Beruflich Dokumente
Kultur Dokumente
a
Research Institute for Industrial, Radiophysical and Environmental Safety (ISIRYM), Universitat Polit
ecnica de Val
encia, C/Camino de Vera s/n, 46022
Valencia, Spain
b
Department of Chemical and Nuclear Engineering, Universitat Polit ecnica de Val
encia, C/Camino de Vera s/n, 46022 Valencia, Spain
c
Depuracion de Aguas del Mediterra neo (DAM), Avda. Benjamin Franklin, 21, Parque Tecnologico, 46980, Paterna Valencia, Spain
a r t i c l e i n f o a b s t r a c t
Article history: In this work, the fouling mechanisms that dominate the ultraltration of residual brines from table olive
Received 30 November 2015 packing plant wastewaters were investigated. For that purpose, Hermia's models adapted to crossow
Received in revised form ltration, resistance-in-series model and a model combining intermediate blocking and cake formation
19 April 2016
mechanisms were tted to the experimental data. Tests were performed with a 5 kDa polyethersulfone
Accepted 23 April 2016
membrane at transmembrane pressures between 1 and 3 bar and crossow velocities between 2.2 and
Available online 26 April 2016
3.7 m s1. Results demonstrated that the resistance-in-series model was the most accurate to predict
permeate ux evolution with time. The predominant fouling mechanism was cake formation followed by
Keywords:
Ultraltration
intermediate blocking/adsorption. The fouling resistances that were determined by means of the resis-
Polyethersulfone membranes tance in series model were tested using a well-established mathematical model proposed by Mondal and
Table olive packing plant wastewaters De that also combines both fouling phenomena (intermediate pore blocking and cake formation). Results
Mathematical models demonstrated that the predicted resistances are consistent with those determined by Mondal and De's
Fouling mechanisms model.
2016 Elsevier Ltd. All rights reserved.
1. Introduction particles from liquid streams (Wang and Song, 1999; Barredo-
Damas et al., 2012). In this work, UF is considered to remove sus-
Spain is the main producer of table olives with 57,3,500 t year1, pended particles and macromolecules from residual brines from
which is around 22.1% of the total world production (International table olive production plants. A subsequent nanoltration (NF) step
Olive Oil Council, 2014). During the production process, large could be performed to recover the phenolic compounds.
amounts of water are used, generating high volumes of wastewater. Currently there are many studies focused on membrane treat-
Three types of wastewater are obtained: debittering, washing and ment of wastewaters from olive oil production, such as, olive mill
fermentation brines (Benitez et al., 2003). Fermentation brine wastewater (OMW) residue from a three-phase production method
wastewater is characterized by an acidic pH (around 4), a high and alperujo residue from a two-phase production method. These
conductivity (80e115 mS cm1), a high concentration of total sus- residues have a high chemical oxygen demand and a high phenolic
pended solids (0.2e2 g L1), dissolved chemical oxygen demand compound concentration, but unlike fermentation brine, its con-
(COD: 10e35 g O2$L1) and phenolic compounds (4.0e6.0 g of ductivity is much lower (between 4.00 and 13.98 mS cm1 for
tannic acid L1) (Garrido Fern
andez et al., 1997). Ultraltration (UF) OMW and 0.88e4.76 mS cm1 for alperujo) (Paredes et al., 1999;
is one of the most used techniques in industry to: concentrate, Alburquerque et al., 2004). Nanoltration (NF) processes have
separate or purify macromolecules, colloids and suspended been considered by most of the authors to recover and concentrate
high added value compounds from olive oil production wastewa-
ters. In order to improve the performance of the NF process, a pre-
* Corresponding author.
treatment with UF has also been proposed (Galanakis et al., 2010;
E-mail address: carcaral@upvnet.upv.es (C. Carbonell-Alcaina). Paraskeva et al., 2007). However, the number of studies on the
http://dx.doi.org/10.1016/j.jfoodeng.2016.04.016
0260-8774/ 2016 Elsevier Ltd. All rights reserved.
C. Carbonell-Alcaina et al. / Journal of Food Engineering 187 (2016) 14e23 15
mechanisms affecting permeate ux decline when UF membranes blocking model, which considers that foulant molecules cannot
were fouled with the residual brine, several mathematical models penetrate inside the porous structure and are deposited on previ-
were taken into account: Hermia's models adapted to crossow ously settled molecules. The complete blocking model (n 2), oc-
ltration, a resistance-in-series model and a model that combines curs when a solute molecule completely seals a pore entrance
the complete blocking and cake formation fouling mechanisms without penetrating inside the membrane pores and solute mole-
developed by Hermia. It is important to highlight the practical cules form a monomolecular layer on the membrane surface.
relevance of this type of empirical models based on exponential Finally, solute molecules that have a smaller size than the mem-
equations, since recent works were published at this regard. For brane pores can pass through the porous structure and block the
instance, Lin et al. used an exponential model with four tting inner pore walls. This corresponds to the standard blocking model
parameters to predict the entire permeate ux curve obtained in (n 1.5).
the ultraltration of protein aqueous solutions (Lin et al., 2008).
They divided the decrease in permeate ux according to two
2.2. Combined model (intermediate pore blocking and cake
fouling phenomena: intermediate blocking for the rst minutes of
formation)
operation and cake formation fouling for the rest of the ultral-
tration curve. Yee et al. studied the crossow ultraltration of whey
According to the literature (Field et al., 1995; Ho and Zydney,
by tting an exponential equation to the experimental data ob-
2000), the typical evolution of permeate ux during the UF time
tained in the fouling experiments (Yee et al., 2009). The empirical
can be divided in two stages: a great decline in permeate ux
model was compared to Ho and Zydney's one, and tting results
during the rst minutes of operation because of a pore blocking
demonstrated that the theoretical Ho and Zydney's model did not
phenomenon and a gradually slow ux decline caused by the
provide high accuracies at great time scales. However, model t-
accumulation of foulant molecules on the membrane surface and
tings using the exponential pattern were in a good agreement with
the formation of a cake layer on it. Along with this evolution, de la
the experimental data. Corbato n-Baguena et al. used empirical
Casa et al. (2008) developed a combined model taking into account
models with theoretical background to t the experimental data
the classical dead-end Hermia's equations for the complete block-
obtained during the ultraltration of enzymatic solutions
ing and cake formation model. In this work, a similar combination
(Corbato n-Ba
guena et al., 2015b). These models were based on
of the intermediate pore blocking and cake formation models
exponential decay patterns whose main parameters have physical
described by Hermia was adapted to crossow operating mode (Eq.
meaning (for instance, ratio among original membrane character-
(2)):
istics and those achieved after fouling and resistances due to
complete blocking and cake formation). In the literature, most of Jcombined model a,Jintermediate blocking model
the mathematical models were tested with model solutions instead
of real solutions. Moreover, the fouling mechanism that causes ux 1 a,Jcake layer formation model (2)
reduction when table olive residual brine is ultraltered has not
been investigated so far. In addition, Astudillo-Castro explained the where a is the fraction of blocked membrane pores. In addition, Eq.
fundamentals of the exponential equations proposed in this work, (2) includes two different model constants (Ki for the intermediate
which are based on the direct relationship between the maximum blocking model and Kcf for the cake layer formation model) as they
resistance value (achieved at the steady state) and that obtained at are the constants that correspond to Hermia's equations adapted to
a certain time (Astudillo-Castro, 2015). These authors applied the crossow operation for the intermediate pore blocking and the
abovementioned mathematical equations to describe the limiting cake formation models, respectively. The physical meaning of these
permeate ux as a function of transmembrane pressure. Another two parameters is the following: Ki represents the membrane
novelty of this work corresponds to the validation of the tted surface blocked per unit of total permeate volume and unit of initial
parameters obtained using a well-established, theoretical model membrane surface porosity, while Kcf is the ratio between the
available in the literature (resistance in series model developed by characteristics of the cake layer on the membrane surface and those
Mondal and De, 2010). of the original, unfouled membrane (Vincent Vela et al., 2009).
2.1. Hermia's models adapted to crossow ltration The resistance-in-series model is based on the Darcy's law,
which relates the permeate ux (J) with the transmembrane
Based on the classical Hermia's models for constant pressure pressure (DP), the feed solution viscosity (m) and the total hydraulic
dead-end ltration (Hermia, 1982), several authors (Field et al., resistance (Rt) (Eq. (3)).
1995; de Barros et al., 2003; Vincent Vela et al., 2009) included
DP
the steady-state ux related to the back-transport mass transfer to J K,DP (3)
adapt the classical models to a crossow conguration. Eq. (1)
m,Rt
shows the general model equation for the adapted Hermia's This model describes the total hydraulic resistance during the
models: ltration process as the sum of several resistances: the original
membrane resistance (Rm), the adsorption and concentration po-
dJ
KJ Jss J 2n (1) larization resistance (Ra) and the cake layer resistance (Rcf) (Eq. (4))
dt re et al., 2001; Turano et al., 2002):
(Choi et al., 2000; Carre
where J is the permeate ux, Jss is the steady-state permeate ux, K Rt Rm Ra Rcf (4)
is the model constant and n is the model parameter related to the
four different fouling mechanisms. If the value of n is zero, a cake According to Carrere et al., the experimental variation of Rt, Ra
layer is formed on the membrane surface due to the accumulation and Rcf follows an exponential trend (Carrere et al., 2001, 2002). In
of solute molecules that are larger than membrane pores. When addition, both adsorption and concentration polarization phe-
n 1, the fouling mechanism corresponds to the intermediate nomena are simultaneously determined in crossow ltration
C. Carbonell-Alcaina et al. / Journal of Food Engineering 187 (2016) 14e23 17
experiments. Thus, Ra can be expressed as an exponential function permeate ux for low time scales were determined. After that,
of the steady-state resistance (R'a), the rate of molecules deposition using the value of RIPB at time t1 and substituting the values of Rcf
on the membrane surface (b) and the ltration time (t), according to from the resistance-in-series model (described in Section 2.3) in Eq.
Eq. (5). Based on Eq. (5), in this work a general equation that ac- (11), the predicted values of permeate ux for time scales greater
count for Rcf as a function of time was newly proposed and repre- than t1 were determined. Finally, the permeate ux predicted
sented in Eq. (6), where R'cf is the steady-state cake resistance and c values were compared to the experimental data and to the resis-
is the rate of cake growth: tance in series method data. The goodness of the ts (in terms of R2
and SD) was determined.
Ra R0a 1 expb,t (5)
3. Materials and methods
Rcf R0cf 1 expc,t (6)
3.1. Feed samples
Substituting Eq. (5) and Eq. (6) in Eq. (4) and considering the
Darcy's law (Eq. (3)), the general equation for the resistance-in- This work was performed using different real solutions from
series model can be obtained (Eq. (7)): residual table olive brine, supplied by a TOPP. Due to the high
suspended solids content, a ltration step with a polyester car-
DP
J (7) tridge lter of 60 mm pore was carried out. Four different samples
m$ Rm R0a 1 expb$t R0cf 1 expc$t were provided by the TOPP. The average characteristics of the
ltered samples are shown in Table 1. The samples were stored at
5 C.
The constants obtained in this work for the resistance-in-series Feed and permeate samples were characterized. The pH and the
model were validated using a model developed by Mondal and De, conductivity were measured with a pH-Meter GLP 21 and EC-
2010. This model is also based on the resistance in series mecha- Meter GLP 31 (Crison, Spain). Total suspended solids (TSS) were
nism and combines the resistances of two classical fouling mech- determined according UNE 77,034 by means of glass microbre
anisms (intermediate pore blocking and cake formation). According lters with 1.2 mm pore size, using samples of 25 mL and differing
to this model, at low time scales (up to a certain time point, t1), weights before and after drying the microbre lters at 105 C, for
membrane fouling resistance is due to the intermediate pore 2 h. Turbidity was measured considering the UNE-EN ISO 7027
blocking phenomenon and as a result, permeate ux sharply de- standard method with a turbidimeter (D-112, DINKO, Spain). Dis-
clines with time (Eq. (8)). Therefore, permeate ux variation with solved COD was determined with Hach Lange kits, LCK014 (LCK,
time can be described as: Germany), dissolving the samples 10e12 times in order to remove
the interferences caused by the high chloride concentration.
DP
J (8)
m$Rm RIPB 3.3. Equipments and procedures
pH 4.0 0.2
Therefore, in order to validate the constants obtained for the Conductivity (mS/cm) 85.3 12.1
resistance-in-series model, Eq. (10) was rstly tted to the exper- Turbidity (NTU) 262.8 92.8
imental data up to the selected t1 values for each experimental TSS (mg/L) 411.7 80.0
condition tested. Once the values of KIPB were obtained, the resis- Dissolved COD (mg/L) 16547.7 3902.0
Phenolic compounds (mg/L Tyrosol eq) 1100.9 325.7
tance RIPB was calculated using Eq. (9) and the predicted values of
18 C. Carbonell-Alcaina et al. / Journal of Food Engineering 187 (2016) 14e23
Fouling and cleaning tests were carried out with varying TMP 3.5
and CFV, set at 1e3 bar and 2.2e3.7 m s1 respectively, for 2.5 h.
against TMP for the different CFV tested. It is observed that the
stationary permeate uxes are far from the osmotic water line. The 3.0
Osmoc water
stationary permeate ux increased with TMP up to a point at which CFV: 2.2 m/s
permeate ux remains constant or decreases with TMP. In this 2.5
CFV: 2.9 m/s
CFV: 3.7 m/s
2.0
2.5
1.5
Permeate flux 10 5 (m3m-2s-1)
2.0 1.0
2.2 m/s (Sample S2)
0.0
0.0 50.0 100.0 150.0 200.0 region, if pressure increases, an increase in particle concentration
Time (min)
on the membrane boundary layer takes place (Miller et al., 2014).
Fig. 1. Evolution of permeate ux with time during the UF experiments at TMP of 1 bar The presence of a high concentration of solutes in table olive re-
and model tting to the experimental data. sidual brine has a great effect on their concentration in the mass
C. Carbonell-Alcaina et al. / Journal of Food Engineering 187 (2016) 14e23 19
Table 3
Models tting accuracy: values of R2 and SD. Values in bold correspond to the best tting model.
TMPa (bar) CFVb (m s1) Sample Feed turbidity (NTU) Complete Intermediate Cake formation Combined Resistance-in-
blocking blocking model series
1 2.2 S2 314.3 0.401 0.122 0.703 0.084 0.896 0.051 0.894 0.059 0.969 0.034
2.9 S1 367.5 0.525 0.108 0.760 0.076 0.908 0.050 0.850 0.068 0.953 0.040
2 2.2 S2 314.3 0.643 0.110 0.835 0.076 0.960 0.040 0.990 0.022 0.989 0.023
2.9 S2 314.3 0.527 0.103 0.747 0.076 0.893 0.050 0.984 0.022 0.985 0.022
2.9 S4 183.4 0.590 0.092 0.743 0.073 0.883 0.051 0.990 0.017 0.988 0.018
3.7 S3 185.9 0.494 0.109 0.676 0.088 0.852 0.062 0.992 0.016 0.986 0.020
3.7 S4 183.4 0.603 0.078 0.739 0.064 0.862 0.048 0.984 0.017 0.980 0.019
3 2.2 S3 185.9 0.713 0.140 0.889 0.094 0.986 0.038 0.995 0.023 0.996 0.023
2.2 S1 367.5 0.186 0.187 0.376 0.168 0.665 0.122 0.984 0.034 0.984 0.030
2.9 S3 185.9 0.670 0.120 0.836 0.089 0.961 0.048 0.996 0.017 0.994 0.020
3.7 S3 185.9 0.626 0.105 0.783 0.082 0.919 0.053 0.994 0.015 0.992 0.016
a
TMP: transmembrane pressure.
b
CFV: crossow velocity.
c
SD: standard deviation.
Table 4
Values of model parameters for the resistance-in-series model at the different operating conditions tested.
TMPa (bar) CFVb (m s1) Sample Feed turbidity (NTU) Model parameters
5.0
Rt steady-state value is achieved. This pattern is related to the values
Rcf of Ra and Rcf. The parameter Ra is related to the pore blocking and
4.0
Ra absorption mechanism and the parameter Rcf is related to the cake
Rm formation. It is expected that, as transmembrane pressure in-
3.0
creases, the values of Ra also increase, due to the more severe
decrease in permeate ux observed in Fig. 3 compared to Fig. 1. This
2.0
trend is clearly observed in Table 4 for all the crossow velocities
tested when transmembrane pressure increased from 1 to 3 bar
1.0
independently of the feed sample. Regarding the effect of crossow
velocity on Ra, it can be observed that this parameter decreased as
0.0 crossow velocity increased. For example, the values of Ra for
0.0 50.0 100.0 150.0 200.0 sample S3 (turbidity of 185.9 NTU) at a transmembrane pressure of
Time (min) 3 bar decreased from 16.140$1012 to 12.590$1012 and then to
11.020$1012 when crossow velocity increased from 2.2 to 2.9 and
Fig. 5. Evolution of the resistances with time for sample S3 ultraltered at 3 bar and
then to 3.7 m s1, respectively. A few exceptions to this trend can be
2.2 m s1. Rt: total hydraulic resistance (m1); Rcf: cake layer resistance (m1); Ra:
adsorption and concentration polarization resistance (m1); Rm: membrane resistance
explained as a result of the different turbidity of the samples. For
(m1). the same operating conditions Ra increased when feed turbidity
increased, as it can be observed for samples S2 and S4 at 2 bar and
2.9 m s1 and for samples S1 and S3 at 3 bar and 3.7 m s1. On the
UF process. Several authors (Ho and Zydney, 2000; de la Casa et al., other hand, regarding the cake formation parameter, as crossow
2008; Mondal and De, 2010) reported that the evolution of velocity increased Rcf decreased, for all the transmembrane pres-
permeate ux with time can be divided in two stages: the rst one sures tested. This is explained by the reduction of the fouling layer
is caused by pore blocking and adsorption phenomena during the formed on the membrane surface during the UF process because of
C. Carbonell-Alcaina et al. / Journal of Food Engineering 187 (2016) 14e23 21
the increase in the shear stress. Also, for a xed crossow velocity, 5.0
Rcf increased when transmembrane pressures increased. However,
Table 5
Fitting accuracy for the model developed by Mondal and De (Mondal and De, 2010) when the resistance-in-series parameters were considered: values of R2 and SD.
TMPa (bar) CFVb (m s1) Sample Feed turbidity (NTU) Mondal & De vs Mondal & De vs
experimental data resistance-in-series
R2 SDc R2 SDc
that of the resistance-in-series model. It was observed that the cake dx.doi.org/10.1016/j.cej.2012.03.079.
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