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Research article
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Article history: This study investigated the cost and CO2 emission reduced as a result of optimizing operating conditions
Received 18 December 2016 for chemical cleaning in a membrane filtration process used for water treatment. A new protocol was
Received in revised form proposed and operating conditions for chemical cleaning of a pilot-scale membrane filtration process
11 February 2017
were optimized. The critical flux for irreversibility was identified as the permeate flux using a modified
Accepted 26 February 2017
Available online 8 December 2017
flux-step method, and was 100 l m2 h1, 20 l m2 h1 higher than the vendor recommended permeate
flux. NaOCl, which is also the vendor recommended chemical, was selected as the optimal chemical
reagent following an examination of the permeability restoration ratios and nature of the irreversible
Keywords:
Irreversible fouling
foulants. The optimized operating conditions of enhanced flux maintenance (EFM), determined using
Chemical cleaning optimization response surface methodology (RSM) were: 6.3 d interval, 500 ppm concentration, and 76 min duration,
Operating cost reduction which represented an increase of 4.3 d, 300 ppm, and 36 min, respectively, as opposed to the vendor
Enhanced flux maintenance recommended conditions. As a result, the total operating cost and CO2 emission were $0.1187/m3 and
Response surface methodology 112.75 g CO2/m3, respectively, and 26.5% lesser compared to the operating cost and CO2 emission based
on vendor recommended conditions. This study found that the reductions in operating cost and CO2
emission using the optimization process were excellent.
© 2017 Published by Elsevier Ltd.
https://doi.org/10.1016/j.jenvman.2017.02.072
0301-4797/© 2017 Published by Elsevier Ltd.
S.S. Yoo et al. / Journal of Environmental Management 206 (2018) 1126e1134 1127
(Kuzmenko et al., 2005; Peter-Varbanets et al., 2011), decreasing recommended conditions that are not the optimized operating
the reduction of flux and increasing TMP. However, excessive conditions.
chemical cleaning can damage the membrane surface, resulting in Most of the previous studies conducted on the optimization of
increase in membrane replacement cost, chemical cost, and sludge chemical cleaning have aimed to increase the efficiency of fouling
disposal cost. In addition, insufficient chemical cleaning cannot removal (Bogati et al., 2015; Kim et al., 2011; Strugholtz et al., 2005;
eliminate fouling completely and can lead to additional chemical Zondervan et al., 2008). Although a few studies focused on cost
costs that eventually increase operating costs (Chen et al., 2003a; reduction of the membrane filtration process, it was difficult to
Regula et al., 2014). Therefore, the operating conditions for chem- apply the protocols in practice, as they were very complicated, or
ical cleaning need to be optimized to reduce operating costs of the were likely to cause errors when they were applied to a pilot- or
membrane filtration process. full-scale plants because they were carried out as lab-scale exper-
The operating conditions of chemical cleaning are cleaning iments (Porcelli and Judd, 2010b). The objective of this study was to
interval, cleaning duration time, chemical type, and chemical investigate the reduction of operating cost and CO2 emission that is
concentration. Energy consumption, chemical use, and sludge achieved by optimizing the operating factors for chemical cleaning
production in the membrane filtration process are reduced by of the membrane. A new protocol was proposed to optimize the
operating condition optimization, and membrane replacement operating conditions and the operating conditions for chemical
cycle is increased by it. This means operating cost reduction in cleaning of a pilot-scale membrane filtration process were opti-
economical aspects as mentioned above and CO2 reduction in mized based on the protocol proposed. In addition, the pilot plant
environmental aspects. Currently, Korea has established green- was operated for 2 months under the optimized operating condi-
house gas(GHG) reduction roadmap in order to reduce GHG tions to investigate the costs saved.
estimation for 2020 business-as-usual by 30% and is enforcing
varous national policies to reduce CO2 emission. Drinking water 2. Materials and methods
and wastewater treatment field also needs to develop and
study new technologies to reduce CO2 (Kim et al., 2011). The 2.1. Experimental setup
operating condition optimization of chemical cleaning in mem-
brane filtration process is considered to be one of the ways to This study was conducted using a pressurized UF membrane
satisfy this. filtration process for drinking water treatment in a pilot-scale plant
In order to optimize operating condition, it is important to un- installed in an existing drinking water treatment facility. The
derstand the characteristics of accumulated irreversible fouling, a schematic diagram of the pilot-scale plant is illustrated in Fig. 1. A
very complicated phenomenon where membrane characteristics pressurized UF membrane developed by Cheil industry, made of
(membrane materials, pore size, configuration, hydrophobicity, PVDF, pore size 0.01 mm, surface area 72 m2 and length 2.16 m, was
charge), process operating conditions (TMP, temperature, permeate used as the membrane module. Raw water was collected from the
flux), and the physicochemical characteristics of the influent (par- front part of sand filtration unit in the water treatment facility, and
ticle size distribution, inorganic or organic mattes) closely influence three samples a week were collected for analysis. The pH and
each other. Hence, it is difficult for general operators to correctly conductivity of raw water was determined using DWA-2000A and
understand the characteristics of irreversible fouling and deter- YSI-30, respectively, and its turbidity was analyzed using HACH
mine appropriate operating conditions (Al-Amoudi and Lovitt, SC200. GE 5310C was used for the analysis of TOC and DOC, and
2007; Gao et al., 2011; Kimura et al., 2004). Additionally, exten- HACH DR4000 was used for UV254. Inorganic materials, such as Fe
sive experiments need to be conducted to optimize factors that and Mn, were analyzed using the standard 3120D digestion method
affect chemical cleaning itself, such as the chemical interval, employing ICP-AES. The characteristics of raw water used are pre-
duration, reagent, and concentration (Gernaey et al., 2004). Thus, it sented in Table 1. Operating mode was cross-flow with permeate
is not practical to perform such experiments at pilot- or full-scale in time of 29 min and backwash time of 1 min. Permeate flux was
terms of cost and time. Therefore, most membrane filtration facil- 80 l m2 h1, backwash flux was 120 l m2 h1, and the air flow of
ities in operation conduct chemical cleaning using vendor air scrubbing during backwash was 0.3 Nm3 h1 m2.
Table 1
Concentrations of influent raw water.
only one backwash was performed per week, without chemical For the chemical reagent which was not included in the national LCI
cleaning, and the permeate flux used was 140 l m2 h1 that is database, an ecoinvent database developed by Switzerland was
higher than the critical flux for irreversibility determined in step 1. used. The parameter and sources of the LCI database used was
To investigate irreversible foulant, fluorescence excita- shown in Table 2.
tioneemission matrices (FEEM) (Tecan Xflour4 Safire II, Germany),
and Fourier-transform infra-red (FTIR) (Vertex 70, Bruker, MA, USA)
analyses were performed. 3. Results and discussion
2.3.3. Operating condition optimization 3.1. Determination of critical flux for irreversibility (step 1)
RSM was performed in the order of experimental design,
response surface design analysis, and response surface analysis Permeate flux can be divided into critical flux, threshold flux,
optimization. A central composite design (CCD) was used to design critical flux for irreversibility, and limiting flux (Field et al., 1995;
experiments randomly. After the experiment was designed, Luo et al., 2012). The critical flux for irreversibility represents the
response surface design analysis was carried out on the results and transition between reversible and irreversible fouling (Chu et al.,
quadratic regression models with an independent variable k were 2014). In other words, as irreversible fouling is formed only above
determined, as shown in Eq. (4). the critical flux for irreversibility, and not below, operating at the
critical flux for irreversibility can result in minimizing the interval
X
k X
k X
k
of chemical cleaning and maximizing treatment of water. There-
Y ¼ b0 þ bi $xi þ bii $ x2i þ bij $xi $xj þ ε (4)
fore, the critical flux for irreversibility was determined as the most
i¼1 i¼1 ij
efficient permeate flux for saving operating costs.
where, Y is the response variable, xi and xj are the ith and jth coded The fouling rate and membrane resistances were calculated
independent variables, respectively. with the flux and TMP data obtained using the modified flux-step
To test the validity of the determined regression models, t-test, method. The results are presented in Fig. 3.
analysis of variance (ANOVA), lack-of-fit test, residual analysis, and When the permeate flux was between 20 l m2 h1 and
calculation of root mean square error (RMSE) for experiment data 80 l m2 h1, Ftot and Firrev were nearly constant at 0.51 kPa h1 and
and predicted data were conducted. The calculation of RMSE was 0.15 kPa h1, respectively. The Ftot rapidly increased to 3.58 kPa h1
based on Eq. (5) below. at 100 l m2 h1, beyond which, Ftot increased with the permeate
flux, reaching 20.25 kPa h1 at 160 l m2 h1. Firrev remained con-
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
Pn 2
stant at 0.15 kPa h1 when the permeate flux was increased to
i¼1 ðXi Yi Þ 100 l m2 h1. However, when the permeate flux was increased to
RMSE ¼ (5)
n1 120 l m2 h1, Firrev rapidly increased to 0.63 kPa h1, a phenom-
enon called TMP-jumping, and kept constantly increasing to a
where, Y is the response variable; xi and xj are the ith and jth coded maximum level of 3.61 kPa h1.
independent variables, respectively, Xi is the experimental data, Yi In order to select the critical flux for irreversibility, both fouling
is predicted data by regression models and n is the number of ex- rate and membrane resistance were calculated. Membrane resis-
periments performed. tance was calculated using Eq. (3) and the result is shown in Fig. 4.
As the number of response variables to be optimized was one or In this study, the resistance of clean membrane (Rm) was
more, multiple response surface methodology (MRSM) was used 4.80 1011 m1. The resistance caused by surface or pore adsorp-
(Ahn et al., 2014; Myers et al., 2009). The desirability function, tion regardless of the flux (Rads) was 0.42 1011 m1. The resistance
which is an efficient method of to standardize the result values caused by the reversible component (Rrev) when the permeate flux
with different units by converting the results into values between was 20e80 l m2 h1 occurred at insignificant levels and was
0 and 1, was used. The desirability value of 1 means an access with ignored; the resistance caused by the irreversible component (Rir-
great satisfaction to the target to be sought for, while 0 means that 11 1
at 100 l m2 h1 resulting in the
rev) was 0. Rrev was 0.3 10 m
the result was obtained below a criterion. Overall desirability is 2 1
increase of Rtot. Even at100 l m h , Rirrev barely increased. Rirrev
defined by the geometric mean of respective desirability, which is started to increase at 120 l m2 h1 and kept increasing till
available as a rating scale of the MRSM optimization (Li et al., 2007). 160 l m2 h1.
The critical flux for irreversibility that minimizes the
2.4. Calculation of operating cost and CO2 emission frequency of chemical cleaning with the most efficient
operating cost was 100 l m2 h1. The reason is that the irre-
Operating costs with the vendor recommended conditions were versible fouling rate started increasing rapidly at 100 l m2 h1.
compared with those of optimized conditions. The pilot-scale plant In addition, the vendor recommended permeate flux of was
used in this paper was operated for two months under the opti- 80 l m2 h1 was determined to be the threshold flux. The dif-
mized conditions. Operating costs, energy (power) cost, chemical ference in operating costs created by increasing the permeate
cost, and sludge disposal cost were calculated, while the common flux from 80 l m2 h1 to 100 l m2 h1 is discussed in detail in
costs such as labor and membrane replacement were not section 3.4.
considered.
The CO2 emissions reduction by chemical cleaning optimization
of membrane filtration process were calculated through the Global Table 2
LCI database source used in this study.
Warming Potential (GWP) category of life cycle assessment (LCA).
The LCA analysis was carried out using a TOTAL program, a Parameter Source
modeling program developed by Korea Environmental Industry Electricity Korea LCI databasea
and Technology Institute. As a life cycle inventory (LCI) database, a Sludge disposal
national LCI database developed by the ministry of environment Chemical reagent (NaOCl) Ecoinventb
and the ministry of knowledge and economy, and provided by the a
www.epd.or.kr.
b
korea environmental industry and technology Institute, was used. www.ecoinvent.org.
1130 S.S. Yoo et al. / Journal of Environmental Management 206 (2018) 1126e1134
Fig. 3. Variation of fouling rate with flux - Change in total membrane fouling rate (Ftot) Fig. 5. Effect of various chemical reagents on restoration ratios: Bar graph shows ef-
and irreversible fouling rate (Firrev) with increase in flux, assessed using modified flux- fects of cleaning using citric acid, NaOH and NaOCl on removal of irreversible fouling;
step method. where J0 is pure water permeability before chemical cleaning, and J1is pure water
permeability after chemical cleaning.
h
YCost ¼ 10:517X1 þ 2:503X2 þ 0:53X3 þ 7:097X12 þ 0:004X22
Where, X1, X2, and X3 are chemical interval, duration time, and
chemical concentration, respectively.
Statistical significance tests were conducted to consider the
applicability of the regression models. ANOVA, t-test, lack-of-fit
test, residual analysis, and comparison between experimental
data and predicted data were conducted. As result of t-test and
ANOVA, TMP increasing rate and operating cost regression models
were shown to be significant in all 1st order terms, 2nd order terms,
and interaction terms (p ¼ 0.05) in which each coefficient was also
significant (p < 0.05). Coefficient of determination (R2) of TMP
increasing rate and operating cost regression models were both
very high at 94.57% and 99.77%, respectively and the prediction of
response values deduced through regression models was expected
to show high accuracy. For TMP increasing rate, influence of 1st
order terms were larger than 2nd order terms and interaction
terms, and it was deducted that change of X2 among 1st order
terms showed most influence on the result values. In the case of
operating cost, influence of 1st order terms and 2nd order terms
were larger than interactions terms, and X1 and X21 had high in-
fluence on result values. As result of lack-of-fit test, p value of the
TMP increasing rate regression model was 0.634 and p value of the
operating cost regression model was 0.811. The null hypothesis
‘Occurred change is 0 because the regression model is not suitable’
was selected because both regression models were not significant
(p > 0.05). Thus, the influence of high-order terms, which were
Fig. 6. Fluorescence EEM of organic matter desorbed by (a) NaOCl, (b) NaOH - Organic
removed during the deduction of regression models, on response
matter desorption by NaOCl showed highest peaks at 360e400 nm/230e260 nm
(emission/excitation) and 430e470 nm/230e250 nm (emission/excitation). Organic
matter desorption by NaOH showed minor peak that was evenly distributed in the
whole domain of organic matter in addition to a main peak at 390e480 nm/
230e240 nm (emission/excitation). Red color is higher in concentration than green
color. (For interpretation of the references to colour in this figure legend, the reader is
referred to the web version of this article.)
Table 3
Ranges of operating conditions coded.
1 0 1
Fig. 10. CO2 emission of the vender recommended and optimized conditions by the
LCA.
Table 4 emission by chemical use, energy use, and sludge disposal was
Central Composite Design of operating conditions coded in operating cost and TMP 0.195 g CO2/m3, 112.241 g CO2/m3, and 0.314 g CO2/m3, respectively.
increasing.
It was calculated that energy use, i.e. CO2 emission by electricity use
Factors Operating cost ($/m3) TMP increasing (%) occupied over 99% of the total emission and that as a result of
Run X1 X2 X3 Predicted Experimental Predicted Experimental optimization, CO2 emission was reduced by about 26.5%, like in
operating cost. Based on this result, it is considered to be most
1 0 0 1 0.12446 0.12421 3.75279 2.45614
2 0 0 0 0.12392 0.12392 3.64434 3.50877 effective to develop a low energy operating system in water
3 1 1 1 0.13774 0.13745 6.43242 7.28070 treatment field, to reduce carbon dioxide.
4 1 1 1 0.12001 0.11959 11.55522 11.40351
5 0 0 0 0.12392 0.12392 3.64434 3.68421
6 0 0 0 0.12392 0.12392 3.64434 3.24561 4. Conclusions
7 1 1 1 0.12022 0.12007 10.12539 9.64912
8 0 1 0 0.12142 0.12256 7.40192 7.89474 This study investigated the operating cost and CO2 emission
9 0 1 0 0.12643 0.12528 1.57736 0.96491
reduced by optimizing the operating conditions for chemical
10 1 0 0 0.14153 0.14152 2.13876 1.31579
11 0 0 0 0.12392 0.12392 3.64434 4.64912 cleaning used to improve the membrane filtration process. A new
12 1 0 0 0.12050 0.12051 5.52472 6.22807 protocol that can be easily used in the field was proposed. Opti-
13 0 0 0 0.12392 0.12392 3.64434 3.59649 mization of operating conditions for EFM was tested using a pres-
14 0 0 1 0.12340 0.12364 5.84051 7.01754
surized UF membrane facility currently in operation. In addition, a
15 0 0 0 0.12392 0.12392 3.64434 3.42105
16 1 1 1 0.12115 0.12143 2.32715 3.07018
pilot plant was operated under the optimized operating conditions
17 1 1 1 0.14711 0.14753 0.25698 0.43860 identified to compare costs of operation, energy, chemicals, and
18 1 1 1 0.13612 0.13585 6.85347 6.14035 sludge disposal.
19 1 1 1 0.12065 0.12094 6.08154 5.26316 A flux-stepping test was performed with a modified flux-step
20 1 1 1 0.14520 0.14536 3.00259 3.50877
method to determine the permeate flux. Ftot and Rrev rapidly
increased from 100 l m2 h1, while Firr and Rirrev rapidly increased
from 120 l m2 h1. Based on the analysis, the critical flux for
Chemical cost was reduced by 37.5% from $0.0030/m3 to irreversibility was selected as 100 l m2 h1, and the existing
$0.0019/m3. Cost was reduced despite an increase in the chemical vendor recommended flux of 80 l m2 h1 was determined as the
concentration used by 2.5 times, due to prolongation of the interval threshold flux.
by over three times. Energy cost was reduced by 22.5% from The permeability recovery rate and irreversible foulant of
$0.1479/m3 to $0.1142/m3. The effect of operating time saved by chemicals were examined to select an appropriate chemical for the
increasing the permeate flux is larger than the cost incurred by the cleaning. It was found that major irreversible foulants were organic
use of a permeate pump. Sludge disposal cost was reduced by 75% as the permeability recovery rate of NaOH and NaOCl was higher,
from $0.0105/m3 to $0.0026/m3. As a result, the total operating cost while that of citric acid was low. The examination of the irreversible
was $0.1187/m3, which is 26.5% lesser compared to the operating foulant through FEEM and FTIR also confirmed that major foulants
cost under a vendor recommended setup, and similar to the were the organic materials like humic acid that have aromatic and
amount predicted by the regression model. This study found that alkene functional groups. Thus, NaOCl, which is specialized in
the effect of operating cost savings achieved through optimization removing organic materials such as humic acid was selected as the
of operating condition for chemical cleaning was excellent. In appropriate chemical.
addition, the effect of saving initial investment costs, such as the The operating conditions of EFM including chemical interval,
decrease of modules due to membrane life and an increase in the duration and concentration, were optimized through RSM. Re-
filtration flux from optimization, were not included. If these factors sponses were the operating cost and TMP increasing ratio, and
are additionally considered, the operating cost savings would be regression models for the responses were developed. The regres-
much higher. sion models were fit based on validity tests including t-test,
When the membrane filtration process was operated in the ANOVA, and lack-of-fit test. The result of multiple response surface
vender recommended condition, CO2 emission by chemical use, optimization showed that the operating cost and the TMP
energy use, and sludge disposal was 0.311 g CO2/m3, 145.439 g CO2/ increasing rate were minimized at an interval of 6.3 d, concentra-
m3, and 1.245 g CO2/m3, respectively and when the membrane tion of 500 ppm, and duration of 76 min. In this setting, the ex-
filtration process was operated in the optimized condition, CO2 pected operating cost was $0.121/m3, and the TMP increasing rate
Table 5
Comparison of operating factors between vendor recommended conditions and optimized condition.
Permeate flux (l m2 h1) Chemical reagent Interval (day) Concentration (ppm) Duration (min)
Table 6
Comparison of unit cost ($/m3) between the vender recommended and optimized conditions.
was 2.021%. membrane filtration with water industry applications. Adv. Colloid Interface Sci.
164, 38e44.
A pilot-plant was operated for a long-term under the optimal
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agencies in the public, commercial, or not-for-profit sectors. tion in glutamine production. Appl. Microbiol. Biotechnol. 74, 563e571.
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associated with this publication and there has been no significant organic load industrial effluents: from lab to pilot scale. J. Environ. Manag. 131,
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