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Solid/Liquid Separations

Selecting

Membrane Filtration
Systems
Wu Chen
Frank Parma
Anant Patkar
Adrienne Elkin and
Subrata Sen,
The Dow Chemical Co.

Proper design and scaleup of a membrane


filtration system requires an understanding
of the availability of membrane material,
pore size and module configurations.
These practical guidelines will help in the
selection process.

HE GROWING NEED FOR FINE FILTRATION


in food and beverage manufacturing, bioprocessing and water treatment has placed membrane filtration at the forefront of separation technologies applied in the chemical process and related
industries. However, membranes increasing prevalence in separation applications has not diminished
the challenges users face when trying to design the
optimal membrane system.
Fundamentally, one must be familiar with the
availability of membrane materials, membrane pore
sizes and membrane module configurations (e.g., spiral-wound vs. flat sheet). One must also consider several crucial operating parameters during the membrane evaluation and design phase, including module
geometry, flow patterns, flowrates (e.g., of the crossflow stream), shear rate, transmembrane pressure and
cleaning strategies. In addition, pilot tests should be
conducted using membrane configurations that are
similar to those of the full-scale system, in order to
minimize problems during scaleup. Any attempts to
design a membrane filtration system based on literature data or small-scale laboratory tests alone will
likely result in failure.

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Membrane classifications
Traditional filtration media such as filter cloth, wire
mesh or sintered metal have been used to remove particles measuring down to 1 mm. But, due to the lack of
technology in manufacturing these media, they have
not been successful in filtering out finer particles. Advances in polymer technology have brought to market
many membranes with pore sizes down to a few
angstroms (1010 m), opening the doors to what is now
called membrane filtration.
Depending on the sizes of particles to be separated,
membrane filtration can be classified as microfiltration
(MF), ultrafiltration (UF) or reverse osmosis (RO). There
are no clear-cut boundaries among these categories. Normally, MF refers to filtration of particles measuring approximately 0.051 m. UF membranes reject particles
measuring down to 30 nm (109 m). RO membranes are
used to remove even smaller particles, such as sodium
ions, from the feed stream. Nanofiltration (NF), a relatively new term, has been employed for applications that
fall within the boundaries of UF and RO.
MF membranes are rated by pore size, which is
measured in microns. These ratings, however, are not
always absolute. Membranes that have the same rating

Table 1. Comparison of membrane filtration processes.


Membrane
Process
Microfiltration
Ultrafiltration
Nanofiltration
Reverse Osmosis

Typical
Pore Size
0.051 m
11,000 kD
0.011 kD
9899%
salt retention

Typical P, psi
550
7100
50150
1201,200

may not exhibit identical rejection behaviors, due to differences in membrane material, membrane microstructure,
particle characteristics and membrane testing methods.
UF and NF membranes are rated using a term called
molecular weight cut-off (MWCO). The unit of measure
for MWCO is the Dalton (D). If a membrane does not
allow molecules with molecular weight of 100 g/mole or
more to pass, then this membrane is considered to have a
MWCO of 100 D. The MWCO is frequently expressed in
kD, where 1 kD = 1,000 Dalton. UF membranes are available in the range of 11,000 kD MWCOs. As in the case
of MF, and for similar reasons, UF and NF membranes
with identical ratings may not behave the same way. Manufacturers of UF and NF membranes use polymers with a
defined molecular weight distribution, such as polyethylene glycol or dextrin, to evaluate membrane-rejection
characteristics. It is important to remember that the hydrodynamic radii of these extended polymers may be different
from those of the molecules one intends to separate. For
example, proteins are usually globular and compact.
Therefore, for complete rejection of a protein, one should
use a membrane rated at one-fifth the molecular weight of
that protein (e.g., a 10-kD membrane should reject a 50kD protein completely).
For RO membranes, the rating is commonly listed as
percent (%) salt retention. Similar to UF and NF, the percent removal depends on the type of salt and operating
conditions. As the pore size decreases, the required driving
force (P) for filtration increases. A summary of membrane pore sizes and pressure drops for MF, UF, NF and
RO is presented in Table 1.

Membrane materials and modes of filtration


Although many membrane materials are discussed in literature, only a few are commercially available for largescale applications. Today, the most readily available membrane materials for full-scale deployment are polyethersulfone (PES), polysulfone (PS), cellulose acetate (CA), regenerated cellulose (RC), ceramic materials and sintered
metals. Less-commonly available materials are nylon,
polypropylene, polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), polyacrylonitriles (PAN) and composites. Many other materials may have been developed,
but have not yet become commercially available. Due to
difficulties in maintaining a wide array of product lines,

Table 2. Commercially offered membranes.


Supplier
Membranes Offered
Alfa-Laval
PES, PS, RC, composite
Dow Chemical
PES
Millipore
PES, PVDF, RC, composite
GE Osmonics PAN, PES, PS,PTFE, PVDF, nylon, composite
Pall (Filtron)
PES, PVDF, RC, ceramic, nylon
PTI
PES, PAN, PS, PVDF, composite
Sartorius
CA, PES, PP

membrane suppliers typically offer a limited selection of


membrane materials (Table 2).
Membrane filters are designed to filter very fine particles,
which tend to form cakes with high resistance to flow. This
can cause a rapid drop in the filtration rate with traditional
dead-end filtration. The drop in filtration rate is especially
severe for compressible cakes formed by some biological
systems (e.g., bacterial cells from fermentation, broken cells
after cell homogenization, mammalian cells after cell culture). Thus, with membranes, crossflow filtration is normally
used to improve the filtration rate (Figure 1).
During crossflow filtration, the suspension flows at a
high speed in the direction that is parallel to the filter surface. This high flowrate provides greater shear at the membrane surface, thereby preventing the solid particles from
forming a cake, which permits a high filtration rate for a
longer period of time.

Equipment options
In membrane filtration, the permeate (or filtrate) flows
through the membrane (in crossflow filtration, this flow is
perpendicular to the membrane surface), while the slurry
(or retentate) remains on the other side of the membrane.
The filtration rate per unit membrane area is called permeate flux, commonly expressed in L/m2h.
Due to the membranes small pore sizes and high medium resistance, the liquid flux is normally smaller than that
seen in conventional filtration processes. A larger filtration
area is therefore necessary to achieve the required filtration

Figure 1. Shown are the two filtration modes: dead-end (left) and
crossflow (right).

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Solid/Liquid Separations

d
c

Figure 2. Membrane element configurations: a)

spiral wound, courtesy of Dow Chemical Co.; b) hollow fiber, courtesy of PCI Membrane Systems, Inc.;
c) flat sheet, courtesy of Alfa Laval; d) tubular
ceramic, courtesy of Pall Corp.

capacity. One of the key issues in designing membrane filters is maximizing the filtration area, while avoiding the
fabrication of very large equipment.
A membrane filtration system is composed of filter vessels in which a number of membrane modules are housed.
Four popular membrane module configurations are the spiral-type filter (Figure 2a), in which the membrane is spiralwound and housed in a cylindrical casing. The retentate
flows in a direction that is parallel to the axis of the cylinder and the permeate flows spirally into the membrane
modules central collection chamber. Today, spiral-type filters are the most common and economic type of membrane
configuration, since they offer the highest membrane area
per footprint (space consumed in plant). However, these
membranes are usually not suitable for systems with a high
concentration of suspended solids.
Another module configuration that is frequently used in
todays industrial environment is the hollow fiber type (Figure 2b). In this configuration, a bundle of hollow fibers
(with each fiber measuring 0.12 mm in internal diameter)
is contained within a shell. The retentate flows inside the
hollow fiber, while the permeate is collected on the shell
side. Hollow fiber membranes, like the spiral-wound membranes, are considered to be an economic option. However,
they are not recommended when solid particles are present.
Flat-sheet membrane systems, such as those shown in
Figure 2c, comprise flat sheets of membranes that are attached to plastic plates, which provide mechanical support.
Many plates can be stacked together to achieve a system
with a large filtration area.
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In this configuration, the retentate flows


across the membrane surface, while the permeate flows through the membrane to the collection channels located at the edges of the
plates. Virtually any type of flat-sheet membrane can be used. Some manufacturers fashion the flat sheets into cassettes that are easy
to replace and validate. However, in this case,
users would be limited to the membrane materials offered by the cassette suppliers.
Last, but not least, is the tubular arrangement (Figure 2d), which is used for polymeric, ceramic or sintered-metal membrane filters. The advantages of ceramic or sinteredmetal filters are higher fluxes, greater tolerances to a broad range of operating conditions
(pH, temperature, solvents, pressure), ease of
cleaning and longer membrane life. Ceramic
membrane modules tend to be more expensive, but are available in a wide variety of
pore sizes. Furthermore, their long lifecycle
may result in lower long-term replacement
costs. Sintered-metal membranes are less
costly than their ceramic counterparts, but
offer a limited selection of pore sizes.

Membrane filter operation


Crossflow rate and trans-membrane pressure (TMP) are
two key parameters in the design and operation of a crossflow membrane filtration system. Sufficient crossflow rate
is required to prevent concentration gradient buildup near
the membrane wall.
Typical crossflow velocities for the cassette, hollow
fiber, tubular and spiral configurations are, respectively,
~13 m/s, 15 m/s, ~5 m/s and ~38 gal/min (for a 2.5 in.
dia. 40 in. long element). TMP controls the permeate
flux. To this end, the following rule of thumb applies: The
higher the TMP, the higher the flux. It should be noted that
crossflow rate and TMP are closely related. High crossflow
rates normally generate high TMPs, unless the back pressure on the permeate side is properly controlled. Further, at
a given crossflow rate, the TMP cannot be decreased beyond a certain value (which is dictated by the pressure drop
on the retentate side) without resulting in reverse flow
(from the permeate to the retentate side) in part of the module. Reverse flow is particularly undesirable in spiral and
some flat-sheet modules. Parameters, such as pH, temperature and ionic strength of the medium may also be important in some systems.
The objective of membrane filtration has to be clearly
defined before attempting to optimize a filtration process.
Often, the operating parameters (crossflow, TMP, pH, temperature, ionic strength) that result in the best filtration flux
may not permit optimal product passage. These parameters
must be carefully tested at the pilot scale to ensure successful process design.

Fouling is a major challenge in membrane filtration. It


could be caused by blocking of the pores at the membrane
surface or inside the membrane, constriction of the pores
by adsorption of particles, or chemical reactions occurring
on the membrane surface. The following techniques are
commonly employed to mitigate fouling:
providing high shear at the membrane surface
selecting a hydrophobic or hydrophilic membrane
based on the properties of the suspensions
operating the membrane under alternating conditions
(low pressure, different pH, temperature, etc.)
coating the membrane with a fouling-resistant material.
If the process flux declines significantly, the membrane
filter (and the system) should be cleaned. The frequency of
cleaning-in-place (CIP) is based upon the acceptable drop
in membrane performance, the desired membrane life (frequent CIP may reduce membrane life) and regulatory considerations. Commonly used chemicals for CIP include filtered water (at room temperature or hot), base solutions
(usually sodium hydroxide), acids (phosphoric, nitric), detergents (ionic, nonionic) and chlorine (usually for applications under alkaline conditions). Multiple steps using different reagents are often necessary to ensure efficient cleaning. One can obtain cleansing products designed specifically for membranes from Ecolab, Alconox and Fibercorp, but
always consult the membrane manufacturer before writing
cleaning protocols to ensure the chemicals are compatible
with the membrane materials.
Membrane sanitization may also be required when filtering products intended for food or pharmaceutical applications. Sanitation reagents include sodium hydroxide, nitric
acid, peracetic acid and chlorine.

Selection of a filtration system


Once a basic understanding of membrane filters is captured, the process of selecting a membrane filtration system can begin.
1. Determine the separation goal. Since membrane filtration systems are normally more expensive than traditional filters, ascertain whether membrane filtration is actually
necessary. Know the characteristics of the particles and liquid, as well as the process conditions, such as temperature,
pressure and capacity requirement.
2. Select a membrane pore size. One rule of thumb is to
select a membrane with a pore size one order of magnitude
smaller than the diameter of the particles to be separated.
However, this rule may not be true for all applications.
Testing is therefore necessary.
3. Ensure chemical compatibility. The suspension
should not attack the membrane and the membrane material
should not be prone to fouling by the suspension. Small
changes in operating conditions (pH, temperature) may improve chemical/membrane system compatibility.
4. Perform pilot-scale tests. Conduct experiments
using the membrane material, pore size, configuration,

etc., that is intended for use on the production unit. It has


been demonstrated over and over that membrane filter
performance can be quite different even for the same
membrane type (e.g., a PVC membrane) that is conformed
to different module configurations (e.g., flat sheet vs. spiral) or physical dimensions (diameter, length, height).
Testing should establish the optimum operating parameters, process reproducibility, cleaning and sanitation methods, as well as estimated membrane life under repeated
cycles of usage and cleaning.
The membrane filtration unit is normally designed
and built by companies that specialize in membrane systems. Most membrane suppliers do not build complete
systems. It is advisable to work closely with membrane
suppliers and system designers during the evaluation and
design phases, as experience still plays an important role
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in this technology.
WU CHEN is a senior specialist at The Dow Chemical Co. (B-1402, 2301 N.
Brazosport Blvd., Freeport, TX 77541; Phone: (979) 238-9943; Fax: (979)
238-0969; E-mail: wuchen@dow.com). He established a fluid/particle
separation laboratory for Dow in Freeport for practical applications of
fluid/particle separation technologies and has numerous publications
about practical aspects of fluid/particle separation in journals,
conferences and books. Chen received his PhD in chemical engineering
from the Univ. of Houston (TX) and is an active member of the American
Filtration and Separation Society (AFS), serving as society chair, board
member, as well as a speaker in numerous meetings. He is currently the
chair for the AFS Education Committee and a solid/liquid separation
course instructor for the ASME-AIChE continuing education program
(www.asme.org/education/shortco/aiche.htm).
FRANK PARMA is a research specialist at The Dow Chemical Co., where he
specializes in solid/liquid separations. In the past 15 years, he has
provided technical support for many Dow sites, both within the U.S. and
abroad. Parmas recent focus has been on the application of solid/liquid
separation technology for water treatment, especially in the area of water
and wastewater treatment chemicals. Parma received his BS in marine
biology from Texas A&M Univ. (Galveston, TX). He is also an active
member of the AFS.
ANANT PATKAR is a senior specialist in the Bioprocessing R&D Group of The
Dow Chemical Co. (5501 Oberlin Dr., San Diego, CA 92121; Phone: (858)
352-4317; Fax: (858) 352-4602), where he engages in bioprocess
development, optimization and scaleup, with a primary focus on
downstream processing. His industrial experience covers both microbial
fermentation and mammalian cell culture operations. Patkar received his
PhD in chemical engineering from Purdue Univ.
ADRIENNE ELKIN, formerly a research engineer in the Bioprocessing R&D
Group at The Dow Chemical Co., is currently employed by Merck & Co. She
is experienced in downstream product recovery and purification process
development, scaleup and pilot-plant operation. Elkin received a BS in
chemical engineering from Penn State Univ.
SUBRATA SEN is a R&D leader of Bioprocessing R&D Group at The Dow
Chemical Co. (Phone: (858) 352-4433; Fax: (858) 352-4602; E-mail:
ssen@dow.com), where he spearheads the downstream recovery and
purification operations. He received his BS in chemical engineering from
Indian Inst. of Technology (Kharagpur), and MS and PhD degrees in
chemical engineering from Brigham Young Univ., specializing in flow
physics and transport processes.

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