BEER CLARIFICATION BY CROSS-FLOW

MICROFILTRATION:
Fouling Mechanisms and Flux Enhancement
Q. GAN, R. W. FIELD (MEMBER), M. R. BIRD (GRADUATE), R. ENGLAND (MEMBER), J. A. HOWELL (FELLOW),
M. T. MCKECHNIE* and C. L. OSHAUGHNESSY*
School of Chemical Engineering, University of Bath, Bath, UK
*BRF International, Nuteld, Redhill, UK
A
n experimental study of beer microltration has been carried out on ceramic
membranes with the eventual aim of carrying this process through to the commercial
scale. Enhancement of surface hydrodynamics through ow pulsation had little impact
on ux suggesting that pore blocking by in-depth adsorption/deposition was the dominant
factor and this was indeed found to be so. The nature of the foulants has been determined by
studying the ltration rates of beer treated with various enzymes which degrade potential
foulant species. Specic classes of carbohydrates and minerals have been identied as foulants.
In particular, pentosans (carbohydrates composed of 5 numbered sugar rings) make a major
contribution. A multi-stage backush programme was developed and optimized in an attempt
to achieve maximum pore clearance with minimal use of permeate and time. Moreover, when
backush (BF) was employed, staged increases in trans-membrane pressure had a more
positive impact on ux improvement. The effect of membrane pore size on product quality and
ux was also investigated in this work. Use of the BF programme achieved a ux improvement
of 400%.
Keywords: membrane fouling; cross-ow microltration; pulsatile ow; backush; beer
clarication
INTRODUCTION AND SCOPE
The processing of beers with microltration membranes for
microbiological stabilization, clarication and tank bottoms
recovery is potentially viable
13
. Studies have been under-
taken with microltration membranes but limitations in
terms of product (permeate) quality or low permeate
productivity have often been encountered
4
,
5
. Recent work
6
using a claried (kieselguhr ltered) lager beer and a
reconstituted rough beer (made from a claried beer and
yeast) is not directly comparable to our study because such
uids do not contain the chill haze that needs to be removed.
Nevertheless it will be seen later that an interesting contrast
can be made between this recent work and the ndings
reported in the current paper.
Through increased process understanding and incorpora-
tion of the latest improvements in hydrodynamics, it was
thought that a new method for the processing of a natural
traditional material could be developed. If successful, such a
development would enable breweries to replace their
kieselguhr lters with a process not requiring the disposal
of spent lter aid to landll. A LINK project involvingBRF
International, Courage Brewing plc and the University of
Bath started with an experimental study of the complex
fouling mechanisms in ceramic membranes during beer
microltration with the eventual aim of carrying this process
through to the commercial scale. This paper presents the
initial results from this interdisciplinary study.
Membrane fouling in beer ltration has in most cases
been severe and complex
1
,
3
. This has caused difculties in
obtaining an economical ux rate as well as good product
quality. This paper specically highlights the fouling
mechanisms and optimization of rough beer clarication
using ceramic membranes. These membranes have the
advantage being robust. This is important, as harsh cleaning
regimes are used in brewing operations. Furthermore, unlike
polymeric membranes, the membrane structure is not
compressible which allows good comparison of data
between successive experiments. The multi-channel cera-
mic membranes, formed using the technology gained from
the development of the catalytic converter, are relatively
inexpensive, especially when a minimum 5 year life can be
assumed compared with a 2 year life for a polymeric
membrane. The life spans given are generally accepted
values but the latter value can vary signicantly with
different applications, sometimes being as short as 6
months.
Flow pulsation has been successfully employed in
reducing surface particle accumulation in microltration
of yeast suspensions
7
,
8
. In this work, however, turbulence
enhancement through ow pulsation had little effect on ux
improvement, at best doubling a very low long-term ux.
This level of ux was less than half that required for the
commercial implementation of the process. High transmis-
sion of beer components is required to preserve product
quality but extensive adsorption/deposition of proteins,
3
02638762/97/$10.00+0.00
q Institution of Chemical Engineers
carbohydrates, and minerals will always occur inside the
membrane pores. Fouling of this nature would be insensitive
to the change of hydrodynamics on the membrane surface.
Yeast cells, cell debris and the larger proteinaceous
components will contribute to surface fouling but the ux
studies indicated that the predominant fouling factor was
in-pore fouling. Therefore the inuence of hydrodynamics
concentrated on a study of the efcacy of backush (BF) in
tackling fouling caused by in-depth pore plugging. The
nature of the foulants was also determined.
EXPERIMENTAL METHOD AND MATERIALS
Rig Set-up
A schematic ow diagram is presented in Figure A. In
addition to provision for conventional cross-ow, special
features of the experimental rig include (i) techniques for
enhancing surface hydrodynamics and producing secondary
ow through two way reversing ow with and without
inserts; and (ii) an automated multi-stage backush facility
which generates backpulses of controllable frequency and
strength.
Methods and Materials
Tubular ceramic membranes basically composed of
alumina from Ceramem (Waltham, USA) with 0.2, 0.5
and 1.3 lm nominal pore diameters were used in cross-ow
ltration. The membranes consisted of twelve channels of
square cross-section with dimensions of 4

300 mm.
Two way reversing pulsatile ow was introduced by
operating an air driven double diaphragm pump (Wilden
M1, Cheshire, UK). Rough beer types A, and C were
commercially supplied. Unless specied otherwise the beer
used was beer A. The beer has a typical suspended solids
concentration of 0.17-0.21g l
-
1
. All ltration was carried
out at a temperature of
<
38C to ensure that the beer was
representative of that being transferred from `cold con-
ditioning to the lter line. The brewery term `cold
conditioning refers to the conditioning of beer by
refrigerated storage for typically 8 days. This is currently
considered necessary in order to ensure successful ltration.
Beer quality was assessed according to recommended
analytical methods
9
,
10
.
Small scale laboratory studies for foulant species
identication were undertaken using an Amicon stirred
cell with 47mm diameter Anotec 0.2 lm pore size
membranes. The enzyme treatment of the beer was carried
out with either pure enzymes (Megazyme and Aldrich) or
commercial grades (ABM, Biocatalyst or Novo Nordisk).
50 ll of the enzyme preparation was added to 50ml of beer,
69 kPa (10 psi) of CO
2
pressure applied, the stirrer set at
250 rpm and the volume of ltrate collected in a set time
noted. Percentage increases or decreases in ltrate collected
consequent to enzyme addition (as compared to runs
without enzyme) were calculated.
To detect the concentration of the minerals in the foulant
layer the deposited minerals were washed out with 0.1 N
HCl. Atomic Absorption Spectroscopy was then used
Backush Programme
The principal aim in designing a good backush regime is
to minimize permeate usage as backush media whilst
achieving the maximum pore clearance within the shortest
possible time. In this work, backush was governed by a
programmed multi-stage backpulse routine with time
varying frequency and pulse strength. The variables are
many and include the CO
2
pressure, the duration of the
pulse, duration between end of the pulse and opening of the
permeate valve and cycle frequency. These variables
inuence the membrane cleaning efciency of the back
pulse, dead-time and the `loss of permeate. The `lost
permeate is permeate recycled from the product to the feed-
side and so this portion does not contribute to the net ux.
RESULTS AND DISCUSSION
Identication of Key Membrane Foulants
Initial studies focused on treating the beer with
commercial enzymes and measuring the ltration rates of
the resultant solutions in a stirred cell apparatus. As the
enzymes are known to digest various particulate and
macromolecular species, the nature of foulants could be
determined by studying these rates. The Anotec membrane
was chosen as it is one of the few at sheet alumina
membranes available. Table 1 shows the effect of the
commercial enzymes.
Care must be taken when interpreting data from
commercial enzymes, as many of them are impure and
may contain more than one active component. Synergistic
4 GAN et al.
Trans IChemE, Vol 75, Part A, January 1997
Figure A. Schematic ow diagram (PT - pressure transmitter, TT -
temperature transmitter).
Table 1. Stirred cell studies (commercial enzymes). Percentage increase or
decrease in ux.
Type of Enzymes Source Beer A Beer C
Bact. a -amylase Bacillus amyloliquefaciens
+
0.25
+
32.80
Bact. b-glucanase Bacillus subtilis
-
3.06
+
25.27
Bact. a -amylase Bacillus stearothermophilus
-
20.08
-
7.0
Fung. a -amylase
-
5.8
-
3.53
Pullulanase Klebsiella planticola
-
10.77
-
8.1
Bact. proteinase
-
12.55
-
7.97
Fung. a -amylase Aspergillus oryzae
+
21.33
+
1.76
Fung. b-glucanase Penicillium funiculosum
+
23.7
+
63.62
Trypsin
+
7.2
+
8.1
Papain
+
3.7
+
7.8
Fung. cellulase Penicillium funiculosum
+
12.3
+
31.75
and antagonistic effects between enzymes are not uncom-
mon. The proteases trypsin and papain are the exception to
this rule, being specic to proteins. The precise activities of
the enzymes vary from type to type and also between
batches, making direct quantitativefoulant analyses difcult
without time consuming assays. All enzymes were added as
a standard volume of preparation (25 units of activity per
50 ml of beer). These data can only be used to identify the
nature of the foulants. Some of the enzyme data in Table 1
indicate a reduction in ux on adding certain enzyme
preparations. In these cases there is no or little benecial
enzyme activity and the enzyme preparation itself fouls the
membrane. However, the increases in ux of over 20% due
to the activity of certain other enzymes clearly indicates that
carbohydrate species such as b-glucans and starch mole-
cules/particulates affect performance. Interestingly, pro-
teases had only a small effect indicatingthat proteins are not
the major foulant. This result was slightly surprising as it is
known that microltration of beer can reduce its foam
stability (Head Retention Value, HRV). This reduction in
HRV is attributed to protein loss and therefore it follows that
proteins are retained by small pore membranes. This factor
inuences the choice of membrane pore size. As our results
show, it does not follow that fouling is mainly a matter of
protein adsorption.
Following the stirred cell studies, commercial grade
enzymes were used with both the stirred and cross-ow
lters. Two commercial grade enzymes (Table 2) were
evaluated in the laboratory stirred cell with two beer types
and then the experiments repeated by treating 50 litres of the
beers with enzymes from the same batches and carrying out
a cross-ow experiment with the 0.5 lm Ceramem module.
It was found that the small-scale studies had been successful
in indicating enzymes for use on the larger scale. Some data
is shown in Figure 1. Subsequent work, still ongoing, with
pure enzymes has quantied the trends reported here and
also identied pentosans (carbohydrates composed of 5
numbered sugar rings) as a specic foulant. The Atomic
Absorption Spectroscopy results, giving the mineral deposi-
tion on the membrane surface, are shown in Table 3.
Single layer ion adsorption will only cause a very limited
degree of fouling because of its very small physical size,
even allowing for hydration. However, membrane fouling
could be aggravated by the problem that divalent ions are
liable to act as sequestering agents to form large molecular
complexes of carbohydrates and proteins when such
materials are concentrated on the membrane surface.
Formation of such macromolecular aggregates may cause
dramatic reduction of the effective hydraulic pore radius. As
indicated, the ions detected were calcium and copper.
Flux Under Steady Cross-ow
The effect of pressure upon ux is shown in Figure 2.
Below a transmembrane pressure (TMP) of 0.8 bar the ux
rates attained a similar steady-state level after an initial and
rapid decline in ux. When TMP was over 0.8 bar, the
steady ux level was lower. For the conditions employed
this indicated a TMP limit of 0.8 bar for conventional cross-
ow microltration.
Flux Under Pulsatile Flow
The increase of ow turbulence through ow pulsation
can be described in terms of a peak oscillatory Reynolds
number Re
p
and a ratio of the size of the amplitude to the
size of the channel. In this study the size of the channel was
not varied. The denition of Re
p
is:
Re
p =
qm
p
D/l
where m
p =
peak velocity of oscillatory flow
=
2pfx
x
=
amplitude (m) q
=
density
f
=
frequency (s
-
1
) l
=
viscosity
Two way reversing pulsatile ow was generated by
operating the air driven diaphragm pump so as to oscillate
the cross-ow. The steady ow was oscillated (with the net
volumetric owrate the same as in Figure 2) to give peak
Reynolds number from 1550 to 4950. Such an increase in
ow turbulence, however, failed to produce a signicant
ux improvement. The results in Figure 3 show a denite
improvement in the ux compared with Figure 2 but the
absolute values are less than half that required for the
commercial implementation of the process on a green eld
site. (For implementation on existing sites that already use
kieselguhr lters, a higher ux is required.) Different
frequency and amplitude parameters controlling the dia-
phragm pump were used and similar results were obtained.
5 BEER CLARIFICATION BY CROSS-FLOW MICROFILTRATION
Trans IChemE, Vol 75, Part A, January 1997
Table 2. Stirred cell studies (commercial enzymes). Treated beers to be
used in cross-ow lter experiments.
% increase in ux
Enzyme Source beer A beer C
Cellulase Penicillum funiculosum
-
120
Amyloglucosidase Aspergillus niger 34
-
Figure 1. Effect of amyloglucosidase addition on cross-ow ux rates,
TMP
=
1
.
3bar, Re
=
6700.
Table 3. Mineral deposition on ceramem membrane surface.
Membrane Surface Concentration
Type of Ions (mg m
-
2
)
Ca
+ +
0.87
Cu
+ +
0.49
Fe
+ +
0
Mg
+ +
0
This result suggests that either increases in bulk ow
turbulence did not produce a sufcient enhancement of
surface shear stress (which is critical in removing surface
deposit) or that the in-pore plugging mechanism (which
is insensitive to the change of surface hydrodynamics)
is dominant. The work with membranes of different pore
sizes (see next section) suggested that the latter was the
case.
Effect of Membrane Pore Size
Figure 4 shows the effects of altering pore size on ltrate
ux. Clearly the smaller pore size gives a higher ux. This
conrms that one of the major mechanisms is in-depth pore
pluggingas smaller pores will exclude much of the ne
material from the membrane matrix.
One important factor is the impact of pore size on
resultant beer quality. Figure 5 shows the head retention
values (HRV) of the ltered beer as a function of time for a
0.2 and a 0.5 lm membrane. The HRV value is a quality
control measure indicating `foam stability and is related to
the presence of head forming protein. Clearly the 0.5 lm
pore membrane will consistently transmit such components
but the 0.2 lm pore size membrane tends to remove them.
Indeed, the rate of removal increases as the membrane
becomes fouled. The implication is that with the 0.2 lm
pore size membrane, some of the ner particles and
macromolecules are being incorporated in to the fouling
layer, and that this layer is ultra-ltering or adsorbing
proteinaceous material. A similar trend was noted with
gravity (density) measurements; for the 0.2 lm membrane
there was a general loss of carbohydrate molecules. It is thus
obvious that product quality issues dictate the use of the
0.5 lm pore size membrane.
It is also noted that the performance of the rough beer
used in this study behaved very differently to the beers used
by Blanpain and Lalande
6
. Their beers were a claried
(kieselguhr ltered) lager beer and a reconstituted rough
beer (made from a claried beer and yeast), whilst in our
study unclaried beers were obtained direct from the
brewery. For both of their beers, results indicated in-pore
fouling followed by the build-up of a cake layer with the
overall membrane resistance being very dependent upon
the latter. In contrast, our results with previously unltered
beer strongly suggest that in-pore fouling is dominant.
Clearly the inuence of the insoluble, non-yeast compo-
nents, present in our feeds (but absent from theirs)
dominates the fouling behaviour of rough beer.
This suggests that the number of days in cold conditioning,
and the efciency of this process, will inuence ltration
performance.
Flux Improvement Through Backush
Filtration with a backush(BF) programme using the
combination of CO
2
and permeate as backush media was
adopted. When only liquid permeate was used, the amount
6 GAN et al.
Trans IChemE, Vol 75, Part A, January 1997
Figure 2. Flux under conventional cross-ow ltration, Re
=
1552.
Figure 3. Flux prole under two way reversing ow pulsation, Re
=
1552,
Re
p =
3400.
Figure 4. Effect of pore size on ux, TMP
=
1
.
3 bar, Re
=
6700.
Figure 5. Effect of pore size on head retention value.
of beer recycled from one side of the membrane to the other
was excessive and the net ux was low. Figure 6 shows a
representative part of the ux prole from a typical run. The
backpressure is the pressure in the CO
2
line at the initiation
of the BF routine.
In Figure 6 the following information is given:
A
1
,A
2
..A
n
: Instant Peak Flux (IPF) immediately after a
backush routine.
B
1
,B
2
..B
n
: Base Flux Level (BFL) towards the end of a
cycle.
C
1
,C
2
..C
n
: Average Flux with backush.
(t
C 1
-t
A 1
),.. (t
C n
-t
A n
) : Duration when ux is above the
moving average.
The following are important characteristics and implica-
tions drawn from the ux proles:
1. BFL is over 100% higher with backush than without. It
is fully expected that the BFL can be further enhanced by
optimizing the backush programme.
2. The instant peak ux (IPF) obtained after committing a
backush routine is short-lived. The longer the ltration
process, the faster the IPF declines after initiating a
backush routine.
3. IPF and BFL are variables whose values decline with
time. This suggests that the backush operation is not
capable of resolving continuous irreversible membrane
fouling caused by particle adsorption/deposition.
The duration of the period when the ux is above the
moving average ranged from 60s at the beginning of the run
down to 10-20s after 5 hours of ltration. The implication is
that a backush programme should be designed to take
account of this. Excessive backush will result in high cost
through the loss of permeate and effective ltration time.
Another consideration is that when BFL is high, a stronger
backush may be used to obtain the best backush effect but
when BFL is low, backush strength should be reduced in
order to reduce the backush cost.
A multi-stage backush programme (Table 4) was
designed to deliver a suitable backush frequency and
strength with regard to the base ux level at different
ltration stages. Application of the programme improved
the ten hour average ux by 400%, to 22kg m
-
2
h
-
1
,
compared to the initial baseline case of standard cross-ow
ltration.
Effect of TMP and Cross-ow Rate
As noted above, a limiting TMP of 0.8 bar was observed
for steady cross-ow ltration without backush (Figure 2).
When the multi-stage backush programme was used, ux
improved signicantly with the increases in TMP (Figure 7).
The suggestion is that a TMP slightly in excess of 1 bar
may be optimal but an exact optimum has yet to be
determined.
This study also revealed that cross-ow velocities at or
below 0.75 ms
-
1
had little inuence on ux performance.
CONCLUSIONS
Membrane fouling in beer microltration is severe and
complicated. For rough beer, in-depth pore fouling by
particle adsorption/deposition was found to be the pre-
dominant fouling factor. The decline in ux was insensitive
to changes in surface hydrodynamics. Carbohydrate species
such as b-glucans and starch molecules/particulates were
identied as key membrane foulants. In particular, pento-
sans make a major contribution. Deposition of Ca
+ +
and
Cu
+ +
on the membrane surface may also promote further
adsorption/deposition of protein and carbohydrate mole-
cules. Overall, for the membrane used, product qualityissues
dictate the use of the 0.5 lm pore size membrane.
With pulsatile ow, increases of peak oscillatory ow
Reynolds number from 1550 to 4950 failed to produce a
commercially signicant ux improvement. However,
backush was more effective. To achieve optimum back-
ush effect the frequency and strength ought to vary with
time to suit the continuous baseline ux decline. A multi-
stage backush programme was developed and optimized to
achieve a ux improvement of 400%. The absolute level of
ux still needs to be improved if cross-owmicroltration is
to be an economic replacement for existing kieselguhr
lters.
7 BEER CLARIFICATION BY CROSS-FLOW MICROFILTRATION
Trans IChemE, Vol 75, Part A, January 1997
Figure 6. Effect of backlash (BF), TMP
=
1
.
3, Re
=
1552 BF
frequency
=
0
.
2/minute, BF length
=
0
.
5 s, Backpressure
=
2
.
0 bar.
Table 4. An optimized multi stage backush programme.
Stage Frequency Length TMP Back Pressure
(hr) (l/minute) (s) (bar) (bar)
1 1 0.5 0.8 2.5
2 2 0.3 1.3 2.5
3 4 0.2 1.7 4.0
4 8 0.1 2.0 5.0
Figure 7. Effect of TMP on ux, Re
=
1552
.
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ACKNOWLEDGEMENTS
The helpful advice and encouragement of Tim ORouke (Courage
Brewing plc) is grateful acknowledged together with the nancial support
of the EPSRC and the DTI. The Director-General of BRF International is
thanked for granting permission to publish this paper.
ADDRESS
Correspondence concerning this paper should be addressed to Dr R. W.
Field, School of Chemical Engineering, University of Bath, Claverton
Down, Bath BA2 7AY, UK.
The manuscript was received 2 July 1996 and accepted for publication
after revision 15 November 1996.
8 GAN et al.
Trans IChemE, Vol 75, Part A, January 1997