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Materials Today: Proceedings 13 (2019) 154–159 www.materialstoday.com/proceedings

ICAMST 2018

The Synthesis of Fiber Membranes from High-Impact Polystyrene

(HIPS) Waste using Needleless Electrospinning as Air Filtration
Media
Akmal Zulfia,b, Dian Ahmad Hapidina,b, Casmika Saputraa,b, Widya Sinta Mustikaa,b,
Muhammad Miftahul Munira,b,*, and Khairurrijal Khairurrijala,b,*
a
Department of Physics, Faculty of Mathematics and Natural Sciences, Institut Teknologi Bandung, Jalan Ganesa 10, Bandung 40132, Indonesia
b
Research Center of Bioscience and Biotechnology, Institut Teknologi Bandung, Jalan Ganesa 10, Bandung 40132, Indonesia

Abstract

The production and characterization of air filter membranes from HIPS waste are presented. The HIPS membranes were
synthesized using needleless electrospinning. The HIPS precursor solutions were made by dissolving the HIPS waste in the d-
limonene:DMF solvent mixing ratio of 3:1, 1:1, and 1:3. The different mixing ratio led to different viscosity, surface tension, and
fiber morphology. Beaded to fine fiber morphology were obtained by increasing the DMF concentration in the mixing solvent.
The filtration test using PM2.5 as test particles demonstrated the good performance of the HIPS membrane as an air filter media
(filtration efficiency up to 98.75%).
© 2019 Elsevier Ltd. All rights reserved.
Peer-review under responsibility of the scientific committee of The 6th International Conference on Advanced Materials Science
and Technology 2018, 6th ICAMST.

Keywords: fiber membrane; needleless electrospinning; air filter; hips waste; nanofiber

1. Introduction

High-impact polystyrene (HIPS) is a graft copolymer containing a small amount of butadiene rubber in the
polystyrene (PS) matrix [1]. HIPS has good mechanical performances (resistance to impact, high thermal stability,

*
Corresponding author: Tel.: +62-22-250 0834; fax: +62-22-250 6452.
E-mail address: krijal@fi.itb.ac.id (Khairurrijal Khairurrijal)

2214-7853© 2019 Elsevier Ltd. All rights reserved.

Peer-review under responsibility of the scientific committee of The 6th International Conference on Advanced Materials Science and Technology
2018, 6th ICAMST.
 Zulfi et al./ Materials Today: Proceedings 13 (2019) 154–159 155

and good flexibility), yet easy to process and low cost [2-3]. The material is widely used in electronic devices,
household appliances, and toys. The Food and Drug Administration (FDA) also approved the utilization of the
material for food packages [2–4]. The extensive uses of HIPS in many areas lead to the increase of its waste.
Moreover, the waste of electrical and electronic equipment (WEEE) is dominated by HIPS-based waste, which
makes the recycling process to this material is necessary [5].
Zulfi et al. [5] have done HIPS waste recycling process by applying an electrospinning technique to convert the
bulk HIPS waste into fine nanofiber for air filter media. The air filter media from HIPS waste has a good filtration
performance compared to commercial filter or filter made from a pure polymer material [4-5]. However, the
conventional electrospinning technique has a limitation on their production rate (usually below 0.3 g/h) [6], which
make the scale-up production difficult. Some researchers have improved the production rate of the conventional
needle-based electrospinning by applying a needleless electrospinning technique [7]. The needleless electrospinning
replaces the needle with a special spinneret, such as wire [8-9], disk [10-11], drum [12], and spherical spinneret
[13], to allow high production rate.
Therefore, we utilized the needleless electrospinning technique to increase the production rate of air filter
membrane from HIPS waste. The high recycling process can be an alternative way to reduce the HIPS waste
abundance. Some characterizations were conducted to the membranes: optical microscopy to observe fiber diameter
and morphology; fourier transforms infrared (FTIR) spectroscopy to identify the remaining solvent in the
membranes; filtration test to determine filtration efficiency and pressure drop. The membranes filtration efficiency
was evaluated using PM2.5 as a test particle from burning incense smoke. The effect of the fiber diameter to the
filtration performance was also studied.

2. Materials and methods

2.1. Precursor solutions

HIPS waste, which was collected from compact disk cover, was cleaned and cut into pieces. Then, the pieces
were dissolved in a solvent mixture of d-limonene (purchased from a local chemical supplier) and N,N
dimethylformamide (DMF) (purchased from Sigma Aldrich, Indonesia) to make the precursor solution. The
precursor solutions were made with a varied d-limonene:DMF solvent mixing ratio of 3:1, 1:1, and 1:3 for the same
concentration of 20 wt.%.

2.2. Synthesis of HIPS fiber membranes

HIPS fiber membranes were fabricated by needleless electrospinning apparatus (Nachtrieb, 620) as shown in
Fig.1(a). The complete design of the apparatus is explained in [8]. The apparatus consisted of a negative and
positive high voltage power supply (+HV and –HV), wire spinneret, solution feeder, rotating drum collector, and
camera. The precursor solution was put in a syringe, and it was ejected to the solution feeder by a syringe pump with
the flow rate of 5 mL/h. The solution feeder transferred the precursor solution to the wire spinneret. The solution
feeder has the mechanical gear to move along the wire axis so that the precursor solution can be evenly distributed
along the wire spinneret. This mechanism improved the membrane thickness homogeneity on the collector.

Fig.1. (a) Needleless electrospinning apparatus; (b) the jet formation on the wire spinneret; (c) fibers collected on the drum collector.
156 Zulfi et al./ Materials Today: Proceedings 13 (2019) 154–159

A nonwoven substrate wrapped the drum collector. The drum was connected to the negative power supply (-HV),
while the wire spinneret to the positive power supply (+HV). The applied voltage to the spinneret and the drum
collector were 15 and -10 kV, respectively. The distance between the wire spinneret and the drum collector was 15
cm. The charged solution on the spinneret will experience an electrostatic force due to an electric field generated by
both power supply. The force leads to the formation of jets along the wire as can be seen in Fig.1. (b) (captured by
the camera). Tens of jets can be generated that increase the membrane production rate simultaneously. The collected
fibers on the drum collector (see Fig.1(c)) form a membrane that will be used as the filter media. All membrane
samples were fabricated at the same spinning time of 30 minutes in 50 % relative humidity.

2.3. Characterizations of HIPS fiber membranes

The HIPS fiber morphology was observed by an optical microscope (National, DC3-163). The captured image
from the microscope was analyzed to determine the fiber size uniformity from their size distribution curve. The size
uniformity of the fibers can be determined by calculating the coefficient of variation (CV) [5,14].The fabricated
membranes were also analyzed by Fourier-transform infrared (FTIR) spectrometer (Bruker, Alpha) to determine the
remaining solvent in the membranes after the spinning process. The FTIR spectra were recorded using the
wavelength range of 500-3000 cm-1.

2.4. Filtration performance test

The filtration performance of the fabricated membranes was tested by the apparatus as shown in Fig. 2. The
apparatus measured the membrane filtration efficiency and pressure drop. The membrane under test was placed
inside an impermeable filter holder. The differential pressure sensor, attached on both side of the filter holder,
measured the membrane pressure drop (∆P) at a given flow rate. The test particle for efficiency measurement used
incense burning smoke. The incense smoke is a good representation of PM2.5 source, a common harmful pollutant
size category [15]. Most filters, especially pollution filter, are designed to capture the airborne particles in PM2.5
category efficiently.

Fig.2. Filtration performance test apparatus.

In Fig. 2, the inlet and the outlet air flow rate were supplied by pumps. A buffer, dryer, pressure regulator, and a
high-efficiency particulate arresting (HEPA) filter were added to the air inlet port to provide clean, dry, and stable
air flow inside the apparatus. A rotameter controls the air flow to a chamber (Q1) where the incense was burned.
The incense smoke inside the chamber was delivered to the filter holder by a small pump with the air flow rate of
Q4. The dilute air flow (Q2), which was controlled by a mass flow controller (MFC1, Horriba Stec-SEC500), was
used to adjust the particle concentration. To measure filtration efficiency, the particle concentration before and after
 Zulfi et al./ Materials Today: Proceedings 13 (2019) 154–159 157

filtration were simultaneously measured by two condensation particle counters (CPC 1, TSI-3025A; and CPC 2,
TSI-3772). A mass flow controller (MFC 2, Horriba Stec-SEC400) was used to control the air flow rate through the
tested membranes as well as the face velocity (= air flow rate/membrane area). During the filtration efficiency
measurement, the face velocity was set constant of 5.3 cm/s.

3. Result and discussions

3.1. Fiber morphology

Fig. 3 shows the microscope images and size distribution of the HIPS fiber for different d-limonene:DMF ratio of
3:1 (sample a, Fig. 3(a)), 1:1 (sample b, Fig. 3(b)), and 1:3 (sample c, Fig. 3(c)). The microscope images depicted
the different morphology of the fabricated fiber for different solvents mixing ratio. As seen in Fig. 3(a), the solvent
mixing ratio of 3:1 resulted in beaded fiber morphology with the mean fiber diameter of 1.44 µm. When the DMF
content is decreased in the solvent mixing ratio of 1:1, the beads were not formed that resulted in pure fiber
membrane with the fiber diameter of 1.93 µm. Lastly, the mixing ratio of 1:3 resulted in pure fiber with the larger
fiber diameter of 4.96 µm.
The fiber diameter was increased when the DMF content in the solvent mixture was increased. Considering the
CV values, membrane sample a and b have uniform fiber diameter, while membrane sample c has nonuniform fiber
diameter. This result indicated a strong influence of solution characteristics to the fiber morphology and size.
Previously, for the same precursor concentration, the increase of DMF content in the d-limonene:DMF mixtures was
reported to increase the viscosity and decrease the surface tension of the HIPS precursor solution [4-5]. The
precursor solution with low viscosity and high surface tension will likely form a beaded fiber. This is because the
attractive force among polymer chain is weak so it cannot counterbalance the surface tension, which tends to make a
sphere-shaped form for decreasing the surface area [5,16].
In contrast, the increase in viscosity and the decrease in surface tension resulted in the increase of attractive force
among the polymer chain so that the jet stretching can be maintained, which resulted in pure fiber formation. The
increase in solution viscosity also affected the fiber diameter. Higher viscosity tends to produce larger fiber because
it needs longer time for the complete elongation [5,17]. In other words, the fibers may arrive on the collector before
the complete elongation that resulted in large fiber formation.

Fig. 3. The microscope image and the size distribution of HIPS fibers for (a) membrane sample a; (b) membrane sample b; and (c) membrane
sample c.
158 Zulfi et al./ Materials Today: Proceedings 13 (2019) 154–159

3.2. FTIR spectra

Fig. 4. shows the FTIR spectra of the membrane sample a, membrane sample b, membrane sample c, and the
cleaned waste HIPS. From Fig. 4, there was no significant peak difference between the three samples to the original
waste HIPS. There were six dominant peaks appeared on the spectra that correlated to HIPS material. The peaks at
the wavenumber of 694 cm‒1 and 793 cm‒1 were related to the C‒H out-of-plane bending vibration of the benzene
ring [18]. The peak at the wavenumber of 1492 cm‒1 was correlated to an in-plane phenyl ring deformation mode in
PS [19-20]. The peak at the wavenumber of 1600 cm‒1 was related to the backbone (C=C) stretching vibrations of
the benzene ring [18-21]. Then, the peaks at the wavenumber of 2849 cm‒1 and 2921 cm‒1 were related to the
asymmetric and symmetric stretching vibrations of CH2 [18].

Fig. 4. The FTIR spectra of membrane samples and cleaned waste HIPS sample.

The d-limonene has the peaks at the wavenumber of ~1100, ~1700, ~2900, and ~3400 cm‒1[22], while the DMF
at the wavenumber of ~1096, ~1256, ~1389, and ~1673 cm‒1 [23]. Based on Fig. 4, no solvent peaks appeared on the
FTIR spectra of the fabricated membrane samples. This indicated the solvents were completely evaporated during
the needleless electrospinning process.

3.3. Filtration performance

Fig. 5. (a) The pressure drop of the membrane samples and the non-woven substrate; (b) the filtration efficiency of the membrane samples and
substrate using PM2.5 as a test particle.
 Zulfi et al./ Materials Today: Proceedings 13 (2019) 154–159 159

Fig. 5. shows the pressure drop of the fabricated membranes (membrane sample a, b, and c) and a non-woven
substrate. Membrane sample c has the lowest pressure drop (closest to the substrate pressure drop), then followed by
membrane sample b and membrane sample c at the highest pressure drop. This indicated that the fiber size affected
the membrane pressure drop. Smaller fiber size could result in smaller pore size of the membrane which obstructed
the air to flow through the membrane [24-25].

4. Conclusion

Air filter membrane has been made from waste HIPS using needleless electrospinning method. The method can
fabricate the HIPS fiber with controllable morphology (beaded or pure) and size by adjusting the solvent mixing
ratio of d-limonene:DMF. The fiber diameter increased as the increase of the DMF in the mixing solvent. The
solvent mixing ratio (d-limonene:DMF) of 3:1, 1:1, and 1:3, resulted in the fiber mean size of 1.44, 1.93, and 4.96
µm, respectively. The FTIR spectra depicted complete evaporation of the solvent during the needleless
electrospinning process. The filtration performance test depicted the membrane with the solvent mixing ratio of 3:1
has the highest efficiency of 98.75%, whereas the membrane with the solvent mixing ratio of 1:3 has the lowest
pressure drop.

Acknowledgments

This research was financially supported by the Ministry of Research, Technology, and Higher Education, the
Republic of Indonesia under the University’s Excellence Research (PUPT) Grant and the PMDSU scholarship of A.
Z and D. A. H the fiscal year 2018.

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