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DESALINATION

ELSEVIER Desalination 162 (2004) 279-286

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Membrane filtration of Mozzarella whey

Attila Rektor*, Gyula Vatai
Department of Food Engineering, Faculty of Food Science, Szent Istvan University,
H-1118 Menesi Street 44, Budapest, Hungary
Tel. +36 (1) 372-6232; Fax +36 (1) 372-6323; email: rektor@omega.kee.hu

Received 17 July 2003; accepted 15 August 2003

Abstract
Whey is a by-product of cheese production which is used mainly as animal feed or released into the wastewater
treatment process, although it is rich in valuable components. Recent developments in membrane filtration have
provided exciting new opportunities for large-scale protein and lactose fractionation. The aim of this research was to
develop a complex membrane filtration technology for whey processing. The microfiltration and ultrafiltration
processes were carried out with pilot-scale equipment. For these filtration procedures three modules-- hollow-fibre,
ceramic and spiral wound-- were used. The permeates from micro- and ultrafittmtion (MF and UF), and the original
whey sample were filtered on nanofiltration (NF) and reverse osmosis (RO) equipment. After the measurements new
methods for using whey were proposed. With this complex method cheese production can be redesigned to a more
environmentally friendly and efficient process. All membrane filtration methods were used to find the potential
applications of membrane systems for whey recycling and utilization.

Keywords: Whey; Microfiltration; Sterilization; Ultrafiltration; Nanofiltration; Reverse osmosis

1. I n t r o d u c t i o n permeate compared to the microbiological con-

Whey processing represents one of the first
fields of application of membrane processes in
the dairy industry [1,2]. Microfiltration (MF) has
been used to reduce the total number of lactic
acid bacteria [3] and other microorganisms in the
*Corresponding author.
dition of the whey [4,5]. The process also resulted
in defatting of the whey and can be considered as
a gentle sterilization method [6,7].
The dairy industry has been one of the
pioneers in the development of ultrafiltration
(UF) equipment and techniques based on the
experience gained from its application in the
dairy field. UF has two possible applications in

Presented at the PERMEA 2003, Membrane Science and Technology Conference of Visegrad Countries (Czech Republic,
Hungary, Poland and SIovakia), September 7-11, 2003, Tatranskd Matliare, Slovakia.
0011-9164/04/$- See front matter © 2004 Elsevier B.V. All rights reserved
PII: s0011-9164(04)00052-9
280 A. Rektor, G. Vatai / Desalination 162 (2004) 279-286
the cheese industry: to fractionate the proteins
from whey and to make cheese from ultrafiltered
milk [8-10]. Whey protein concentrates, which
are obtained by whey UF, are available in a great
variety concerning the protein content and
functional properties. Another aspect which must
not be neglected is the utilization of the by-
product resulting from the permeate of UF. In
this case new technologies have also been
developed [nanofiltration (NF), reverse osmosis
(RO)] for lactose, which can be used in the
sweets industry or for fermentation procedures
[11-13].
The most prevalent and economical process
for demineralization of evaporated (EV) whey is
electrodialysis (ED) [14]. NF is an alternative for
the concentration and demineralization of whey
by EV+ED [15]. NF can be used for concentra-
tion of the permeate which penetrates the mem-
brane during UF of milk or whey and which
consists mainly of lactose in the same concen-
tration as in the water phase of the original fluid.
UF permeate has a biological oxygen demand of
30,000-45,000 mg O2/L; therefore, it cannot be
directly disposed as waste water into sewage [ 16].
One of the important problems in the dairy
industry is the high COD value (60,000 mg/L) of
the milk whey. RO can be used to concentrate the
milk whey [17,18].
In this research complex membrane filtration
methods (MF, UF, NF and RO) were developed
for whey processing [19,20]. The whey is rich in
valuable components, but unfortunately it is
mainly used as a feedstock, or is just fed into the
canal. This can be avoided by using a complex
method, and cheese production can be redesigned
as a more environmentally friendly and wasteless
process.
2. Materials and methods
The examined material was mozzarella whey
(Table 1) transported to the laboratory of the
Table 1
Ingredients of the mozzarellawhey
Component %
Water content -94
TS content: 5.87
Fat 0.79
Protein 0.72
Lactose 3.90
Salts 0.46
university directly from the dairy (Sapori
d'Italia). The MF and UF processes were carried
out on pilot-scale equipment built by Hidrofilt.
For the filtration procedure three modules - -
hollow-fibre (MF), ceramic multi-tube (MF) and
spiral wound (UF) - - module were used
(Table 2).
The procedure was as follows: 40 L of whey
sample was fed into the tank of the pilot plant.
The circulation pump was started, and the
temperature was adjusted. Then the appropriate
pressure value and the recirculation flow rate
were fixed. During the process, the permeate flux
was measured with a rotameter.
The microbial measurements took place in a
sterile laboratory. MRS and YEPD media were
used, and a dilution rate of 100-109 from the
permeate was made. From the diluted samples
0.1 ml dispelled on the sterile medium. Colony
forming units were counted after 48 h of incuba-
tion at 37°C.
NF was carried out on YPROLAB 2 type
laboratory equipment (Millipore). The original
whey and the permeates of the MF and UF were
concentrated by this equipment. During this
process a spiral-wound module was used. Table 3
shows the characteristics of the module.
The RO concentration of the whey and the
permeates was carried out on DDS Minilab 20
laboratory equipment. One plate-and-frame
HR-30 membrane module was used for the
experiments (Table 4), and the operation
 A. Rektor, G. Vatai / Desalination I62 (2004) 279-286 281

Table 2
Characteristics of the modules

Modules Manufacturer Maximum Pore size or Module

pressure, bar NMW cut-off area, m 2

Hollow fibre Microdyn 2 0.2 gm 0.75

Ceramic multi-tube Microdyn 8 0.1 gm 0.2
Spiral wound Hoechst 8 100 kDa 1.5

Table 3 Table 5
Nanofiltration module characteristics Concentration of the components/ceramic multi-robe

Module R75A Fat, % Protein, % Lactose, %

Manufacturer Millipore
Max. pressure, bar 35 Whey 0.79 0.72 3.90
NMW cut-off, Da 400 MF-permeate 0.01 0.24 3.14
Area, m 2 0.3
Using the Kjeldal method for protein deter-
Table 4 mination, the results were unexpected concerning
Characteristics of the applied RO membranes the protein content. The membrane retentioned
- 6 7 % of proteins. The microfilter had to let
Type of membrane HR-30 through all the protein because, according to the
Manufacturer Dow scientific literature, the largest casein micelles are
Material Polyamide smaller than the pore size. These results can be
Salt retention, % 99.5 explained as whey contains more small size whey
proteins than larger molecule size casein micelles.
During protein analysis, we examined the
parameters were 30°C and 40 bar, and the quantity of the substances that contain nitrogen,
recirculation flow rate 400 1/h. and between these substances about 30% NPN
can be found. The retention can also be explained
by the gel layer that developed on the membrane
surface.
3. Results and discussion The change can be seen in the case of lactose
3.1. Microfiltration as well, but the retention was not as much as in
the case of proteins. During filtration, the loss of
Table 5 shows the difference of composition lactose was only 19.5%.
between the original whey and the MF-permeate.
The retention of fat content was 98.7%, so the
3.2. Microbiological experiments
filtration was successful concerning the separa-
tion of fat. The reason for this large-scale Microbiological experiments were carried out
retention was the small pore size (0.2 gm) & t h e to determine if the MF procedure is efficient
membrane because, according to the scientific (based on a literature survey) for sterilization.
literature, the sizes o f the fat-balls are between Two different media were used: MRS-agar and
0.1 and 20 gin [20]. YEPD.
282 A. Rektor, G. Vatai / DesalinatT"on 162 (2004) 279-286
Fig. 1. Microbiological results.
3. 2.1. Results for MRS agar
The medium was used to determine the cell
number of Lactobacillaceae. The initial cell
number was determined by 104 and 105 dilution
rates. The dilution rate o f 10 4 gave a more exact
value; therefore, the colony forming unit was
counted at this rate. The result was 1.39x
107 efu/cm3.
Three samples were collected from the
permeate: one sample at the beginning o f the
filtration procedure; the second in the middle and
the third one at the very end o f MF. The results
showed that there were no Lactobacillaceae in
the permeate. The conclusion was that the
membrane retention for LB was 100%.
3. 2.2. Results for YEPD-agar
Further microbiological experiments were
carried out on the YEPD medium. This medium
is proper for all microorganisms; all types are
able to grow on its surface. The procedure was
the same: three samples were collected, but no
colony units appeared. As a result, we can state
that the membrane retained all the micro-
organisms.
Based on the microbiological results we can
state that MF is efficient in whey sterilization.
3.2. Ultrafi ltration
The experiments were carried out at constant
operating conditions conceming the temperature,
Table 6
Concentration of the components
Fat, % Protein, % Lactose° %
Whey 0.79 0.72 3.90
UF-permeate 0.00 0.18 2.31
pressure and recirculation flow rate. Table 6
shows the difference o f composition between the
original whey and the MF-permeate.
UF completely retained the fat. The protein
retention o f the membrane was also high - - 75%
- - as in case o f the MF membrane; the
explanation should be similar. The membrane
retained about 40% of the lactose, which was due
to the gel polarization layer.
Summarizing the results o f UF, the separation
of proteins and lactose was not so efficient. I f the
whey is microfiltered in the first step, then
separation and the sterilization can be carried out
in one step.
Before the concentration o f whey, experi-
ments were carried out to determine the influence
o f the operation parameters on the permeate flux
o f water and whey (as can be seen in Fig. 2) as a
function of transmembrane pressure and recycle
flow rate.
With a pressure increase, permeate flux
increased as well. Therefore, it is recommended
to determine the maximum values o f the curves
and carry out the concentration at this pressure
 A. Rektor, G. Vatai /Desalination 162 (2004) 279-286 283
ss: ..................................................................................... q
~°°1
gO
7

~ 60
i180.................................................................................
_~ 7 0

S 0

40
........... ~ ......................... e .....................

30 '°"

lS . . . . . . .

0 ~ o 2 4 6 8 lo 12 ]4 16 I~
0 1 2 3 4 5 6 T i m e [nfm]
Transmembrane pressure [bar]

Fig. 2. Effect of recycle flow rate on permeate flux in Fig. 3. Permeate flux of whey in a function of time on the
whey microfiltration on a ceramic multi-tube module. hollow-fibre module.
7O
x~UF pc*nn.,3(I bar l~S0"C m4tl"C A30;C I
s0 AMF l~in., 30 bar 60
u MF perm., 25 bar
e Whey 30 bar
so 50

~30

20 , ,_.__._._._ 2O

lO

2 3 4 5 6 7 Z 3 4 5 6 7 8
VCII VCR

Fig. 4. Examination of the concentrationof permeatesand Fig. 5. Effect of temperature on concentration of MF

whey samples on R75A membrane permeate on the R75A membrane.

value. As the recirculation flow rate also had a were examined on a RA 75 Millipore NF
great influence on the permeate flux, concen- membrane considering the permeate flux, and the
tration was carried out at the highest flow rate lactose and salt content o f the permeate and
(3000 L/h) and pressure (2 bar). The results o f the retentate.
concentration are shown in Fig. 3. The operating parameters were constant
The permeate flux decreased with time, which during the procedure: the transmembrane pres-
was due to the higher concentration o f the sure was 30 bar, the recirculation flow rate was
retentate. This decline decreased until no change 200 L/h and the operating temperature 40°C.
occurred at 23 L/mZh. At the beginning of the Fig. 4 shows the results where the flux o f
procedure the flux was higher, but by the time a permeates and whey can be seen in a function of
gel layer was formed on the surface of the volume concentration reduction (VCR).
membrane, there was a steady-state flux o f the The measurements at constant operating con-
permeate. ditions show the differences o f the filtration
characteristics in the case o f different samples.
The highest flux was determined in the UF
3. 3. N a n o f i l t r a t i o n
permeate and the lowest in the original whey
The permeates from MF and UF and the sample. The UF permeate contained less protein
original whey sample were filtered on Millipore and lactose and had no fat content. NF showed
NF equipment. The effect o f operating conditions the same gel layer formation on the membrane
284 A. Rektor, G. Vatai / Desalination 162 (2004) 279-286
surface and the flux curves followed the decreas-
ing trend as in the UF procedure.
The concentration of the MF samples was also
carried out at transmembrane pressure of 25 bar.
At the beginning of the concentration, the flux
increased with the pressure, but with time, as the
VCR increased, the flux values decreased and at
a concentration rate of 5-6, the transmembrane
pressure had no more influence on permeate flux.
Therefore, the higher the VCR is, the lower the
effect on the flux. The determination of this VCR
value is important due to energy utilization which
can be decreased and the lifetime of the pumps
increased.
The concentration of MF permeates was
carried out at three different temperatures to
obtain the optimal temperature value for concen-
tration and to examine the role of temperature
during the filtration procedure. The experiment
took place at the same transmembrane pressure of
30 bar and a recirculation flow rate of 200 L/h.
The effect of temperature is shown in Fig. 5. The
higher the temperature, the higher the permeate
flux.
Transmembrane pressure had the same effect.
Both parameters resulted in permeate flux, but in
the case of temperature, as the VCR increased,
the differences in permeate fluxes decreased. As
a result of the experiment, one can state that
higher VCRtemperatures should be decreased to
spare energy.
In summary, we can say that the NF procedure
is to be done at higher temperatures, but this can
be affected by the heat resistance of the samples.
Energy consumption has to be taken into con-
sideration when choosing the maximum recom-
mended temperature of the membrane.
3. 4. Reverse osmosis
The effect of the pre-treatment of the samples
on the permeate flux was examined during the
RO concentration process. Fig. 6 shows the whey
and permeate fluxes as a function of VCR.
1 1,5 2 ~-"
VCR
Fig. 6. Whey and permeate fluxes as a function of VCR
in reverse osmosis concentration process.
There was less change in the permeate flux
during the concentration of the NF (MF) sample.
The flux was nearly the same at the beginning of
the concentration, even at a VCR of 2. During
this procedure, no polarization gel layer was
formed as the sample contained no fat or protein
and lactose content was low as well. The
differences with VCR increase in the permeate
flux can be observed better in the samples from
UF and MF. Surprisingly, at the same VCR the
differences in flux of the whey and MF permeate
were lower than in the case of MF and UF
permeates.
In conclusion, during the RO process, the fat
content had a lower influence on the flux decline
than the protein and lactose content. Conse-
quently, fat globules had a lower influence on
membrane fouling than the smaller components.
4. Conclusions
On the basis of laboratory and pilot plant
membrane filtration experiments with mozzarella
whey, three alternative treatment lines can be
proposed. The alternatives differ in the separation
efficiency of the valuable whey components and
complexity of the proposed treatment technology.
The alternatives are shown in Fig. 7.
In all alternatives, the first step is defatting
and sterilisation of the whey by MF. The
 A. Rektor, G. Vatai / Desalination 162 (2004) 279-286
I. line
i,,~ ~
('i i i i:;g~ ~:' !
' i
Fig. 7. Alternatives of whey recycling.
separated fat can be pasteurised by conventional
techniques and used as raw material for butter
production.
Line 1: NF is used for the concentration o f the
microfiltered whey. The produced concentrate is
a perfect raw material for ice-cream production.
This solution should be suitable for small- and
middle-sized dairies because the modular type of
membrane filtration enables its adaptation for a
certain capacity o f the dairy, and investment costs
are commensurate with the built-in membrane
surface [21].
Line 2: In this line there are two membrane
filtration separation steps after MF: the UF step
with high rejection o f proteins partially combined
with diafiltration, which can be used for the
production of whey protein concentrate. The
permeate o f UF concentrated by NF and com-
bined with crystallization as proposed by
Kiammel [19] results in lactose that is good for
the pharmaceutical industry. This line can be
profitable for middle-sized and large factories
because the two-stage process needs more basic
materials and the costs o f investment and opera-
tion are higher.
Line 3: This complex membrane separation
method would be the best solution for small
factories. Using RO, all components of the
defatted and sterilized whey can be concentrated.
285
Who ~
2. line 3. line
~',~
~ e~ 'L
~:~-"J
This concentrate can be recycled in the line o f
cheese making so the economical efficiency
should be improved. The end filtrate has small
COD and BOI values so it can be discharged
directly to sewers or used for irrigation.
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