solids.
Thus, it can be stated that the MBR permeate shows high qual-
ity, with low concentrations of organic matter and nutrients. How-
ever, there is still a significant concentration of dissolved solids,
since the MBR microfiltration membrane is not able to retain com-
pounds in solution. Therefore, in order to remove these solids and
to generate a final treated wastewater suitable for reuse, the MBR
permeate was sent to an NF unit.
3.2. Determination of the best NF operating conditions
Fig. 2 shows values of permeability of the NF membrane with
wastewater divided by the permeability with water for the clean
membrane at three different cross-flow velocities.
A positive impact on the permeability with wastewater, i.e. an
18% raise, was observed by increasing the cross-flow velocity from
4.4 to 6.1 m/s. This increase was responsible for an improvement in
the hydrodynamic conditions of the system, reducing the thickness
of the boundary layer near the surface of the membrane and the
fouling [13]. In addition, according to Luo et al. [28], higher shear
rates may reduce the accumulation of solutes on the membrane
surface, minimizing the difference in osmotic pressure across it,
and increasing the effective driving force for permeation, thus
increasing the flow.
An even greater increase in flow velocity, up to 7.8 m/s, also in-
creased membrane permeability with the wastewater, although
less significantly, which shows that there are types of foulings
which cannot be removed by establishing better hydrodynamic
conditions. The gain obtained in this operation was 4%, and the
permeability with wastewater reached a value corresponding to
97% of permeability with water.
Table 2 shows the values of the physicochemical parameters of
NF feed and of the permeates obtained for the three conditions
tested. It is noteworthy that NF tests were conducted in batch
mode. Thus, the MBR permeate, collected during some hours,
was fed into the NF system. Therefore, the concentration of some
parameters of the NF feed shown in Table 2 may differ slightly
from those shown for the permeate of the MBR in Table 1, since
in the latter case they refer to average values obtained during
40 days of monitoring.
Improvement in all parameters monitored was noted with the
increase in the feed velocity. Since increased flow rate reduces
the accumulation of solutes retained on the membrane surface, it
also reduces their concentration gradient between the feed and
100%
Effluent permeability in relation
80%
to water permeability
60%
40%
20%
0%
4.4 m/s 6.1 m/s 7.8 m/s
Fig. 2. NF permeability with wastewater in relation to permeability with water for
three feed flow conditions.
 L.H. Andrade et al. / Separation and Purification Technology 126 (2014) 21–29 25

Table 2
Values of the physicochemical parameters for the feed and the permeates obtained for the different cross-flow velocity and their respective retention efficiencies.

Parameter Feed Permeate

4.4 m/s 6.1 m/s 7.8 m/s
Value Retention (%) Value Retention (%) Value Retention (%)
Conductivity (mS/cm) 2.28 0.316 86.1 0.244 89.3 0.151 93.4
Color (Pt-Co units) 36.8 8.9 75.7 6.4 82.7 3.3 91.0
TS (mg/L) 1.482 767 48.3 523 64.8 488 67.1
TC (mg/L) 231.2 6.7 97.1 4.4 98.1 4.1 98.2
TOC (mg/L) 24.9 0.6 97.4 0.6 97.4 0.5 97.9

TS – total solids; TC – total carbon; TOC – total organic carbon.

(a) Membrane Internal External

the permeate, reducing the driving force for their transport. In 20.0
addition, due to less fouling at high flow rates, the passage of sol- 20

Resistance (x1013 m-1)

vent is favored, contributing to dilution of the permeate [28]. 18 16.1
The reduction in the conductivity of the permeate in relation to 16 14.0
the feed was greater than that of the total solids, indicating that 14
most of the retained solids correspond to divalent salts which con- 12
10
tribute to conductivity to a greater degree. This is consistent with 7.0
8
expectations for an NF membrane. It is also noted that TOC concen-
6
tration is well below that of TC, indicating that most of the carbon 2.9 3.5
4 2.1
still present in the MBR permeate is not due to organic compounds, 1.7
2 0.2
but rather to the carbonates or other forms of inorganic carbon 0
which were efficiently retained in the NF. 4.4 m/s 6.1 m/s 7.8 m/s
Fouling is the greatest problem facing most membrane separa-
tion processes, causing significant reduction of permeate flow,
(b) Membrane Internal External
100%
increased frequency of cleaning, and reduced useful life of the
membrane. Fouling is caused by adsorption of solutes in the mem- 78 79
80%
Resistance (%)

brane material, total or partial blockage of the pores, deposits of 69

particles on the membrane surface (cake) and formation of a gel
layer [23,45,46]. In the case of NF, the reduction of permeate flow
due to the effects of concentration polarization is also highly signif-
icant. Due to convective transport, the concentration of retained
solutes becomes greater near the surface of the membrane than
within the bulk solution, leading to concentration polarization. In
some cases, this concentration may reach threshold values, causing
the precipitation of inorganic compounds (scaling) and contribut-
ing even more to the increased resistance to filtration [47].
Regarding membrane filtration of dairy wastewater, the protein
materials may act as powerful fouling agents, while the surfactants
may alter the permeability of the membrane by concentration
polarization or by the formation of micelles [48]. Furthermore, dur-
ing the reclamation of wastewater, organic constituents contained
in the biologically treated wastewater, such as polysaccharides,
proteins, humic and fulvic acids, and nucleic acids, designated as
wastewater organic matter, are found to play an important role
as membrane foulants, especially the hydrophobic fraction [49].
Fig. 3 shows the resistances to filtration for the three cross-flow
velocity that were analyzed. The resistances were divided into
membrane resistance (Rm); external fouling resistance (Re), which
includes formation of a gel layer, concentration polarization and
scaling; and, internal fouling resistance (Ri), which basically con-
sists of adsorption and pore blockage. As the membrane used in
this study had characteristics closer to those of a reverse osmosis
membrane, in this case the pores refer to the free volume between
the polymeric chains. Membrane resistance acquired different val-
ues in the three tests performed, due to variations in the mem-
brane permeability with water measured after chemical cleanings.
For the lowest velocity evaluated, the greatest contribution to
resistance (without considering the resistance of the membrane it-
self) came from the external fouling component (24% of the total
resistance). A concentration gradient of the retained solutes was
formed on the membrane surface, due to the low feed flow rate
and the lower turbulence generated, causing a diffusive transport
60%
40%
24
20
20% 14
7 8
1
0%
4.4 m/s 6.1 m/s 7.8 m/s
Fig. 3. Resistances to NF filtration: (a) values and (b) percentage.
in the opposite direction from the convective flow of the permeate,
and increased resistance to filtration. In addition, the increase in
the solute concentration near the membrane may have led to the
increase in viscosity and the formation of a gel layer.
When the velocity was increased to 6.1 m/s there was a 76%
reduction in external resistance, which corresponds to only 8% of
the total resistance for this flow condition. This result justifies
the permeability gain observed previously, and is related to the in-
creased turbulence in the region near the membrane. Nevertheless,
there was an increase in internal resistance, showing that the
external fouling that was formed may retain solutes and reduce
the availability of the membrane to internal fouling by adsorption
since, according to Contrerasa et al. [50], dissolved organic com-
pounds may be adsorbed by colloids that are deposited on the
membrane.
The subsequent increase in cross-flow velocity to 7.8 m/s
reduced external resistance even more, by 91%. Although there is
also an increase in internal resistance, the resistance due to the to-
tal fouling (internal + external) was reduced from 4.6 to
3.7  1013 m1.
Kaya et al. [24] divided the total resistance of a nanofiltration
process into gel layer resistance, internal resistance, concentration
polarization resistance, and membrane resistance. For the effluent
evaluated by those authors, a synthetic wastewater based on
26 L.H. Andrade et al. / Separation and Purification Technology 126 (2014) 21–29
anionic and non-ionic detergents, dyes and sodium chloride, the
total resistance ranged between 3 and 5  1013 m1, values
approximately 5 times lower than those obtained in the present
study. On the other hand, László et al. [27] obtained resistances
from internal fouling and from the gel layer of 1.2  1014 and
5.5  1014 m1, respectively, for nanofiltration of model residual
water prepared with powdered skim milk and anionic surfactant.
The differences observed between the results found in the litera-
ture and those obtained in the present study may be related to
the different water permeabilities of the membranes used in each
study, and to the fact that the other authors used simulated waste-
water based on basic compounds that, therefore, had much less in-
ter-relational complexity among the constituents than the real
wastewater studied here.
Thus, due to the significantly greater efficiency in the retention
of solutes and the lower fouling at the cross-flow velocity of 7.8 m/
s, this was selected as the best operating condition among the
three evaluated.
Following determination of the best flow rate, the greatest per-
meate recovery rate (RR) at which the system could operate with-
out damage to its performance was determined. To accomplish
this, the wastewater was nanofiltered using the pressure of
10 bar and the selected feed velocity of 7.8 m/s. The variation in
permeate flux resulting from the RR is shown in Fig. 4. The maxi-
mum RR value attained was 70%, due to operational restrictions
of the system.
In Fig. 4, the bars represent the positive and negative values of
standard deviation permeate flux. These standard deviations were
calculated according to the formula for determining the combined
standard uncertainty:
vffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
u N  2
uX @f
uc ðyÞ ¼ t  uðxiÞ
@xi
i¼1
where uc(y) is the combined standard deviation of the variable y, f is
the function y = f(x1, x2, . . . , xN) and u2(xi) is the uncertainty related
to the parameter xi. If the flux of permeate (J) is calculated by:
V=t
J¼
p  D2=4
where V is the volume of permeate collected in a given time, t is the
sampling time (assumed in this case as 60 s) and D is the diameter
of the membrane, the combined uncertainty of J can be calculated
by:
25
20
Permeate flux (L/h.m²)
15
10
5 10
0 0
0% 10% 20% 30% 40% 50% 60% 70%
Recovery rate
Fig. 4. Variation in permeate flux with the RR for feed cross-flow velocity of 7.8 m/s
and pressure of 10 bar.
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
u2 ðVÞ u2 ðtÞ 4u2 ðDÞ
uc ðJÞ ¼ J  þ 2 þ ð6Þ
V2 t D2
The increase in RR may lead to reduction in permeate flux, due
to several factors: increase in the difference of osmotic pressure
between the feed and the permeate, due to the increased concen-
tration of retained solutes; thickening of the gel layer due to in-
creased concentration of macromolecules and colloids on the
membrane surface; increased viscosity of the fluid flowing through
the membrane pores; increased fouling due to internal and exter-
nal adsorption [46]. However, considering the standard deviation,
no significant fluctuations or clear change in the permeate flux pro-
file were observed with the increase of the RR, which may also be
related to the relatively low maximum RR attained.
Fig. 5 shows the results of conductivity, total solids (TS) and to-
tal carbon (TC) of the NF permeate as a function of the RR applied.
There was little variation in the quality of the permeate for RR
below 45%. However, for higher RR, the effect of the accumulation
of retained molecules causes an increase in the driving force for
passing solutes through the membrane, and the conductivity and
the concentration of TS and TC of the permeate increase. With
the RR at 70%, this effect was highly significant and a big drop in
permeate quality can be seen.
Therefore, despite there being no significant reduction in the
permeate flux with the increase in the concentration, the 45%
recovery rate may be selected as the best, due to the drop in per-
meate quality observed at the higher values. However, for larger
scale applications, it is important to note that a higher recovery
rate can be achieved if a combination of modules in series is used,
in several steps, instead of parallel modules operating at 45% RR
each.
Furthermore, the data collected from the industry supplier of
ð4Þ
the wastewater show that 1300 m3/day of water are consumed
in the industrial plant, of which 1000 m3/day are transformed into
wastewater and 300 m3/day1 are lost to evaporation or are incor-
porated into products. Of the volume collected (1300 m3/day),
60% is used for cleaning operations (clean in place) and must meet
potability standards, 30% is used to replace water in cooling and
ð5Þ heating systems, and 10% is used in good manufacturing practices
(cleaning floors, bathrooms, external areas, etc.). Therefore, since
the direct reuse of effluents as potable water is not recommended
due to the associated risk [5], the aim was that the NF permeate
could meet the quality requirement of the 40% of water which is
TC TS Conductivuty
50 350
300
40
Conductivity (µS/cm)
250
TS (mg/L)
TC (mg/L)
30 200
150
20
100
50
0
0% 10% 20% 30% 40% 50% 60% 70% 80%
Recovery rate
Fig. 5. Results of conductivity, total solids, and total carbon of the NF permeate as a
function of the RR.
 L.H. Andrade et al. / Separation and Purification Technology 126 (2014) 21–29 27

Table 3
Standards for cooling and boiler water, and values obtained for the NF permeate.

Parameter NF permeate Cooling watera Steam generationa

Low pressure (<10 bar) Medium pressure (10–50 bar) High pressure (>50 bar)
TDS (mg L1) 233 500 700 500 200
Alkalinity (mg L1) 166 350 350 100 40
pH 8.9 6.9–9.0 7.0–10.0 8.2–10.0 8.2–9.0
COD (mg L1) 4.0 75 5.0 5.0 1.0
Calcium (mg L1) 0.44 50 + 0.4 0.01
Magnesium (mg L1) 0.041 0.5 + 0.25 0.01
Copper (mg L1) 0.04 + 0.5 0.05 0.05
Zinc (mg L1) <0.1 + + 0.01 0.01
Iron (mg L1) 0.05 0.5 1 0.3 0.05

TDS – Total Dissolved Solids.

+ Accepted as received, if other threshold values are met.
a
Source: Asano et al. [5].

NF Permeate
MBR Permeate NF
Dairy Wastewater COD = 4,0 mg/L
COD = 34 mg/L
COD = 3274 mg/L Color =35,5 Pt-Co units Color = 15,0 Pt-Co units
Color = 1802 Pt-Co units TS = 1783 mg/L TS= 233 mg/L
TS = 2323 mg/L

NF Retentate
COD = 73,4 mg/L
MBR Color = 75,1 Pt-Co units
TS = 3087 mg/L

Fig. 6. COD concentration, color and total solids of the raw wastewater, MBR permeate, NF retentate and NF permeate.

used for washing, cooling and heating (520 m3/day). Thus, if the
industry wastewater were treated by the proposed system, com-
prising MBR and NF, and if 45% NF recovery rate were applied,
450 m3/day of reusable water would be generated, supplying al-
most all of the demand for non-drinking water in industrial
facilities.
Although the aim of this study is not the definition of a route for
the exclusive reuse by the industry in question, it is believed that
its water balance is representative of other industries in the sector
which fabricate the same products, and that similar decisions
could be made in more general settings.
However, direct comparison of water balance of different indus-
tries can lead to erroneous interpretations, since water consump-
tion levels are determined by production output and the applied
technologies and may significantly vary from one industry to an-
other [6]. For example, according to Gleick et al. [51], water use
in the dairy products industry is divided as following: 71% for cool-
ing, 23% process, 3% restrooms, 3% landscaping; while other
authors suggest a different distribution: 53% non-contact cooling/
heating, 27% process, 19% sanitary use [52].
3.3. Reuse of the final treated wastewater
To verify the possibility of reusing the NF permeate, its physico-
chemical properties were compared to quality standards for cool-
ing and boiler water, as shown in Table 3.
It is observed that the quality of the NF permeate meets all the
standards for water used in cooling and low pressure steam gener-
ation, enabling its reuse for such applications, as well as for wash-
ing floors, external areas and trucks, which require a lower quality
water. However, the only parameters that do not fall within the
boiler water standard at medium pressure are alkalinity and cal-
cium. Therefore, if there is interest also in reusing wastewater for
Table 4
Removal efficiencies of the MBR, of the NF and the combination of the two processes.
Parameter
COD (%) Color (%) TS (%)
MBR 99.0 98.4 47.0
NF 88.2 57.7 86.9
Overall 99.9 99.3 93.1
boilers which operate at pressures greater than 10 bar, options
such as the use of a subsequent degassing unit to remove CO2
and reduce alkalinity, exchanging nanofiltration for reverse osmo-
sis, or implementing a final polishing system with ionic exchange,
could be evaluated.
No studies were found in the literature that reported the use of
MBR and NF for treating dairy wastewater aimed at reuse. How-
ever, some authors used NF as the only treatment system for this
type of wastewater [1,23,28]. Vourch et al. [1] used NF to treat a
synthetic dairy wastewater, comprising whole milk, skim milk
and milk whey, with COD concentration of 8200 mg L1and con-
ductivity of 700 lS cm1. The NF permeate had a COD concentra-
tion of 87 mg L1, conductivity of 637 lS cm1 and calcium
concentration of 3.2 mg L1. Fernandéz et al. [23] evaluated the
operation of a pilot NF unit used for the recovery of clean in place
(CIP) solution consumed in the dairy industry. The feed solution
had a COD concentration between 3000 and 10,000, total dry ex-
tract between 1.0% and 2.0%, and conductivity of 15 mS cm1;
while the permeate had 1500–2500 mgCOD L1, conductivity of
15–20 mS cm1, and total dry extract of 0.9–1.0%. The concentra-
tions of the permeate obtained in the present study were found
to be lower, which is probably due to the contribution of the high
removal of pollutants in the MBR in order to generate a final per-
meate with high quality.
28 L.H. Andrade et al. / Separation and Purification Technology 126 (2014) 21–29
Fig. 6 shows the final result of the treatment route tested. The
values shown for the concentrations of pollutants in the raw
wastewater and in the MBR permeate differ slightly from those
shown in Table 1 because those were the mean concentrations ob-
tained during the entire operating period of the MBR; while those
shown in Fig. 6 are the measurements made on the day that the
samples to be used for conducting the NF tests were collected.
The MBR is found to function efficiently in removing organic
matter and color contained in the raw wastewater. However, the
concentration of total solids, predominantly composed of dissolved
solids, was still high and had to be removed in order to provide
water with quality for reuse. This was obtained by passing the
MBR permeate through NF, which showed high retention of solids
and also of residual COD. As can be seen in Table 4, the overall sys-
tem efficiencies were very high. It is emphasized that the NF reten-
tate could be recycled in the industry as reused water for
applications that do not require very high quality, such as for irri-
gating gardens, or could be discarded into bodies of water. The COD
concentration of 73 mg L1 not only meets the discharge parame-
ters of environmental legislation in effect in the state of Minas Ger-
ais, Brazil (180 mgCOD L1), but is also well below this standard,
thus contributing to the release of better quality effluent and to
the preservation of water bodies.
4. Conclusion
 The MBR is a viable system for treating dairy wastewater, pro-
viding high removal efficiencies not only of organic matter but
also of color and nutrients. The MBR permeate showed high
quality; however, the concentration of dissolved solids is still
high to be reused as industrial water.
 Cross-flow velocity of 7.8 m/s was selected as the most suitable
for the NF of the MBR permeate, once this condition led to
increased turbulence and, therefore, less fouling and better per-
meate quality. The results of the resistances to filtration showed
that, when the cross-flow velocity increases from 4.4 to 7.8 m/s,
the resistance due to external fouling significantly reduces;
however, there is a slight increase in the resistance due to inter-
nal fouling.
 The permeate recovery rate was observed to have no influence
on permeate flux. However, the increased RR provided an
increase in the passage of pollutants to the permeate and a drop
in quality. Based on this information and on the water balance
of the dairy industry, the RR of 45% was selected as the
optimum.
 The quality of the NF permeate met all the standards for cooling
water and water for low pressure steam generation, proving
that it may be reused for these applications as well as for wash-
ing floors, external areas and trucks, that require a lower quality
water.
Acknowledgments
The authors gratefully acknowledge PAM Membranas Seletivas
Ltda for supplying the membranes, CNPq for the scholarship
awarded, FAPEMIG for the financial resources granted to the
research and DESA for the resource for the article translation.
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