Available online at http://ijcpe.uobaghdad.edu.iq and www.iasj.net
Iraqi Journal of Chemical and Petroleum
Engineering
Vol.23 No.2 (June 2022) 47 – 53
EISSN: 2618-0707, PISSN: 1997-4884
Corresponding Authors: Name: Zaid Waadulla Rashad , Email: zaid@coeng.uobaghdad.edu.iq
IJCPE is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License.
Studying and Analyzing Operating Conditions of Hollow Fiber
Membrane Preparation Process: A Review Paper
Zaid Waadulla Rashad
University of Baghdad/College of Engineering/Chemical Eng. Dept.
Abstract
Polymeric hollow fiber membrane is produced by a physical process called wet or dry/wet phase inversion; a technique includes
many steps and depends on different factors (starting from selecting materials, end with post-treatment of hollow fiber membrane
locally manufactured). This review highlights the most significant factors that affect and control the characterization and structure of
ultrafiltration hollow fiber membranes used in different applications.
Three different types of polymers (polysulfone PSF, polyethersulfone PES or polyvinyl chloride PVC) were considered to study
morphology change and structure of hollow fiber membranes in this review. These hollow fiber membranes were manufactured with
different process conditions and a reasonable starting point for factors remained constant to study the changing effect of specific
factors.
Keywords: Hollow fiber membranes, phase inversion, ultrafiltration, polymers
Received on 26/05/2022, Accepted on 19/06/2022, published on 30/06/2022
https://doi.org/10.31699/IJCPE.2022.2.7
1- Introduction
Membrane separation is the most flexible reliable and
promising technology over the past decades. Membrane
technology offers high performance among other
processes Adsorption, Extraction, Distillation, and
leaching in terms of environment friendly and cost effect
[1], [2].
A membrane is described as a barrier separating two
phases [3] made of high chemical stability materials.
Membranes are often linked to their application to choose
the right process and membrane module [4].
From the food industry to desalination (providing
drinking water for millions around the world), dialysis
(saving the life of kidney disease patients), automotive
industry (electroplating bath recovery), and gas
separation, membrane processes can be applied to a wide
range of applications [4].
Fig. 1 describes membranes classification according to
their morphology into dense, porous, and composite.
Asymmetric porous membranes invented by Loeb and
Sourirjan, [5] are the most commercially available
membranes in the present day. The structure of
asymmetric membranes is a defect-free skin layer based
on a porous layer [4]. This structure can be achieved by
simple principles but is quite tricky with a process called
phase inversion.
The process starts with polymer solution
thermodynamically unstable by one of FOUR methods;
immersion precipitation, vapor induced phase separation,
thermally induced phase separation, and dry casting,
which leads to polymer separation to polymer lean create
pores and voids and polymer-rich phases the porous
structure of membrane [4-6].
Fig. 1. Membrane classification according to structure
morphology [4]
Hollow fiber ultrafiltration membrane was first stated
in1966, this type of membrane is not suitable for RO or
NF process which applied high pressure because of poor
mechanical properties [7], however, it is one of the most
interesting membranes modules as it has many advantages
among other modules such as high productivity per unit
volume [8], self-supporting and easy operation [4].
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Z. W. Rashad / Iraqi Journal of Chemical and Petroleum Engineering 23,2 (2022) 47 - 53
48
The importance of hollow fiber membranes as low-
pressure membranes (LPHF) is their ultrafiltration
performance, ultrafiltration together with microfiltration
gives good separation performance for drinking water.
Recent studies suggest that MF and UF can remove all
particles and colloids as well as viruses completely when
used with suitable pre-treatment or post-treatment which
gives this technology advantage to be the new technology
generation for drinking water of the 21st century [9].
Fabrication of hollow fiber membranes is not an easy
operation especially when specific structure morphology
is required [10].
This review demonstrates literature from some
researchers to simplify the process steps and give start
point for researchers to study the change in hollow fiber
membranes structure by changing one or two factors of
the preparation process.
However, many researchers reported different and
conflicting results for the same operating conditions but
different polymers, in terms of permeation and rejection
(membranes performance).
2- Preparation Main Steps and Factors
The purpose of studying membranes technology is to
improve its performance (flux and rejection) via structure
control as mentioned before [1]. The structure is usually
sponge-like or finger-like with a selective skin layer on
the surface as shown in Fig. 2, sponge-like is the favored
as finger-like leads to a lack in the mechanical stability of
hollow fiber membranes [4].
Preparation steps are the dope solution, spinning
process, and post-treatment of hollow fiber membranes,
these steps are discussed in the next section, and all
operating conditions remain constant except for the factor
to be changed and studied.
Fig. 2. (A) Finger-like structure, (B) Sponge-like
structure, (C) Uniform sponge-like structure [11]
2.1. Dope Solution Preparation
The first step to prepare dope or polymer solution is to
select a suitable polymer powder and good polymer
solvent. After materials selection, a magnetic stirrer is
required to homogenize the polymer solution as shown in
Fig. 3.
Fig. 3. Polymer Solution Preparation [12]
Firstly, polymer powder should be dried to remove
moisture. For PSF polymer drying, 60 °C for at least 12 h
is required then polymer powder added to NMP solvent of
22/88 PSF/NMP weight percent and mixed until
homogenized at room temperature (25-27 °C) [13].
PVC polymer is a good inexpensive choice for hollow
fiber manufacturing[N]. PVC powder was dissolved in di-
methyl acetamide DMAC chemically and thermally stable
solvent [14] after dried for 24 hr. at 70 °C under
continuous mixing period (5 days) at room temperature
(25 °C). PVC/DMAC ratio was 14/88 w/w, [10].
Mustaffar et al. [1] chose PES polymer with three
different concentrations and polyethylene glycol PEG as
polymer additive, 18/72/10, 20/70/10, and 28/62/10,
PES/NMP/PEG weight percent of 100-gram polymer
samples were stirred at 30 °C. Wang et al. [15] followed
the system PSF/NMP/H2O ( water as a non-solvent
additive) and also use three concentrations of PSF
polymer 26/70/4, 28/68/4, and 30/66/4, PSF polymer
powder was dried at 100 °C for 10 hr.
Adding PEG to polymer solution in the system of
Mustaffar et al. [1] is to enhance porosity on the
membrane skin layer. Polymer concentration together
with the solvent ratio is the most significant parameter
that directly affects membrane properties. Increasing
concentration leads to an increase in dope solution
viscosity, dense skin layer becomes thicker, and reduction
in macro voids, [1] as well as transferring membrane
structure from finger-like to sponge-like [7]. On the other
hand, adding a specific amount of non-solvent (water,
ethanol, acetone) to the polymer solution well provides a
good membrane porous structure [13-16].
2.2. Spinning Process
The spinning process includes several stages as shown
in Fig. 4, starting with dope solution located in a spinning
container Fig. 4 No.4 and leaving for 24 hr. to de-bubble
or de-gas polymer solution [10], [16] [17].
Z. W. Rashad / Iraqi Journal of Chemical and Petroleum Engineering 23,2 (2022) 47 - 53
49
The dope solution was pressed to a spinneret with a
specific inner and outer diameter by nitrogen pressure,
0.5, 0.6, 0.75, or 0.8 bar are recommended pressure as the
morphology of the hollow fiber membrane was not
affected by changing dope solution pressure in this range
[12].
Fig. 4. Spinning process stages, (1) Nitrogen cylinder, (2)
Pressure valve regulator, (3) Nitrogen pressure gauge, (4)
Dope solution container, (5) Dope solution control valve,
(6) Bore fluid container, (7) Dosing pump, (8) Spinneret,
(9) Air gap, (10) Coagulants bath, (11) Take-up unit, (12)
Hollow fiber collecting vessel, (13) Distilled water for
extra wash [12]
a. Air gap
Airgap is defined as the distance between the spinneret
and the external coagulants surface, this distance switches
the phase inversion process from wet phase inversion to
dry/wet phase inversion [10]. Many researchers study the
effect of air gap length on the hollow fiber membrane's
structure and came back with confusing results about how
the air gap increase or decrease membrane performance in
terms of permeation and rejection, Table 1 illustrates
some of the researcher's conclusion about air gap length
outcome for polysulfone PSF, Polyvinyl chloride PVC,
and polyether sulfone PES.
Table 1. Effect of air gap on membrane performance
reported by different researchers
Polymer
Air gap
length
Permeation
Separation
factor
Reference
PSF Increased Decreased Increased Aptel et al. [18]
PSF Increased No-effect No-effect East et al. [19]
PSF Increased
Increased then
decreased with
further increase
of airgap length
- Kim et al. [20]
PSF Increased
Not significantly
affected
Increased Tsai et al. [21]
PES 15-120 cm Decreased Increased et al. [22]
PES 0-14.4 cm
Significant
decrease
-
Chung and Hu
[23]
PVC 5-25 cm Increased Decreased Khayet et al. [10]
For PSF polymer Tsai et al. [21] explained the increase
in the separation factor is due to the increase in the skin
layer of the hollow fiber membranes structure. Chung and
Hu [23] describe the change in permeation as related to
the high elongation stress of hollow fiber membrane in
the presence of an air gap. Khayet et al. [10] indicated an
increase in the mean pores of outer hollow fiber
membranes surface while the inner pore size almost
remained the same with increasing air gap and also linked
this change to elongation force.
b. Bore Fluid and Coagulants
Bore fluid or internal coagulant is maintained in a
container Fig. 4 No. 6 and pumped with a dosing pump to
the inner tube of spinneret together with a dope solution
which inter the external spinneret tube, bore fluid fed with
a very low flow rate (2, 3 or 4 ml/min), distilled water at
room temperature is a good choice [10], [12]. Polymer
falls from spinneret with a speed rate the same as gravity
speed [10]. Bore fluid or internal coagulant also a key role
to control membrane structure, distilled water is a good
non-solvent for PSF while alcohol (ethanol) is weak,
choosing the optimized ratio of water/alcohol mixture
may reduce the big macro-voids in membrane structure
[15].
Once the nascent hollow fiber membranes touch the
external coagulation fluid (usually tap water), solvent
non-solvent exchange occurred and form the asymmetric
structure, generally the fast the coagulation rate the more
finger-like macro voids formed while the slow
coagulation rate gives the favored sponge-like structure
[13].
To slow down the coagulation rate, a small amount of
solvent additive to bore fluid or coagulant bath well
reduces the coagulation and induces the formation of a
sponge-like structure [15]. Appropriate additives should
be environmentally friendly, low toxicity, and
commercially available. The best coagulant to be used is
water, the NMP and DMAC are the best as solvent
additives [15].
The temperature of coagulants is considered an
important factor to control membrane structure, Wang et
al. reported that reducing coagulation bath temperature
from 27 C to 20 °C increases the membrane permeation
and decreases the selectivity, while further temperature
reduction to 10-15 °C leads to a significant reduction in
membrane selectivity performance due to the formation of
macro voids on the membrane surface [15].
2.3. Post Treatment
The final step of fabrication of hollow fiber membrane
is post-treatment, the importance of post-treatment is to
avoid membrane collapse and get rid of residual solvent
[10], [15], [16]. Many researchers reported a different
kind of post-treatment to protect the membrane from
damage.
Z. W. Rashad / Iraqi Journal of Chemical and Petroleum Engineering 23,2 (2022) 47 - 53
50
Wang et al. [15] suggest keeping hollow fiber PSF
membranes in water for 72 hr. followed by a drying step
at conditions of 25 °C and (60-65%) relative humidity.
Khayet et al. [10] made it three steps, first, wash hollow
fiber PVC membranes with water for 48 hr. to remove the
solvent, and second immerse hollow fiber membranes in
glycerol aqueous solution of 40% volume ratio to avoid
collapse, and third dry at room temperature.
Another method is to treat hollow fiber membranes with
non-solvent with low surface tension such as ethanol [13],
Mansourizadeh & Ismail [13] submerged PSF hollow
fiber membranes in ethanol for half an hour and then let
the non-solvent evaporate by air exposure at room
temperature to prevent pores breakdown. For PES hollow
fiber membranes, Mustaffar et al. recommended two days
of water washing, two days of methanol immersion, and a
drying period by hanging hollow fiber membranes for 7
days before use.
3- Hollow Fiber Membranes Characterization and
Performance
The characterization of hollow fiber membranes was
evaluated by Scanning Electron Microscope SEM as this
device gives a clear image of membrane structure in terms
of skin layer thickness; porosity distribution and pores
shape also give a good indicator of inner and outer
diameter measurements [16].
The inner and outer diameter also can be measured by a
linear Vernier microscope with ±1µm. accuracy [10].
Permeation and selectivity performance required a
specially designed lab-made unit as shown in Fig. 6 which
was suggested by some researchers.
Before explaining the performance system the hollow
fiber must be cut to more than 20 cm (depending on tube
design) and secured in a special tube usually made of
stainless steel with an inlet and outlet open on the side as
shown in Fig. 5 and get a free end of membranes by
sealing the two end of the tube with epoxy resins and let it
cure for 24 hr. [12], [24].
Fig. 5. Hollow fiber membrane special tube [24]
Fig. 6. Schematic diagram of hollow fiber membrane
performance system, (1) feed tank, (2) pump, (3) control
valve, (4) flow meter, (5) gauge pressure, (6) hollow fiber
tube, (7) gauge pressure, (8) retentate, (9) permeate, (10)
collecting tank [12]
Performance system for pure water permeation PWP
includes forcing distilled water to the inlet tube with
specific pressure and flow rate and passes through hollow
fiber membranes from outer to the inner surface and by
collecting permeates for a specific time, PWP can be
calculated by the following equation:
𝑃𝑊𝑃𝐹 =
Q
A ΔP
(1)
Where:
Q: volumetric flow rate, l/h
A: membrane surface area, m2
ΔP: Pressure drop, bar [25]
For rejection calculation, a solution with a specific
amount of PEG (800, 1000 ppm) [12], [16] is pumped
instead of distilled water and the equation used was as
follows:
𝑅(%) = ( 1 −
𝐶𝑝
𝐶𝑓
) × 100 (2)
Where:
Cp: concentration of PEG of permeation, ppm
Cf: concentration of PEG of the feed solution, ppm [25]
Note: UV spectrometer is used to find concentration by
knowing PEG wavelength and create a calibration curve
4- Conclusion
There are many factors to be controlled in the
fabrication of hollow fiber membranes. Some of these
factors direly affect the structure of the membrane and
eventually, the overall performance and even slight
change give a different morphology.
It is important to keep operating conditions constant
when studying the change of specific factor.
Z. W. Rashad / Iraqi Journal of Chemical and Petroleum Engineering 23,2 (2022) 47 - 53
51
1- Polymer concentration is remarked as the most
effective on the morphology of hollow fiber
membranes, the high the concentration the thick the
skin layer, and a more sponge-like structure is
produced. From researcher reports, 14% of polymer
concentration and above is a good start, not to forget
the effect of suitable additives to the dope solution on
the performance of the membranes. DMAC is a
suitable solvent for a different type of polymers as it is
miscible with water and have good thermal and
chemical stability
2- The air gap was the most conflicting factor, however,
5-10 cm of air gap was expected to enhance
membranes selectivity, especially for PSF and PES
while decreasing it for PVC
3- Water is fantastic for bore fluid and coagulants with
appropriate additives, alcohol in a coagulant bath
gives a reduction in macro-voids formation. A small
amount of solvent like DMAC to bore fluid or
coagulation bath raises the sponge-like structure of
membranes
4- Post-treatment of hollow fiber membranes has two
main reasons, wash residual solvent, and prevent
membrane collapse.
5- Finally, the favorite performance (increasing
permeation or selectivity) of hollow fiber membranes
depends on its application, gas separation, or drinking
water production
Abbreviation
PSF: Poly Sulfone
PES Poly Ether Sulfone
PVC Poly Vinyl Chloride
RO Reverse Osmosis
NF Nano Filtration
LPHF Low Pressure Hollow Fiber
UF Ultra-Filtration
NMP N-methyl-2-pyrrolidone
DMAC N,Ndimethyl acetamide
SEM Scanning Electron Microscope
PWPF Pure Water Permeation
UV Ultraviolet
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تحضير االغشية النفاذية المجوفة ورقة مراجعة في دراسة وتحليل ظروف التشغيل لعملية
زيد وعدهللا رشاد
جامعة بغداد/كلية الهندسة
الخالصة
تنتج االغشية النفاذية المجوفة عن طريق عملية فيزيائية تسمى انقالب الطور الرطب أو الجاف / الرطب.
وانتهاًء التصنيع، مواد اختيار من )بدًءا مختلفة عوامل على وتعتمد الخطوات من العديد التقنية تتضمن
ت محلًيا(. المصنوعة المجوفة النفاذية لالغشية الالحقة أهم بالمعالجة على الضوء هذه المراجعة دراسة سلط
الداخلي التركيب توصيف في وتتحكم تؤثر التي الفائق ألالعوامل الترشيح ذات المجوفة األلياف غشية
المستخدمة في التطبيقات المختلفة.
سلفون )بولي البوليمرات من مختلفة أنواع ثالثة على باالعتماد الدراسة سلف PSFتمت إيثر بولي ون ،
PES و بولي فينيل كلوريدPVC لدراسة تغير مورفولوجيا االغشية الليفية المجوفة مع عوامل تصنيع مختلفة )
تاثير دراسة المراد العامل وتغيير التشغيل عند تثبيتها يجب والتي المؤثرة للعوامل معقولة بداية نقطة وإعطاء
تغييره على االغشية.
النفاذية المجوفة, انقالب الطور, عملية الترشيح, البوليمر الكلمات الدالة: االغشية