Separation and Purication Technology 54 (2007) 329339

Cleaning-in-place coupled with membrane regeneration

for re-using caustic soda solutions
G. G esan-Guiziou
a,
, N. Alvarez
b
, D. Jacob
a
, G. Daun
a
a
INRA, Agrocampus Rennes, UMR 1253, Science et Technologie du Lait et de lOeuf, 65 rue de Saint Brieuc, F-35000 Rennes, France
b
GES, Les basses Forges, 35 530 Noyal sur Vilaine, France
Received 9 August 2006; received in revised form 5 October 2006; accepted 9 October 2006
Abstract
Industrial use of soda cleaning-in-place (CIP) solution in dairy plants yields a modication of the composition of the cleaning solution (suspended
solids, SS; chemical oxygen demand, COD; surface tension, ). The increase of SS and decrease of generate decreased and enhanced cleaning
performances, respectively. The paper aims at determining the more appropriate regeneration operation (ltration, centrifugation) by modelling
and simulating coupled regeneration CIP process on industrial assumptions and at designing and sizing the coupled CIP process according to the
required physicochemical characteristics (SS, , COD) and cost.
The coupling of re-use CIP with membrane regeneration (microltration, ultraltration and nanoltration) makes it possible to control the
functional characteristics of the solution (SSand maintained under critical values) as opposed to centrifugation and decantation. The discontinuous
mode is to be preferred regarding the caustic solution composition and functionality, but the continuous mode is simpler to use at a lower capital
cost. The microltration operation seems to be the more appropriate operation: surfactants are only slightly retained and costs are reduced; however
COD content of re-used solutions are relatively high compared to values obtained with ultraltration and nanoltration. In case of very high levels
of COD in re-used caustic soda solutions, cleaning efciency and kinetics should be further investigated.
2006 Elsevier B.V. All rights reserved.
Keywords: Cleaning-in-place; Coupled membrane process; Soda; Regeneration; Simulation
1. Introduction
Cleaning-in-place (CIP) systems are commonly used in the
food industry for ensuring hygienic safety of foods and for
recovering plants performances. Caustic soda (NaOH) solutions
are the most commonly used chemical cleaning detergent on
an industrial scale [1]. These solutions are either discharged
after one use (single-use system) or re-used before being dis-
charged and renewed (multi-use and re-use systems [2,3]). The
frequency of cleaning solutions discharge varies according to
the dairy equipment and plants to be cleaned (1 day1 year) but
is solely based on subjective criteria such as colour or odour of
the solutions.
Re-use of caustic cleaning solutions in dairy plants results in
modications of its composition: increase in suspended solids

Corresponding author. Tel.: +33 2 23 48 53 25; fax: +33 2 23 48 53 50.

E-mail address: genevieve.gesan-guiziou@rennes.inra.fr
(G. G esan-Guiziou).
(SS) and in chemical oxygen demand (COD), accompanied by a
decrease in surface tension () [47]. Recent works have shown
that during CIP with re-used NaOH solutions the decrease of
results in higher cleaning efciency and cleanliness of ultral-
tration membranes fouled with skimmed milk [6] and in a much
faster cleaning rate [8]. However, the increase of SS, simulta-
neously observed with the decrease of is detrimental to the
cleaning rate [8].
Membrane operations for regeneration of caustic cleaning
solutions such as microltration (MF), ultraltration (UF) and
nanoltration (NF) are relevant for both ensuring the recovery of
NaOHsolutions and reducing the load of industrial solutions dis-
charge [915]. Industrial membrane regeneration systems such
as MF [1618], UF [19] and NF [20] operate in order to simul-
taneously control the composition of the cleaning solution and
reduce the caustic rejections and the volume of the overall waste
stream. However, the choice of ltration operation is generally
done on a limited number of criteria, where the evolution of
the soluble COD (COD
S
) with time in regenerated NaOH solu-
tion is taken into account without considering the evolution of
1383-5866/$ see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.seppur.2006.10.007
330 G. G esan-Guiziou et al. / Separation and Purication Technology 54 (2007) 329339
Nomenclature
A
m
membrane area (m)
C concentration of pollution in the CIP tank (g L
1
)
C
max
maximum pollution concentration in CIP tank
(g L
1
)
C
p
concentration of pollution in the permeate (g L
1
)
CIP cleaning in place
COD chemical oxygen demand (g
O
2
L
1
)
COD
S
soluble chemical oxygen demand (g
O
2
L
1
)
Input
CODs
increase rate of soluble chemical oxygen
demand in the CIP tank (g h
1
)
Input
SS
increase rate of suspended solids in the CIP tank
(g h
1
)
J permeation ux (Lh
1
m
2
or ms
1
)
MF microltration
n
c
number of cycle
NF nanoltration
Q
CIP
cleaning ow rate (m
3
s
1
)
Red
CODs
reduction of soluble chemical oxygen demand
SS suspended solids (g L
1
)
t
c
duration of cycle (h or s), t
c
=t
f
+t
Cl
t
Cl
duration of cleaning (h or s)
t
f
duration of ltration (h or s)
TP transmembrane pressure (Pa or bar)
UF ultraltration
V
CIP
volume of CIP solution to be treated (m
3
)
V
FB
fed-batch retentate compartment volume (m
3
)
VRR volume reduction ratio
Indices
c constant
h high
i intermediate
l low
v variable
Greek symbols
surface tension (mJ m
2
)
P pressure drop (Pa or bar)
SS and , which are the major parameters in terms of clean-
ing performances [8,13]. Moreover, when equations proposed to
describe the evolution of the composition of used caustic soda
solution in coupled membrane CIP systems are considered, they
are incomplete; they are actually based on simplifying assump-
tions such as constant permeation ux (J) or soluble chemical
oxygendemandreduction(Red
CODs
), whichare never veriedin
practice [21].
The paper aims at determining the more appropriate mem-
brane regeneration operation by modelling and simulating
coupled regeneration CIP process on industrial assumptions and
at designing and sizing the coupled CIP process according to
the required physicochemical characteristics (SS, , COD
S
) and
cost. In that accord, the model proposed by Dresch et al. [21] was
improved in order to describe simultaneously the evolution of
COD
S
, SS and in industrial conditions. The developed model
was based on realistic industrial assumptions of simulation (evo-
lution of J and Red
CODs
in the course of the time; stops of
the regeneration system for membrane cleaning). The obtained
results will be compared with another mode of regeneration, i.e.,
discontinuous centrifugation.
2. Theoretical background and assumptions
2.1. Description of CIP regeneration system: assumptions
Several assumptions related to the CIPand to the regeneration
solution systems have been chosen.
2.1.1. Cleaning-in-place system mode of operation
Assumptions on the CIP system mode of operation were
similar to those proposed by Dresch et al. [21]:
- The system operates in continuous mode, 24 h a day,
at constant volume, V
CIP
=10 m
3
(in industrial conditions:
0.5 V
CIP
20 m
3
);
- The ow rates in and out of the CIP system, Q
CIP
are constant
and equal;
- The amount of foulant matter increases in the re-used NaOH
cleaning solutions in the course of cleanings: the input rate
of contamination in COD
S
, Input
CODs
, and SS, Input
SS
,
in the CIP tank, are supposed to be constant over time:
Input
CODs
=800 g h
1
and Input
SS
=200 g h
1
[21]. In reality,
a fraction of contaminated solutions is drained to the puri-
cation station during the sorting out of uids (waterNaOH
solution and NaOH solutionwater). The addition of fresh
NaOH used to adjust the concentration of cleaning solution
in the CIP tank induces therefore a progressive dilution of SS
and COD
S
. This point has already been conrmed by previous
measurements on industrial NaOH solutions coming from a
milk standardization plant [5]: the contamination of the CIP
solution with SS and COD
S
, measured over 1 week, linearly
increases in the course of the rst cleanings and levels off
after about 200 cleanings. The progressive dilution is not
taken into account in our calculations: the real contamination
in the CIP tank is therefore lower than the calculated value, in
particular for COD
S
, not retained by MF and centrifugation;
- The lost of OH

ions, consumed by the reactions of

chemical hydrolyses with the deposit are not taken into
account;
- The systemis consideredas closed: the additionof freshNaOH
to compensate for the lost volume during the sorting out of
uids is not taken into account;
- The volume mass (kg m
3
) of the used NaOH solutions is
supposed constant.
2.1.2. Regeneration system mode of operation
The CIP system is coupled to a regeneration system, which
can be either a ltration running in continuous mode (Fig. 1a) or
in discontinuous mode (Fig. 1b), or a centrifugation in discon-
tinuous mode (Fig. 1c). During the regeneration in continuous
G. G esan-Guiziou et al. / Separation and Purication Technology 54 (2007) 329339 331
Fig. 1. Cleaning-in-place system coupled with regeneration of cleaning solu-
tions. (a) Continuous membrane regeneration, (b) discontinuous membrane
regeneration and (c) regeneration with discontinuous centrifugation. Symbols:
see list of abbreviations.
mode, the regeneration operation runs on the running CIPsystem
tank. During the regeneration in discontinuous mode (ltration
or centrifugation), the regenerated NaOH solution runs in the
CIP system while the contaminated solution regenerates in a
second tank. A third tank is therefore added to collect the regen-
erated solution (Fig. 1b and c).
The periodical draining is performed after 1 week: cycle
duration, t
c
=168 h; regeneration duration, t
f
=166 h; cleaning
duration, t
CIP
=2 h. Under industrial conditions, the draining
period is in the range <1 day1 year.
2.1.2.1. Volume reduction ratio, VRR. Regardless of the regen-
eration mode (ltration or centrifugation), the systems run in
fed-batch mode [21] up to a given VRR, with a periodical stop
for cleaning.
VRR quanties the reduction of volume completed by the
membrane or centrifugation operation at the end of the operation
t
f
(h). It is calculated according to:
VRR =
V
treated
V
residue
(1)
where V
treated
is the volume to be treated (m
3
) and V
residue
is
the residual volume after regeneration (m
3
). It corresponds to
V
pellet
which is the volume in the centrifuge pellet (m
3
) or V
FB
which is the holding volume of the retentate compartment of the
ltration system (m
3
).
In previous work, V
FB
=0.125 m
3
[21].
For a discontinuous ltration operation [21]:
VRR =
V
FB
+A
m

t
f
0
J(t) dt
V
FB
(2)
where A
m
is the membrane area (m
2
) and J is the permeation
ux (Lh
1
m
2
).
Table 1
Simulation of CIP systemcoupled with membrane regeneration in continuous mode: characteristics of chosen combinations permeation ux (J)reduction of chemical
oxygen demand (Red
CODs
)
Combination JRedCODs Operation J (Lh
1
m
2
) Red
CODs
A
m
a
(m
2
) Reference
Constant
[J
h
RedCODs =0]
c
MF
b
266.8 0 0.226 [21]
[J
i
RedCODs
i
]
c
UF
b
166.8 0.217 0.361 [21]
[J
l
RedCODs
h
]
c
NF
b
56.8 0.317 1.061 [21]
Variable
[J
h
RedCODs =0]
v
MF
b
0.4t +300
c
0 0.226 [4]
[J
i
RedCODs
i
]
v
UF
b
0.4t +200
c
0.001t +0.3
c
0.361 [4]
[J
l
RedCODs
h
(1)]
v
d
NF
b
0.4t +90
c
0.001t +0.4
c
1.061 [5,22]
[J
l
RedCODs
h
(2)]
v
d
NF
b
0.4t +90
c
0.00341t +0.6
c
1.061 [5,22]
[J
l
RedCODs
h
(3)]
v
d
NF
b
6 ln(t +0.05)0.22317 t +100
c
0.001t +0.4
c
1.061 [5,22]
Indices: c, constant vs. time; h, high; i, intermediate; l, low; v, variable vs. time.
a
A
m
, membrane area required to reach VRR=80 in a ltration time, t
f
=166 h.
b
Membranes used: MF, multichannel tubular inorganic membrane (Kerasep, Orelis, Miribel, France) 19 channels, 0.1 m mean pore diameter. UF, multichannel
tubular inorganic membrane (Kerasep, Orelis, Miribel, France) 19 channels, 300 kg mol
1
cut-off. NF, prototype solgel (Kerasep, Orelis, Miribel, France) 19
channels, lactose (1g L
1
) retention =0.35.
c
time, t in h.
d
Three different cases ((1), (2) and (3)) of J
l
RedCODs
h
evolutions in nanoltration, NF runs were considered according to previous experimental work [5,22].
332 G. G esan-Guiziou et al. / Separation and Purication Technology 54 (2007) 329339
For a continuous ltration operation:
VRR =
A
m

t
f
0
J(t) dt
V
FB
(3)
Eqs. (2) and (3) permit to calculate the membrane area, A
m
required to reach a target VRR (=80 arbitrary) according to the
J level at the end of the ltration (t =t
f
) (Table 1).
Regardless of the operation (ltration or centrifugation), the
nal VRR is considered as equal. This hypothesis is realistic
according to Dresch [4].
2.1.2.2. Reduction of COD
S
and SS; evolution of J. Regardless
of the ltration operation, reduction of suspended solids and
caustic soda are considered total and nil, respectively (Red
SS
=1,
Red
NaOH
=0), in agreement with the experimental results of
Dreschet al. [9]. The reductionof COD
S
(Red
CODs
) is denedas:
Red
CODs
= 1
C
p
C
(4)
where C
p
(g L
1
) is the COD
S
concentration in the permeate
compartment and C (g L
1
) is its concentration in the CIP tank.
For the centrifugation operation, Red
NaOH
=0, Red
SS
=0.3
and Red
CODs
=0 [4].
Three hypotheses are proposed to describe the evolution of
the permeation ux, J and the reduction of COD
S
, Red
CODs
in
the course of the time:
- J and Red
CODs
vary linearly with time according to previously
reported laws obtained in conditions comparable to industrial
operation: MF, UF [4] and NF [5,22] (Table 1);
- J (for values J <120 Lh
1
m
2
) varies according to non-linear
relationship in order to simulate a real ltration operation
[5,22] and Red
CODs
varies linearly (Table 1);
- J and Red
CODs
are constant (noted as [J, Red
CODs
]
c
in Table 1)
[21]; the values of J and Red
CODs
are chosen, for each
JRedCODs couple, as the mean values of variables J and
Red
CODs
during t
f
(Table 1).
The combinations of JRed
CODs
are representative of MF,
UF and NF operations (Table 1).
2.2. Coupling of cleaning and regeneration systems
2.2.1. Modelling the evolution of the characteristics of
cleaning solutions
2.2.1.1. Surface tension, . Surface tension, is calculated
from COD
S
values. The experimental relationships between
(mJ m
2
) and COD
S
(g L
1
) have been established with indus-
trial NaOH solutions sampled from industrial single-use and
re-use CIP systems, at 50

C [8]:
= 74.0 for COD
S
= 0 g L
1
(fresh caustic soda)
= 39.1 6.5 ln[COD
S
] for 0 < COD
S
4 g L
1
= 30.0 for COD
S
> 4 g L
1
(5)
The surface tension of industrial solutions after nanoltra-
tion is low ( 35 mJ m
2
) and generally slightly higher than
surface tension of the initial solutions: +23 mJ m
2
[4]. In the
simulations performed, the slight increase in of the ltrate is
not taken into account: is considered as depending exclusively
on COD
S
concentration in the CIP tank.
2.2.1.2. Suspended solids, SS; soluble chemical oxygen
demand, COD
S
. In the case of periodical draining, the evolu-
tion of the COD
S
concentration in the CIP solution, C (g L
1
)
is calculated according to Dresch et al. [21]:
C(t) =
Input
CODs
V
CIP
t (6)
where t is the operating time of the CIP system since the last
draining (h).
After drainingandrenewal, C(t) is decreaseddownto0 g L
1
.
In the case of regeneration in a discontinuous mode (ltration
or centrifugation), the solution is regenerated during a cycle,
t
c
(equal to the durations of the ltration, t
f
and of membrane
cleaning, t
Cl
) and the regenerated solution is readjusted to V
CIP
with fresh NaOH at the end of the regeneration. According to
Dresch et al. [21], the maximum concentration of COD
S
in the
regeneration tank, at the end of the n
c
cycle, C
max
(n
c
) is given
by:
- whenever Red
CODs
=1:
C
max
(n
c
) =
Input
CODs
t
c
V
CIP

n1

i=0

(1 Red
CODs
)
i

1
1
VRR

(7)
- whenever Red
CODs
=1
C
max
(n
c
) =
Input t
c
V
CIP
(8)
In the case of a continuous mode ltration, the mass balance
in the CIP tank during the regeneration leads to [21]:
dC(t)
dt
+
J(t) Red
CODs
(t) A
m
V
CIP
C(t) =
Input
CODs
V
CIP
(9)
When J and Red
CODs
are not constant, in opposition to ideal
systems previously described [21,23], the concentration in the
CIP tank is calculated (from Eq. (9)) by numerical integration:
the C
i+1
concentration at time t
i+1
is calculated from the C
i
concentration at time t
i
:
C
i+1
= C
i

1
(J
i+1
+J
i
)(Red
CODs
i+1
+Red
CODs
i
)A
m
4 V
CIP
(t
i+1
t
i
)

+
Input
CODs
V
CIP
(t
i+1
t
i
) (10)
At t =0, the concentration of COD
S
in the CIP tank is equal to 0.
At the beginning of each cycle, after the membrane cleaning, the
calculated concentration in the CIP tank takes into account both
the addition of fresh NaOH required to compensate for the lost
G. G esan-Guiziou et al. / Separation and Purication Technology 54 (2007) 329339 333
retentate volume and the pollution brought by the CIP system
during the interruption of regeneration system for membrane
cleaning. The initial concentration, C
0
for the next regeneration
cycle is consequently given by:
C
0
=
V
CIP
C
t
+Input
CODs
t
Cl
V
CIP
+V
FB
(11)
where C
t
is the concentration in the CIP tank before the mem-
brane cleaning (g L
1
).
From Eqs. (10) and (11), the evolution of SS, COD
S
and
then in the CIP tank can be calculated in the course of time.
The accuracy of C due to the calculation method of Eq. (10) is
2%.
2.2.2. Cost modelling
2.2.2.1. Investment costs. The investment cost of a centrifuge
(5006000 Lh
1
; 22 kW) is estimated at D 90,000.
The investment cost of a ltration pilot including pumps,
sensors, tanks, pipes, regulations and membrane modules is
D 61,000. The ltration modules are composed of 7 mem-
brane tubes (19 channels 3.5 mm1.2 m) in series or parallel.
A 10 m
3
thermally isolated stainless steel tank is estimated at
D 30,000.
2.2.2.2. Operating costs. The operating costs of the centrifuge
are divided into three stations:
- Energy(D 0.05 kWh
1
): for runningthe centrifuge andheating
the solutions from 20 to 70

C according to:
E = mC
water
T (12)
where m is the mass of solutions to be heated (kg), C
water
the specic heat of water (=4.18 kJ kg
1
K
1
) and T is the
difference in temperature (K) (50 K).
- Readjustment of the cleaning solution with fresh NaOH
solution, considering the cost of NaOH at D 0.4 kg
1
and
the price of water (purchase and treatment) at D 1.52 m
3
.
The volume of readjustment is estimated at 1 V
FB
NaOH
(20 g L
1
).
- Labour: 10 min/cycle of duration t
c
(at D 22 h
1
) for monitor-
ing the centrifuge.
The operating costs of the ltration operations are divided
into four stations:
- Inorganic membrane replacement (D 3000 m
2
), with an esti-
mated lifetime of 6 years;
- Cleaning of membranes: the volume of required water is
assumed to be equal to 4 V
FB
: 2 V
FB
of water for rinses, 1
V
FB
for complex detergent (10 g L
1
) for membrane cleaning
and 1 V
FB
of NaOH (20 g L
1
) for readjusting the CIP solu-
tion volume (NaOH, D 0.4 kg
1
; water, D 1.52 m
3
; complex
detergent, D 2.7 kg
1
);
- Labour (D 22 h
1
): 10 min/cycle of duration t
c
for monitoring
an automated ltration plant;
- Energy for pumping and heating (D 0.05 kWh
1
).
The energyrequiredfor heatingthe solutions from20to70

C
is calculated following Eq. (12). Loss of heat during ltration is
negligible.
According to running hypotheses, in fed-batch mode, the out-
put pressure of the pump should be at least equal to the sum of
the chosen mean transmembrane pressure, TP and of half the
pressure drop of the plant. The pump works with a uid having
a relative pressure equal to zero, since the retentate is recycled
into a tank at atmospheric pressure [4]. The energy required
for the circulating the uids in the ltration loop is therefore
calculated according to:
P =
Q

TP +
P
2

(13)
where is the pump yield and Qis the volumetric owrate in the
ltration module. Q is calculated from crosssections and cho-
sen crossow velocity of each ltration system (MF, 7.0 ms
1
;
UF, 7.0 ms
1
; NF, 2.7 ms
1
). TP is the transmembrane pres-
sure (Pa). The values used for the simulation were extracted
fromexperiments performed by Dresch [4]: 0.5 10
5
Pa for MF,
1.2 10
5
Pa for UF and 4.0 10
5
Pa for NF. P is the pressure
drop in the plant (Pa), calculated by adding 20%excess pressure
drop to the pressure drop of a smooth membrane evaluated by
Blasius (P
Blasius
). The 20% extra pressure takes into account
the membrane rugosity and pressure drop at the entrance and at
the outlet of the membrane module [4]:
P = 12 P
Blasius
and
P
Blasius
= 0.16 L
m
d
1.25
c

0.75
v
1.75

0.25
(14)
where L
m
is the membrane length (m), the retentate volu-
metric mass, 1000 kg m
3
, the retentate dynamic viscosity,
0.45 10
3
Pa s and d
c
is the channel hydraulic diameter,
3.5 10
3
m.
2.2.2.3. Savings generated by the regenerationre-use of the
NaOH solution. The reference system is a CIP system with
either a weekly draining of the CIP tank or a draining at a given
chosen concentration, equal to a limiting concentration. Savings
are calculated considering the following:
- consumed water and NaOH solution;
- energy required to heat the total volume of the CIP system to
70

C after every renewal.

2.2.2.4. Pay-back time. If the annual operating cost is lower
than the performed savings, the pay-back time, PB is calculated
according to:
PB =
I
S
AN
RC
AN
(15)
where I is the investment (D ), S
AN
the annual savings (D /an) and
RC
AN
is the annual operating costs (D /an).
If the annual operating cost is higher than the performed
savings, the process is not economical.
334 G. G esan-Guiziou et al. / Separation and Purication Technology 54 (2007) 329339
3. Results and discussion
The impact of the characteristics of the crossow ltration
(different couples [J, Red
CODs
] and A
m
, representative of MF,
UFandNFoperations (Table 1)) onthe compositionof the regen-
erated caustic solutions (COD
s
and SS concentrations, values)
is studied using Eqs. (10) and (11). This study enables to dene
the most appropriate operation and operating conditions for the
re-used caustic soda regeneration.
3.1. Impact of the evolution of permeation ux and COD
S
reduction on the characteristics of regenerated NaOH
solutions
Regardless of the simulated couples [JRedCODs] (Table 1),
the characteristics of the regenerated NaOH solutions change
with the number of regeneration cycles (Figs. 2 and 3): SS and
COD
S
increase in the course of time, conrming the tendency
already reported by Dresch et al. [21] (Fig. 2a and b); decreases
to reach a limiting value (Fig. 3), suggesting that molecules
originating from the alkaline hydrolysis of milk components
(mainly proteins and fat) have surfactant properties [6,8].
Fig. 2. Impact of the evolution of the permeation ux, J and soluble chemical
oxygen demand reduction, Red
CODs
on the characteristics of regenerated solu-
tions:soluble chemical oxygen demand, CODs (a), suspended solids, SS (b) vs.
the number of cycles for several combinations JRed
CODs
withVRR=80 and
t
f
=166 h. ( ) [J
l
RedCODs
h
]
c
; ( ) [J
h
RedCODs =0]
v
; ( )
[J
l
RedCODs
h
(1)]
v
; ( ) [J
l
RedCODs
h
(2)]
v
; ( ) [J
l
RedCODs
h
(3)]
v
. See operating conditions and explanations in Table 1. Abbreviations: see
list.
Fig. 3. Impact of the evolution of the permeation ux, J and soluble
chemical oxygen demand reduction, Red
CODs
on the characteristics of
regenerated solutions: surface tension, in the course of the number of
cycles for several combinations JRed
CODs
with VRR=80 and t
f
=166 h.
[J
l
RedCODs
h
]
c
; [J
h
RedCODs =0]
v
; [J
l
RedCODs
h
(1)]
v
; [J
l
RedCODs
h
(2)]
v
; [J
l
RedCODs
h
(3)]
v
. See operatingconditions andexplanations inTable 1.
Abbreviations: see list.
The inuence of linear and non-linear evolutions of J and
Red
CODs
with time on the characteristics of the regenerated
NaOH solutions is studied in a continuous ltration mode
with three different combinations of low J and high Red
CODs
([J
l
RedCODs
h
(1)]
v
, [J
l
RedCODs
h
(2)]
v
, [J
l
RedCODs
h
(3)]
v
; Table 1) and considering Red
CODs
>0. The characteris-
tics of the simulated regenerated NaOH solutions are compared
to characteristics of solutions obtained with constant J and
Red
CODs
([J
l
RedCODs
h
]
c
; Table 1), which is considered as
reference [4].
With the linear and non-linear evolutions of J and Red
CODs
in the course of time ([J, Red
CODs
]
v
), uctuations of COD
S
and
SS concentrations are observed (Fig. 2a and b). The uctuations
are generated by the competition between the quantity of matter
coming into the tank due to the plant cleaning and the quantity
of the matter retained by the membrane: at the beginning of the
ltration run, high values of J and Red
CODs
induce a decrease of
the COD
S
concentration in the CIPtank, C. Then, J and Red
CODs
decrease ([9]; Table 1) and the ltrate coming back to the tank
could no more compensate the contamination input due to the
return of CIP solution, leading therefore to an increase in C.
The concentration of SS, totally retained by the membrane
(Red
SS
=1), uctuates around values obtained with constant J
(Fig. 2b).
The concentrations of COD
S
obtained with [J
l
RedCODs
h
]
v
are lower than values observed with constant J and Red
CODs
([J
l
RedCODs
h
]
c
), as suggested by the mathematical integra-
tion of Eq. (9) (Fig. 2a). The sharper the J and Red
CODs
evolution
in the course of time the higher the difference between constant
and non-constant values (Table 1 and Fig. 2a). For example, after
20 cleaning cycles, the average COD
S
values reaches 40.8 g L
1
with [J
h
RedCODs
h
]
c
, 38.9 g L
1
with [J
l
RedCODs
h
(1)]
v
and 35.0 g L
1
with [J
l
RedCODs
h
(2)]
v
(Fig. 2a and Table 1).
Regardless of JRedCODs combination, decreases as soon
as the rst cycle begins andreaches a limitingvalue of 30 mJ m
2
imposed in our assumptions (Fig. 3). Red
CODs
is inefcient, even
in NF, to increase up to a higher plateau value.
G. G esan-Guiziou et al. / Separation and Purication Technology 54 (2007) 329339 335
According to the results presented, a non-linear evolution
of J(t) ([J
l
RedCODs
h
(3)]
v
; Table 1) does not signicantly
modify the evolution of COD concentration compared to linear
and constant laws (Figs. 2a, 2b and 3).
3.2. Selection of the operation of ltration, the volume
reduction ratio and correlated membrane area
For assessing the characteristics of the regenerated CIP
solution, the role of the three parameters (permeation ux, J;
Red
CODs
and membrane area, A
m
) must be quantied. These
parameters characterize crossow ltration operation (MF, UF,
NF; Table 1) and govern the amount of material retained and/or
transmitted by the membrane.
The effect of the couple [J, Red
CODs
] and of A
m
on the
evolution of re-used NaOH solutions characteristics was quan-
tied with continuous mode and the hypothesis of a linear
evolution of J and Red
CODs
versus time ([J
h
RedCODs =0]
v
;
[J
i
RedCODs
i
]
v
; [J
l
RedCODs
h
(1)]
v
; Table 1).
Two cases were successively studied for each operation: con-
stant VRR and identical A
m
.
3.2.1. Constant VRR
With constant VRR, the treated volume and ltration time
(t
f
=166 h) are the same regardless the ltration operation; the
nal VRRis xed at 80 and the required membrane area depends
on the ltration operation type (Table 1).
In that case, the average limiting SS concentration
(3.3 g L
1
) is slightly affected by the numerical values of J
(Fig. 2b): for a high J value ([J
h
RedCODs =0]
v
) the average
SS concentration is around 3.3 g L
1
and for a low J value
([J
l
RedCODs
h
(1)]
v
), 3.4 g L
1
. However, the magnitude of
the oscillations and consequently maximum values for SS are
lower when J is high (Fig. 2b). A high J regeneration operation
(MF, for example) will then limit SSpeak values and give a lower
limit level of SS concentration within the CIP caustic solution.
COD
S
concentration is higher when Red
CODs
is lowand thus,
when the membrane pore size is large, in the particular case
of MF (Red
CODs
=0), COD
S
level increases quasi linearly and
reaches 60 g L
1
after less than 5 weeks (Fig. 2a).
The evolution of is independent of [JRedCODs] combi-
nations and decreases with time (Fig. 3).
3.2.2. Identical A
m
for each ltration operation
With identical A
m
, chosen as the larger NF membrane area
(A
m
=1.061 m
2
), and after the same ltration time (t
f
=166 h),
the higher the J, the higher the treated volume of solution and
the higher VRR. Then nal VRR increases signicantly for MF
and UF. With the same membrane area and the same ltration
time, the average limit of SS level in the ltered solution is
lower when J is high or intermediate ([J
h
RedCODs =0]
v
and
[J
i
RedCODs
i
]
v
with A
m
=1.061 m
2
; Fig. 4a). For DCO
S
, the
average limit value depends on both J and Red
CODs
(Fig. 4b).
When A
m
increases with Red
CODs
>0, the average COD
S
level decreases (Fig. 4b), in accordance with the results previ-
ously reported [4]. For example, when A
m
increases from 0.361
up to 1.061 m
2
, the combination [J
i
RedCODs
i
]
v
gives an aver-
Fig. 4. Selection of the ltration operations (MF, UF, NF), the volume reduction,
VRR and membrane area, A
m
: suspended solids, SS (a) and soluble chemical
oxygen demand, CODs (b) of regenerated NaOH solutions for several combi-
nations of permeation ux, Jreduction of soluble chemical oxygen demand,
Red
CODs
at constant VRR and A
m
. ( ) [J
i
RedCODs
i
]
v
; ( )
[J
l
RedCODs
h
(1)]
v
; ( ) [J
h
RedCODs =0]
v
. See operating conditions
and explanations in Table 1.
age COD
s
level lower to [J
l
RedCODs
h
(1)]
v
: from 58 down to
20 g L
1
(Fig. 4b).
As previously shown (Fig. 3), the evolution of is indepen-
dent of the JRedCODs combination.
3.3. Criteria for the selection of the regeneration operation
(MF, UF, NF, CF) and its processing mode (continuous,
discontinuous)
3.3.1. Sizing of the regeneration plant to maintain
SS 0.3 g L
1
Due tothe detrimental inuence of suspendedsolids onclean-
ing kinetics, the sizing is performed by arbitrarily xing a low
SS limit value, equal to 0.3 g L
1
. A zero value is unrealistic
since a NaOH solution is enriched with suspended solids at the
beginning of cleaning. The actual critical values for SS, COD
S
and ought to be identied for each existing industrial CIP sys-
tem by using experiments aiming at evaluating their effect on
cleaning efciency and kinetics.
For each ltration operation (MF, UF, NF), the sizing for con-
tinuous mode is based on the simplifying assumption of constant
J and Red
CODs
ltration. In effect, as previously shown, the aver-
336 G. G esan-Guiziou et al. / Separation and Purication Technology 54 (2007) 329339
age values for SS, COD
S
and of the regenerated solution have
the same order of magnitude of that for linear evolution of the
combination [JRed
CODs
] versus time.
Continuous mode ltration is compared to discontinuous l-
tration mode and discontinuous centrifugation regarding NaOH
solution functionality (SS, COD
S
, ) and costs.
For maintaining simultaneously SS 0.3 g L
1
and nal
VRR close to 80 (Eqs. (7)(11) do not permit to get constant
VRR value strictly equal at 80) a compromise between t
f
and
A
m
has to be established. Table 2 reports t
f
and A
m
values and
the characteristics of regenerated solutions after operating for 1
year, both for continuous and discontinuous modes of operation.
The ltration cycle duration, t
f
must be decreased from 166 h
down to 12 h for every operation while A
m
remains unchanged
for MF and decreased for UF and NF (Table 2). The reduction
in t
f
results in an increase of cleaning frequency and of NaOH
solution volume disposal.
For MF, unchanged A
m
and decreased t
f
(16612 h) result in
a quasi stabilization of the concentration in COD
S
, the level of
which after 1 year operation is reduced by around 6: 90 g L
1
(t
f
=12 h; Table 2) versus 510 g L
1
(t
f
=166 h); for NF and UF,
COD
S
increases due to decreased membrane area. The maxi-
mum values consequently decrease but values are still close
together: 30 and 31.3 mJ m
2
for UF and NF, respectively.
values remain unchanged for MF: 30 mJ m
2
.
3.3.2. Compared performances of separation operations
and operating modes
3.3.2.1. Filtration: continuous; discontinuous. The perfor-
mances of purication of ltration operations in continuous and
discontinuous modes are similar in close conditions (t
f
=12 h;
A
m
=3.2, 5.1, 14.8 m
2
for MF, UF, NF, respectively; VRR close
to 80). Despite a slight difference in the nal VRR (Table 2),
the calculated COD
S
concentration is not signicantly different
(Eq. (7)). Regardless of the ltration operation, MF, UF or NF,
maximum COD
S
and SS values are of the same order of mag-
nitude in continuous and discontinuous modes, as previously
reported for COD
S
[4]. However, the concentrations of SS or
COD
S
in the course of each cycle are lower for discontinuous
mode (Fig. 5) and as a consequence, higher for surface tension.
The gap, insignicant for UF, remains small but signicant for
NF (Fig. 6).
Fig. 5. Choice of the operating mode: suspended solids, SS of the regenerated
NaOH solutions in the course of regeneration cycle number (after about 1 year
of operation) for several modes and operation of regeneration. Regeneration is
performed at constant permeation ux and reduction in soluble chemical oxygen
demand.
Fig. 6. Choice of the operating mode: surface tension, of regenerated NaOH
solutions in the course of regeneration cycle number (after about 1 year of
operation) for several modes and operation of regeneration. Regeneration is
performed at constant permeation ux and reduction in soluble chemical oxygen
demand.
3.3.2.2. Discontinuous centrifugation. Purication by discon-
tinuous centrifugation is less effective than by ltration, despite
a value as low as the limit that was xed according to our
hypotheses (30 mJ m
2
). The maximum COD
S
level is high
(Red
CODs
=0), as for MF, and the maximum SS is 0.91 g L
1
Table 2
Filtration duration, t
f
and membrane area, A
m
for achieving SS0.3 g L
1
and characteristics of regenerated solutions (suspended solids, SS; soluble chemical
oxygen demand, CODs; surface tension, ) after 1 year of operation in continuous and discontinuous modes
Operation t
c
(h) t
f
(h) A
m
(m
2
) VRR SS (g L
1
) COD
S
(g L
1
) (mJ m
2
)
Continuous
MF 14 12 3.2 82.0 0.27 0.02 90.1 0.5 30.0 0.0
UF 14 12 5.1 81.7 0.27 0.02 4.75 0.05 30.0 0.0
NF 14 12 14.8 80.7 0.28 0.01 3.35 0.05 31.3 0.1
Discontinuous
MF 14 12 3.2 83.0 0.14 0.14 89.2 0.5 30.0 0.0
UF 14 12 5.1 82.7 0.14 0.14 4.2 0.5 30.2 0.2
NF 14 12 14.8 81.7 0.14 0.14 3.3 1.1 32.3 1.2
Operating conditions: volume reduction ratio, VRR close to 80; regeneration ltration performed at constant permeation ux and COD
S
reduction (see Table 1). t
c
,
cycle duration; t
c
=t
f
+t
Cl
(h); t
f
, ltration time (h); t
NCl
, duration of membrane cleaning (h). Abbreviations: see list of abbreviations.
G. G esan-Guiziou et al. / Separation and Purication Technology 54 (2007) 329339 337
with a cycle duration t
c
=14 h, identical to that of ltration
(Table 2). The SS is thus 3.3 times higher than that obtained
by ltration (Fig. 5) owing to a smaller reduction in sus-
pendedsolids withcentrifugation(Red
SS
=0.3). For maintaining
SS0.3 g L
1
, centrifugation with a periodicity equal to t
c
/3
should be performed, what would increase the rejected volume
of sludge by 3 and then the volume of fresh NaOH to be added,
so as to compensate for the volume loss.
As a consequence, integrating ltration operations such as
MF, UF or NF, permits maintaining favourable characteristics of
the cleaning solutions: SS lower or equal to a xed critical level
(0.3 g L
1
) and low (30 < <33.5 mJ m
2
). By performing
discontinuous centrifugation, similar levels of SS and can be
achieved provided there is a shorter regeneration cycle time,
t
c
, what results in a waste volume increase. Decantation, not
simulated in the present work, does not allowachieving a critical
value of 0.3 g L
1
and yields a much higher volume of sludge
[4].
Contrary to NF and UF, MF and centrifugation result in a
higher COD
S
concentration owing to a zero COD
S
reduction.
Should a high COD
S
limit value be unacceptable (viscosity, crit-
ical micelle concentration, . . .) UF or NF operation would be the
selected choice. The membrane area to be used on an industrial
scale shall be calculated from industrial experiments aiming at
establishing the relationship of the NaOH solution functionality
(cleaning efciency and kinetics) and and SS values.
Regarding the targeted CIP cleaning solution composition,
the discontinuous mode of operation should be preferred: even
if the average levels of SS, COD
S
and are similar in both
modes (continuous and discontinuous), the discontinuous mode
yields a residual COD
S
concentration lower or equal to that of
the continuous mode. Moreover, it leads simultaneously to a
slightly higher or equal and slightly lower or equal SS content
in the CIP tank, which are favourable for the functionality of the
cleaning solution [8].
3.3.3. Economical assessment
With a criterion of critical SS concentration of 0.3 g L
1
the
pay-back time of the four operations MF, UF, NF and CF is
short: <3 years and even <2 years for the ltration operations
(Table 3). Pay-back time for centrifugation is 2.8 years, longer
than those for MF, UF, NF, and the sludge volume to be rejected
is three times that of ltration. Pay-back time increases from
MF to NF: 1.1 and 1.9 years, respectively (Table 3). Thus, MF
appears to be the most investment and operating cost-effective,
having the smaller membrane area and energy consumption.
The pay-back times calculated according to our hypotheses are
shorter than those reported by Dresch [4]: NF pay-back time
in the range 1116 years. These very signicant difference
is related to the different choices made on the constraints
imposed over the running CIP solution (different critical
SS concentration which induces a quite different membrane
area) and, at a lower degree, numerical values for calculation
(pollution input, water cost, etc.).
The capital cost of a discontinuous regeneration operation is
higher than a continuous one since it requires two extra tanks
(kD 60); their respective operating costs, not presented in this T
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338 G. G esan-Guiziou et al. / Separation and Purication Technology 54 (2007) 329339
paper, are quite similar even if energy for maintaining the tem-
perature of the two tanks in discontinuous mode has to be added.
Despite of this short pay-back time, the cost of weekly dis-
posal of the re-used cleaning solutions still remains lower than
the savings realized by integrating a ltration operation. The
functionality of that highly contaminated solution is probably
very different owing to its high SS concentration: 3.4 g L
1
according to the input
SS
value.
Moreover, the economical evaluation does not take into
account the decrease in the duration of the alkaline cleaning
phase, which could be achieved due to a faster cleaning kinetics
related to the lower surface tension of the CIP solutions [6,8].
Such an outcome shown for UF membrane cleaning should be
quantied on an industrial scale for CIP cleaning of stainless
steel plants treating or transforming milk, whey or dairy uids.
The MF operation is the recommended operation, the less
expensive one, which retains fewsurfactants compounds, ensur-
ing a lowsurface tension caustic solution. If the high COD
S
level
alter cleaning efciency and kinetics, then UF would be more
appropriate for regenerating the solution but at a higher cost.
4. Conclusions
Numerical simulation of cleaning-in-place systemcoupled to
a regeneration operation (crossow ltration or centrifugation)
shows that it is possible to control the cleaning solution from
a qualitative and quantitative point of view. Suspended solids,
SS, surface tension, and soluble chemical oxygen demand,
COD
s
, are maintained at xed levels. Their evolution versus time
depends on the CIP system parameters (CIP volume, input of
COD
S
and SSinto the systemtank) and on the regeneration oper-
ation performances: combination of ltration uxreduction of
COD
s
(JRed
CODs
) of each ltration operation (MF, UF, NF),
membrane area, A
m
, and cycle duration, t
f
for ltration; Red
CODs
and t
c
for centrifugation.
Numerical simulation of such CIP processes is a powerful
tool which permits selecting and sizing the more appropriate
regenerationseparation, MF, UF, NFor centrifugation, regarding
the targeted CIP cleaning solution composition: SS, COD
S
,
and process costs.
The ltration processes are more performing and less expen-
sive compared to centrifugation. The equations which govern
the operation of a continuous ltration operation, established
from hypotheses coming from a real ltration system operation
(ltration ux, J and COD
S
reduction, Red
CODs
not constant
versus time; interrupting the ltration system while membrane
cleaning) highlight an alteration of the process performance as
compared to an ideal system with constant J and Red
CODs
.
The discontinuous mode is to be preferred regarding the caustic
solution composition and functionality, but the continuous mode
is simpler to use at a lower capital cost.
Among the different membrane operations, MF is the most
appropriate operation since it retains less surfactants compounds
(lower CIP caustic surface tension) and is less expensive. How-
ever, MF results in higher COD
S
concentration in the caustic
solution compared to UF and NF. If such a higher level is prob-
lematic for cleaning, then UF is to be selected. Experimental
quantication of the role of NaOHsolution characteristics in the
efciency and kinetics of cleaning of industrial stainless steel or
membrane equipments used for the treatment and the transfor-
mation of milk or dairy uids is compulsory so as to quantify
and control the level of the critical values for SS, COD
S
and .
Acknowledgements
We thank GES (Noyal/Vilaine, 35, France), Even
(Ploudaniel, 29, France) and Coopagri Bretagne (Landerneau,
22, France) for nancial support, and Uzi Merin for helpful
discussion.
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