Effect of BMIM-Chloride Physio Chemical Properties of Electrospun Nanofiber

Membrane for Waste Water

by

Ahmad Tarmizi bin Mohd

18439

Progress Report submitted in partial fulfilment of

the requirement for
the Bachelor of Engineering (Hons)
(Chemical)

FYP 2 SEPTEMBER 2018

Universiti Teknologi PETRONAS,

32610, Bandar Seri Iskandar,
Perak Darul Ridzuan

i
 CERTIFICATION OF APPROVAL

Effect of BMIM-Chloride Physio Chemical Properties of Electrospun Nanofiber

Membrane for Waste Water
by

Ahmad Tarmizi bin Mohd

18439

A Progress Report submitted to the

Chemical Engineering Programme
Universiti Teknologi PETRONAS
in partial fulfilment of the requirement for the
BACHELOR OF ENGINEERING (Hons)
(CHEMICAL ENGINEERING)

Approved by,

_____________________
(Dr Mohd Dzul Hakim Wirzal)

ii
 UNIVERSITI TEKNOLOGI PETRONAS
BANDAR SERI ISKANDAR, PERAK
September 2018
CERTIFICATION OF ORIGINALITY

This is to certify that I am responsible for the work submitted in this project, that the
original work is my own except as specified in the references and acknowledgements,
and that the original work contained herein have not been undertaken or done by
unspecified sources or persons.

________________
AHMAD TARMIZI BIN MOHD

iii
 ABSTRACT

Water is a source that crucial to any life on earth. In industrial, water is being
used for various process that change the purity of water to be contaminated, hence
could not be used for any other purpose. As part of water treatment before being release
into environment, the processed water must have a certain minimum composition to
be able for the treated water to comply with regulation of OSHA. However, the
separation of contaminant need to be efficient with reducing cost of treatment as part
of economical and environment to be balanced. Nanofiber membrane is the answer to
increase the proficiency of liquid separation. The membrane being fabricated using an
electrospinning method, as in to achieve the diameter of nano size for the membrane
thread. Hence, increasing the surface area of membrane and the porosity as well as
selectivity of permeate. Despite the advantages over the usage of nanofiber membrane,
being said that the nanofiber membrane would gain an increase if the polymer itself
fuse with ionic liquid. In this particular case, nylon 6, 6 being the polymer that having
properties of hydrophilic, with additive of ionic liquid, 1-Butyl-3-methylimidazolium
Chloride (BMIM-Chloride). Ionic liquid additives in polymer nanofiber membrane
would increase the performance of membrane with an increase of tensile strength of
the membrane. This research would taking in the comparison of the presence of
BMIM-Chloride in the nylon 6, 6 nanofiber membrane. An initiative taken also being
observe is the difference in BMIM-Chloride concentration presence in nylon 6, 6 as
part of optimization of ionic liquid usage in polymer nanofiber membrane fabrication.
Apart from that, the fusion method of the BMIM-Chloride and nylon 6, 6 would
investigated as part of increasing the research value of polymeric ionic liquid
membrane.

iv
 ACKNOWLEDGEMENTS

All praises to the Almighty for granting me the strength and health throughout
my project. I would like to thank to my supervisor, Dr Dzul Hakim Wirzal for his
guidance and supervision for this research. Despite being pressed under tight schedule
and tied with others responsibility and commitment, it does not stop him from giving
me the support I needed during the whole research ongoing. A lot of thanks to members
of YOURS 4.0 for the support and information sharing, especially those whom under
Dr Dzul Hakim Wirzal supervision. It help a lot on helping to improve the research.
To my parents and family, their presence motivate me to go through hardship during
the research ongoing. It is beyond my imagination on how they contributed to my
mental support. To my friends, thank you for the helps and support, the memory shall
be cherish together. Thank you for the push you gave me for me to reach the final line.

v
 TABLE OF CONTENT

CERTIFICATION OF APPROVAL ii
CERTIFICATION OF ORIGINALITY iii
ABSTRACT iv
ACKNOWLEDGEMENTS v
LIST OF FIGURES viii
LIST OF TABLES ix

CHAPTER 1: INTRODUCTION 1
1.1 Background Study 1
1.2 Problem Statement 2
1.3 Objectives of the Study 3
1.4 Scope of Study 3

CHAPTER 2: LITERATURE REVIEW 4

2.1 Membrane Technology 4
2.2 Nanofiber Membrane 4
2.3 Electrospinning 5
2.4 Soaking 6
2.5 Nylon 6, 6 6
2.6 1-Butyl-3-Methylimidazolium-Chloride 6-7
2.7 Membrane Fouling 8
2.8 Previous Application of Nanofiber Membrane 9 - 10

CHAPTER 3: METHODOLOGY 11
3.1 Experimental Flow 11
3.2 Materials 12
3.3 Membrane Fabrication 13
3.3.1 Preparation of BMIM-Cl Solution 13

vi
 3.3.2 Preparation of Nylon 6, 6 Solution 13
3.3.3 Preparation of Nylon 6, 6/BMIM-Cl 13
(Soaking)
3.3.4 Preparation of Nylon 6, 6/BMIM-Cl 13 - 14
(Fusion)
3.3.5 Electrospinning of Nylon 6, 6/BMIM- 14
Cl
3.4 Membrane Characterization 15
3.4.1 Porosity 15
3.5 Filterability Analysis 16
3.5.1 Flux 16
3.5.2 Permeability 17
3.5.3 Filtration of Oily Wastewater 17
3.6 Gantt Chart 18

CHAPTER 4: RESULTS AND DISCUSSION 19

4.1 Porosity Test 19
4.2 Permeability & Flux Test 19

CHAPTER 5: CONCLUSION 20

REFERENCES 21 - 22

vii
LIST OF FIGURES

Figure 2.1 Electrospinning process diagram 5

Figure 2.2 The structure of Nylon 6, 6 7

Figure 2.3 The structure of BMIM-Chloride 8
Figure 3.1 Flow of the methodology 12

viii
LIST OF TABLES

Table 2.1 The comparison between same researches of different 9 - 10

materials.
Table 3.1 Amount of material for sample preparation 14
Table 4.1 Data taken for porosity test. 19
Table 4.2 Calculated data for porosity 19
Table 4. 3 The permeability test result 20

ix
 CHAPTER 1

INTRODUCTION

1.1 Background of Study

As part of crucial resource on earth, the water is essential in human and

environment need. It is being reported that, almost one over fourth of world population
does not have the reach for fresh water with decent quality and amount, with over 80
countries is facing the issue of water cut out (Karagiannis & Soldatos, 2008). But, the
building over facility to cover water shortage is rapidly being constructed in form of
mega structure such as pipeline, and aqueducts, in the 20th century, giving out huge
benefit to world population with on specification quality of water (Gleick, 2003).

Furthermore, modern usage is consuming a large number of water to their plant

usage such as cooling water, demineralized water and as part of process itself. The
used water has to be released out after being contaminated and need to be treated before
getting release into environment, or recycled into storage. Most of the time, there are
two method of water treatment being used; physical method which is through
sedimentation & filtration, disinfection & chemical oxidation as part of chemical
method, & biological process of anaerobic and aerobic digestion (Liao et al., 2017).

Having said that, the answer to the high quality of water produced with low
cost, membrane have gain popularities in terms of industrial and research values. The
membrane technology itself being class into few such as microfiltration (MF),
ultrafiltration (UF) and nano-filtration (Fane et al., 2015).

Nanofiber membrane most efficiently being fabricated with its fluid control
over the diameter of nanofiber, the microstructure and having vast material selection.
(Liao et. Al 2018). Furthermore, the presence of ionic liquid inside nanofiber

1
membrane would increase the viscosity and conductivity of the membrane, with range
of certain concentration (Javed et al., 2017).

1.2 Problem Statement

Polymer membrane is best separation current being existed in particular scope

area, but despite that, it lacks few ingredient to make it more valuable and awakens its
full potential.

The fabrication through electrospin seems to be affected by the conductivity of

the polymer itself. Polymeric nanofiber membrane itself has gain increase in
performance in porosity & permeability. But, it lacks the ability to perform better
separation on selectivity regarding for maximum efficiency to produce a product that
has low ppm of unwanted components to increase its value.

Polymer nanofiber membrane also seen to be have low resistance when it

comes to thermal stability or high pressure included in certain process. This could
reduce the attraction of polymer nanofiber membrane usage in industry as the
separation process usually occur in critical condition.

Risk of fouling is an event that commonly occur which reduce its separation
capability. The surface layer of membrane blocked by residual of feed, lowering the
entering percentage into membrane. It is eventually to occur in any process involving
membrane application, but still could be controlled if the problems are known (Drews,
2010).

2
 1.3 Objectives

This study is to investigate the effect of BMIM-Cl in improving the properties

of the membranes. Thus, the objectives of this study are listed as follows:

i. To study the effect of additives in the fabrication of nanofiber membranes.

ii. To research the effect of concentration of additives in fabrication of nanofiber
membranes.
iii. To investigate the performance of nanofiber on oily waste water treatment
separation.
iv. To compare the method of additives fusion with nanofiber membrane.
v. To characterize and optimize the nanofiber membrane in presence of additives.

1.4 Scope of Study

To fulfil the objectives of this study, below are the scopes covered in this study:

i. Fabrication of nylon 6, 6 and nylon 6, 6/ BMIM-Chloride as electrospun nanofiber

membrane.
ii. Addition at different concentration of BMIM-Chloride powder (0 wt. %, 1 wt. %,
2 wt. %, 3 wt. %, 4 wt. %, and, 5 wt. %) as the additives to the polymeric nanofiber
membrane.
iii. Comparing the method of adding additives, BMIM-Chloride to nylon 6, 6
nanofiber membrane ; Soaking nylon 6, 6 electrospun nanofiber membrane into
BMIM-Chloride (0 wt. %, 1 wt. %, 2 wt. %, 3 wt. %, 4 wt. %, and, 5 wt. %)
iv. Study of the morphology and the cross sectional of the membrane by using Field
Emission Scanning Electron Microscope (FESEM).
v. Observation on the infra-red spectra and interaction between nylon 6, 6 and
BMIM-Chloride by using Fourier Infrared Spectra (FT-IR).
vi. Analyzation of the nanofiber membrane surface roughness by using Atomic Force
Microscope.
3
vii. Evaluation on the separation performance of the membrane by conducting flux and
permeability experiment.

4
 CHAPTER 2

LITERATURE REVIEW

2.1 Membrane Technology

Membrane technology are currently being studied on its potential of

application on many field that including the separation process and selectivity of
materials. Most currently being study is the acid gas removal using membrane and the
oily waste water removal.

Membrane technology proves to have low energy consumption, mild operating

condition for separation, and optimization of membrane with diverse requirements
(Liao et al., 2018). The core application of membrane is for the membrane to have high
permeation rate for targeted separation, selectivity of process, and having versatility
in different module, as well as ability to tolerate against thermal excursion (George et
al., 2016).

2.2 Nanofiber Membrane

Electrospun nanofiber membrane has become part of the membrane technology

progressing in order to increase its efficiency in separation process. The characteristic
of nanofiber membrane inherited from the nanofiber based architecture, it gain the
nature of high surface area, higher porosity & gaining high orientation of the
nanofibers alignment (Liao et al., 2018).

The application of nanofiber membrane has been widen to several fields of

science, such as energy storage (Thavasi et al., 2008), healthcare and biotechnology
(Sun et al., 2014).

5
2.3 Electrospinning

This process has been going on starting on 1900s with aspect of forming a
complex process to control nanofiber formation, setting the rise of nanotechnology and
being the foundation of current modern analysis methods (Formhals, 1934).

This process using electrospinning, shown in figure 2.1, compared to the gas
jet method and melt fibrillation, showing lower cost with resulting in higher production
rate (Lin et al. 2008). Electrospinning also prove to have high level of diversity in
aspect of nanofiber controls diameter, and the microstructure arrangement with wide
selection of material to be use as components. The membrane fabricated also gain high
porosity which higher than 90% with wide surface to volume ratio (Liao et al., 2018).

Figure 2.1: Electrospinning process diagram.

6
2.4 Soaking

According to L. J. Lozano et al., 2010, soaking or direct immersion is one the

three method to produce supported ionic liquid membranes (SILM), which is direct
immersion, pressure, & vacuum. Direct immersion is a direct contact of the membrane
into the ionic liquid to allow the ionic liquid to seep in the membranes (P. Scovazzo et
al., 2004). The pressure method, otherwise require to the membrane to be place into
ultrafiltration unit, putting ionic liquid into at certain amount and let the nitrogen
pressure to advert pressure, forcing the ionic liquid to replace the air inside membrane
pores by ionic liquid (F. J. Hernández-Fernández et al., 2009). Vacuum method, the
membranes is being fully submerge in certain amount of ionic liquid, while the vacuum
is being applied towards the setup, causing for the air to press out from the membranes
pores (R. Fortunato et al., 2005).

Based on L. J. Lozano et al., 2010, the method of those three results shows that
the ionic liquid has been averagely distributed throughout the membranes, excluding
the huge macrospores which is partially filled. Comparing the three methods, vacuum
shown that amount of ionic liquid filled the pores differ according to the ionic liquid
viscosity, which higher viscosity lead to less being filled into the membrane pores.

SILM stability is majorly being affected by its type of membrane and ionic
liquid, production of SILM, and as well as the interfacial tension of aqueous and
membrane (J. Wang et al., 2016). The stability of SILM is greater when it comes to
hydrophobic membrane compared to hydrophilic membrane (L. Ropel t al., 2005).

7
2.5 Nylon 6, 6

This polymer is constructed with chain of adipic acid and

hexamethylenediamine with 12 carbon atoms, as show in figure 2.2. Due to its
hydrophilic nature, nylon 6, 6 is a promising candidate in fabrication of nanofiber
membrane. Other of its properties is decent mechanical characteristic and high
compatibility with a polyamide selective film (Huang & McCutcheon, 2014).

The nature of hydrophilic formed in nylon 6, 6 as the presence of functional

group of amide as it connected to oleophilic hydrocarbon chain. The low specific
gravity of nylon 6, 6 contributed to ideal target on fabrication of light fabrics.

Figure 2.2: The structure of Nylon 6 6

2.6 1-Butyl-3-Methylimidazolium chloride, BMIM-Chloride

BMIM-Chloride, shown in figure 2.3, is part of ionic liquid family with melting
point range 77 to 79 oC. BMIM-Chloride has the greater effect in nanofiber membrane
presence on aspect of viscosity and conductivity of the membrane, as well as the
morphology of membrane (Javed et al., 2017).

The research of BMIM-Chloride conducted shown that higher concentration of

BMIM-Chloride shown an increment in viscosity but starting to drop after passing
certain concentration. It is due to the presence large quantity of BMIM+ and small
presence of Cl- has invaded the hydrogen bond between cellulose, causing it to break.

The presence of BMIM-Chloride in cellulose acetate also seems to enhance the

size of diameter to be larger 5 times compared to 0% of BMIM-Chloride in cellulose
acetate.

8
 The increasing conductivity within higher concentration of BMIM-Chloride
also affecting the jet stability, reducing the bead formation onto fibres (Javed et al.,
2017).

Figure 2.3: The structure of BMIM-Chloride

2.7 Membrane Fouling

Every membrane separation is struck with the problem that always get in the
way which is fouling. This weakness greatly affect the membrane effectiveness and
life span in industrial usage. Membranes fouling could occur in various unwanted
events which cost the company through maintenance and replacement (Singh, 2006).

The fouling occur when deposition of particles & macromolecules from the
feed stream forming a layer at the surface of the membrane and its pores causing the
entering part is partially blocked. This reduce the usage of membrane to perform
separation processing. This has resulting for flux declination (Chang et al., 2002). The
fouling removal method is to apply back pressure onto the membrane or by using
specific chemical to remove it, but it is only possible for temporary-fouled membrane.
This would never could be done for the permanent fouled membrane.

This phenomena would commonly affect a hydrophobic type of membrane due

to the hydrophobic molecule attraction towards the surface of membranes, which
resulting the membrane to be fully covered by deposition (Rana and Matsuura, 2010).
To overcome this problematic issue, composite type of membrane are being used

9
instead of polymeric (Muhamad et al., 2016). The composited type of membrane could
fabricated through blending the membrane base which hydrophobic to hydrophilic
activities, which improve the wetting resistance (Liang et al., 2013).

10
 2.8 Previous Applications of Nanofiber Membrane

The previous research on the fusion of ionic liquid into polymeric nanofiber membrane is compared in table 2.1. The method
is being constant as term of comparing the result base on the chemical used. These shown almost same result achieved, in term of
tensile strength and diameter of nanofiber

Table 2.1: The comparison between same researches of different materials.

No Materials Application Method of Types of Results References

9

Fabrication Separation
1  Polycaprolactone Oil/Water Electrospinning MF  Tensile strength increase (R, P. Sundaran, A, &
Athiyanathil, 2017)
 Beeswax (BW) Separation  High oil sorption capacity
 BW concentration
increase, average diameter
fibre decrease
2  Polylactic Acid Oil/Water Electrospinning MF  High roughness lead to (Dai et al., 2016)
(PLA) Separation higher oil wettability.
 ZIF-8  Mechanical property
improvement.
  Tensile strength increased.
 ZIF-8 presences decrease
the diameter of fibre.
3  Polyether Sulfone Oil/Water Electrospinning MF  PES/PVDF membrane has (Cao et al., 2017)
(PES) Separation increase in thermal
 PVDF properties performance.
4  PVA Waste water Electrospinning MF  ZIF-8/PVA has stable and (Fan et al., 2017)

10

ZIF-8 flexible structure of

membranes.
 Most likely to be new type
of adsorbent for
membrane.
 CHAPTER 3

METHODOLOGY

3.1 Experimental Flow

Below is the steps of flow of experiment taken to start the experiment, which
distributed in five stages. This included the preparation of polymer solution and
additives, fabrication of membrane, characterization of the membrane and evaluation
of separation performance.

Base on the figure 3.1, the flow for experimental work is being generally
represented for the whole research.

11
 Figure 3.1: Flowchart of the methodology.

3.2 Materials

Materials being used for this research is; formic acid, FA (98-100%, MERCK),
glacial acetic acid, AA (99.85%, VWR Chemicals), nylon 6, 6 pellets (Sigma Aldrich),
1-Butyl-3-methylimidazolium chloride ≥98.0% (HPLC), De-ionized water

12
3.3 Membrane Fabrication

3.3.1 Preparation of BMIM-Chloride

BMIM-Chloride was prepared by solving the BMIM-Chloride powder into de-

ionized water to turn it into 99% -100% solution.

3.3.2 Preparation of Nylon 6, 6

Nylon 6, 6 mixture solution is done by dissolving the nylon 6, 6 pellets (14.0

wt. %) in a mixture of formic acid and acetic acid glacial with ration of 1:1. Nylon 6,
6 were gradually added into the mixture of formic acid and acetic acid each 2 hours.
10 wt. % at first, left for two hours, and adding 20 wt. % to the mixture, after two
hours, balanced of 70% is added into the mixture. The solution is heated at 60 oC with
180 RPM on the magnetic stirrer. The solution is then left stirred overnight for 12
hours until the homogenous solution is formed.

Nylon 6, 6 and solvent (Formic Acid and Acetic Acid) were kept constant at
14.0 wt. % and 86.0 wt. % of 20 g basis respectively. The weight of BMIM-Chloride
added into polymer membrane is calculated with equation 3.1.

𝑥
𝐴% = (𝑥+𝑌) (3.1)

Where;
 A = Wt. % of BMIM- Chloride
 x = Weight of BMIM-Chloride used in nylon 6, 6 mixture
 Y = Weight of nylon 6, 6 used in mixture with acids mixture.

13
3.3.3 Preparation of Nylon 6, 6/BMIM-Chloride Membrane (Soaking)

BMIM-Chloride with particular concentration, as shown in table 3.1, is turn

into aqueous solution by diluting into de-ionized water. The membrane with same area
size is immersed directly into the ionic liquid for overnight. The membrane then will
be taken out and exposed to open air for drying.

Table 3.1 Concentration of Ionic Liquid with total volume of ionic liquid

Concentration, % Volume of Ionic Liquid, ml Volume of De-

Ionized Water, ml
1 1 99
2 2 98
3 3 97
4 4 96
5 5 95

3.3.4 Electrospinning of Nylon 6, 6 and Nylon 6, 6 /BMIM-Chloride

A 5 ml syringe used as the solution container attached with capillary needle

with tip of 0.6 mm inner diameter. The machine was set with 0.4 mL hr-1 of flowrate.
The tip of needle clipped with voltage of 20.0 kV and collector was set up a distance
of 15 cm from the tip of needle. The collector were covered with aluminium foil for
easy harvest and set with rotation of 500 RPM.

3.4 Membrane Characterization

Membrane will have it analyse by using Field Emission Scanning Electron

Microscope (FESEM) was used to observe the morphology and microstructure of the
nanofiber membrane. All sample were loaded into a metal substrate and coated with
thin layer of gold, by using the carbon tape. The Fourier Infrared Spectra (FT-IR) used
to observe the infrared spectra and the interaction between the nylon 6, 6 and BMIM-
Chloride particles. Atomic Force Microscope were used to read the surface roughness
of the membrane.
14
3.4.1 Porosity

Fabricated membrane will have its membrane run through porosity test. Each
membrane sample will be 15 mm length and width. The thickness will be measured
each. Each membrane pieces will have its weight initial taken before immersed into
distilled water for 5 minutes. The weight after soaking will be taken again will the
extra water dripping being wiped first without absorbing the water content inside. The
membrane pieces will be put into oven, heated up to 60 °C for 2 hours. The weight
after drying is recorded. The data taken will be use to find the value percentage of
porosity each pieces of membrane through Equation 3.2, Equation 3.3, and Equation
3.4.

𝑉𝑡𝑜𝑡𝑎𝑙 = 𝐿 × 𝑊 × 𝑥 (3.2)

Where;
L : Length of membrane
W : Width of membrane
x : Thickness of membrane

𝑤 −𝑤
𝑉𝑤𝑎𝑡𝑒𝑟 = 10001 𝑘𝑔/𝑚
2
3 (3.3)

Where;
W2 : Weight of the wet membrane
W1 : Initial weight of the membrane

𝑉𝑤𝑎𝑡𝑒𝑟
𝑃𝑜𝑟𝑜𝑠𝑖𝑡𝑦 = ( ) × 100 (3.4)
𝑉𝑡𝑜𝑡𝑎𝑙

Where;
Vwater : Volume of water inside membrane
Vtotal : Volume of membrane

15
3.5 Filterability Analysis

3.5.1 Flux

The flux membranes were tested for their ability for pure water flux (PWF) as
a reference to wastewater flux. The membrane were tested by using Cross-flow set up.
The membrane size of 9 cm2 were cut and fit in between set up casing to be seal and
pump the water through the membrane.

𝑉 𝐿
𝐽= ( ) (3.5)
𝐴𝑡 𝑚2 ℎ

Where;
V = Volume (L)
A = Effective filtration area (m2)
t = Time (h)

3.5.2 Permeability

Permeability (L) of the membranes were calculated as Equation 3.6.

𝐽 𝐿
𝐿= ( ) (3.6)
𝑇𝑀𝑃 𝑚2 ℎ 𝑏𝑎𝑟

Where;
TMP = Trans-membrane pressure

16
3.5.3 Filtration of Oily Wastewater

The membranes is being evaluated by using real process wastewater obtain

from Kerteh Industrial Area. This test is include the flux and permeability of the
membrane. The sample of wastewater will undergo for turbidity evaluation for its
initial and final value. The reading of initial and final for turbidity measured by using
a turbidity meter. The data gain is calculated and recorded using the equation 3.7.

𝑐0 −𝑐𝑓
𝑅𝑒𝑚𝑜𝑣𝑎𝑙 % = × 100% (3.7)
𝑐0

Where;
C0 = Initial concentration of constituents (µg/L)
Cf = Final concentration of constituents (µg/L)

17
 CHAPTER 4

RESULT & DISCUSSION

4.1 Porosity Test

Table 4.1: Data taken for porosity test.

1 2 3
Thickness, mm 0.268 0.312 0.337
Weight1 (Initial), g 0.012 0.013 0.012
Weight2 (Wet), g 0.095 0.096 0.095
Weight3 (Dried), g 0.012 0.012 0.011

Table 4.2: Calculated data for porosity.

1 2 3
VTotal, m3 6.08 × 10-8 7.02 × 10-8 7.58 × 10-3
VWater, m3 8.30 × 10-8 8.30 × 10-8 8.30 × 10-8
Porosity, % 137.65 118.23 102.62

The data average is numbered 1, 2, and 3 taken from single base nylon 6, 6
electrospun nanofiber membrane with 0 wt% of additive. The porosity average is
119.50 % which exceed the 100% value. This proves the efficiency of electrospinning
method on nanofiber membrane production. For current time, this will be the
reference value for future update of membrane with additive of fusion and soaking
method.

19
4.2 Permeability & Flux Test

Using the equation of 3.5 & 3.7, the flux gain for nylon 6, 6 with 0 wt% with
pure water testing is 399.992 L/m2h, with permeability of 3999.92 L/m2 h bar. Table
4.1 show the result from nanofiber membrane that has been soaked to several different
concentration of BMIM-Chlorine.

Table 4.3 The result of permeability

Concentration Average volume collected per Permeability L/m2

Membrane 10 minutes h bar
1% 75 8333.33
2% 50 5555.55
3% 25 2777.77
4% 55 6111.11
5% 155 17222.22

Despite the result of permeability has shown bad trending, second round of
testing will be done in order to details more during the experiment done.

4.3 Field Emission Scanning Electron Microscope (FESEM)

To be able to observe the membrane at microscopic level, FESEM is used to

observe the topography of the membrane & detect any reaction occur to the membrane
during soaking process using BMIM-Chloride.

Figure 4.1: The FESEM of polymeric nanofiber membrane at 10000x magnification,

with a, b , c, d as in 1 % ,2 %, 3%, & 4% concentration respectively.

20
 Figure 4.1 shows the picture of nanofiber polymer membrane with 1 % to 4 %
with 10000x magnification. Figure 4.1 shows a webbing pattern that exist in between
the nanofiber membrane thread which shows the ionic liquid trapped inside the pores
of nanofiber membrane.

Figure 4. 1 show the BMIM-Chloride which shown the increase in numbers of

web pattern in (a) to (d). The thread also shown to be in nano-meter size. Hence, to be
known that visually, BMIM-Chloride did not affect the membrane nano thread size.

21
 CHAPTER 5

CONCLUSION & RECCOMENDATION

Current result and discussion shows the nylon 6, 6 nanofiber membrane of 0

wt% with over 100% porosity. The electrospin method has proved its efficiency to
fabricate a good quality of membrane. FESEM will be conducted on the membrane for
nanofiber diameter and geometry. For the soaking method, this is provide an ideal
environment for the ionic liquid to fill into the membrane pore, and expected to yield
a good data. Further data will be updated for concrete conclusion.

Permeability gain with current nylon 6, 6 nanofiber yield high result. The
membranes with additive expected to yield a better permeability. Further research
experiment will be conducted to conclude the effect of BMIM-Cl presence in the nylon
6, 6 with range of concentrations.

22
 REFERENCES

Cao, J., Cheng, Z., Kang, L., Chu, M., Wu, D., Li, M., Wen, R. (2017). Novel stellate
poly(vinylidene fluoride)/polyethersulfone microsphere-nanofiber
electrospun membrane with special wettability for oil/water separation.
Materials Letters. https://doi.org/10.1016/j.matlet.2017.07.044
Dai, X., Cao, Y., Shi, X., & Wang, X. (2016). The PLA/ZIF-8 Nanocomposite
Membranes: The Diameter and Surface Roughness Adjustment by ZIF-8
Nanoparticles, High Wettability, Improved Mechanical Property, and Efficient
Oil/Water Separation. Wiley Online Library, 1–6.
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 APPENDICES

1. Gantt Chart
a) FYP 1
No Week 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Task
1 FYP title selection
2 Preliminary Research
Work
 Background
Studies
 Objectives and
Scope of
research.
 Literature
Review
 Methodology
3 Extended Proposal
Submission
4 Laboratory Work
Research

5 Proposal Defend
6 Interim Report
Submission ( Draft)
7 Interim Report
Submission ( Final)

24
 b) FYP 2
No Week 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Task
1 FYP 2 Work Planning
2 Research Work
 Testing the
membrane
 FESEM &
FTIR Analysis

3 Progress Report
Submission
4 Laboratory Work
Research

5 Pre SEDEX
6 Final Report
Submission ( Draft)
7 Dissertation
Submission (Soft
Bound)
8 Technical Paper
Submission
9 Viva
10 Submission of Project
Dissertation (Hard
bound)

25
2. FESEM
a) 1 %

26
27
28
b) 2 %

29
30
c) 3 %

31
32
d) 4 %

33
34