Bioresource Technology Reports 25 (2024) 101728

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Bioresource Technology Reports

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Fabrication of composite membrane with microcrystalline cellulose from

lignocellulosic biomass as filler on cellulose acetate based membrane for
water containing methylene blue treatment
Romario Abdullah a, Dinia Astira a, Utari Zulfiani a, Alvin Rahmad Widyanto a, d,
Alvin Romadhoni Putra Hidayat a, Dety Oktavia Sulistiono a, c, Zeni Rahmawati a,
Triyanda Gunawan a, Yuly Kusumawati a, Mohd Hafiz Dzarfan Othman b, Hamzah Fansuri a, *
a
Department of Chemistry, Faculty of Science and Data Analytics, Institut Teknologi Sepuluh Nopember, Sukolilo, Surabaya 60111, Indonesia
b
Advanced Membrane Technology Research Centre (AMTEC), Universiti Teknologi Malaysia, 81310 Skudai, Johor Bahru, Malaysia
c
Automotive Engineering, Engineering Department, Politeknik Negeri Jember, Jember 68101, Indonesia
d
Department of Applied Chemistry, Shibaura Institute of Technology, 3-7-5 Toyosu, Koto-ku, Tokyo, 135-8548, Japan

A R T I C L E I N F O A B S T R A C T

Keywords: A composite membrane based on cellulose acetate polymer with microcrystalline cellulose (MCC) based filler
Composite membrane from lignocellulosic biomass is one of the right solutions to reduce methylene blue (MB) levels in water. MCC has
Microcrystalline cellulose been successfully isolated from water hyacinth, sengon wood, and kapok fiber with an alkalization method. The
Lignocellulosic
three MCCs have shown X-ray and FTIR diffraction patterns with characteristic peaks from cellulose and are
Wastewater treatment
Clean water and sanitation
stable up to 317 ◦ C. Cellulose acetate (CA)/MCC membranes have been prepared using the phase inversion
method and characterized by FTIR, tensile strength, contact angle, SEM, and porosity. The characterization
results show that the addition of MCC can increase the tensile strength (3.05 N⋅mm-2), hydrophilicity (52◦ ), and
porosity (88 %). The CA/MCC membrane performed better than the neat membrane in separating MB. The
composite membrane with MCC from kapok fiber showed optimum performance with increased flux and MB
rejection up to 84 L⋅m− 2⋅h− 1 and 99 %, respectively.

1. Introduction 2021) and electrocoagulation (Suryanto et al., 2023) have been

The United Nations World Water Development in 2021 reported that,
on a global scale, up to 80 % of industrial effluent is discharged into the
environment without being treated first (Lin et al., 2022). Industrial
wastewater generally contains compounds classified as toxic and haz­
ardous materials, which include organic compound pollutants (70 %)
and inorganic elements/compounds (30 %) such as heavy metals, ni­
trogen, and other toxic compounds that are harmful to living organisms
and the environment (Chan and Wu, 2022). One type of organic
pollutant in primary industrial wastewater is dye. Methylene blue (MB)
is a widely used pigment in the textile industry (Oladoye et al., 2022).
The presence of MB in wastewater can lead to human health issues and
environmental pollution (He et al., 2022b). Consequently, a few stra­
tegies have been developed to combat it.
Membrane filtration (Tang et al., 2022), coagulation (Ayat et al.,
2022), flocculation (Teixeira et al., 2022), adsorption (Santoso et al.,
employed to remove MB from industrial waste. Filtration with a mem­
brane is the most effective method for reducing the concentration of
dyes for the following reasons: the configuration of a filtration system
with a membrane is relatively simple, the energy required/consumed is
low, and it has a high selectivity for dye separation. In addition, mem­
brane filtration is also considered better than other methods that have
been reported, especially in terms of ease of synthesis and use (Hube
et al., 2020). Based on the constituent materials, filtration membranes
are divided into inorganic and organic (polymer) membranes (Maroufi
and Hajilary, 2023). Inorganic membranes provide a structurally robust
and thermally resistant material (Chen et al., 2017; Goh and Ismail,
2018; Zhang et al., 2018). Nevertheless, the low permeability of inor­
ganic membranes makes them less appropriate for wastewater treat­
ment. Furthermore, the production of inorganic membranes necessitates
exceedingly high temperatures, resulting in their relatively high cost.
Polymer membranes are favored for their pliability, elevated

* Corresponding author.
E-mail address: h.fansuri@chem.its.ac.id (H. Fansuri).

https://doi.org/10.1016/j.biteb.2023.101728
Received 13 September 2023; Received in revised form 29 November 2023; Accepted 3 December 2023
Available online 5 December 2023
2589-014X/© 2023 Elsevier Ltd. All rights reserved.
R. Abdullah et al.
permeability, economical nature, and straightforwardness in fabrication
and implementation (Divya and Oh, 2022).
Several polymers have been developed in membrane technology,
including cellulose acetate (Abdelhameed et al., 2021), polyvinyl
alcohol (PVA) (Mehdipour Ghazi and Bagherian, 2022), polyether sul­
fone (PES) (Giwa and Hasan, 2020), polyvinylidene fluoride (PVDF)
(Darmayanti et al., 2023; Widiastuti et al., 2022; Zhu et al., 2023), high-
density polyethylene (HDPE) (Zulfiani et al., 2023), and polyamides
(Huang et al., 2021). In the wastewater treatment process, cellulose
acetate is a very suitable polymer for use as a membrane-building ma­
terial because it is biodegradable, has good chemical stability, and is
more hydrophilic than other polymeric materials (Vatanpour et al.,
2022a). Tahazadeh et al. (2021) reported that using a cellulose acetate
membrane could increase water flux and filter MB by up to 98.2 %.
Nonetheless, cellulose acetate polymer membranes are notoriously
weak. To address this issue, numerous composite membranes with
enhanced characteristics and efficacy of polymer membranes have been
developed. It has been demonstrated that adding fillers to the polymer
matrix enhances the strength and hydrophilicity of the membrane and
decreases the fouling rate (Zambare et al., 2017).
Various inorganic materials, such as Fe3O4 (Tran et al., 2021), TiO2
(Zhafiri et al., 2023), ZIF-8 (He et al., 2022a, 2022b), ZnO (Abu-Dalo
et al., 2021), and Al2O3 (Yan et al., 2023), have been employed as fillers
in composite membranes developed for MB separation. Nevertheless,
there is concern that the utilization of metal or metal oxide-based fillers
might give rise to additional issues when leaching takes place during the
filtration process (Kajau et al., 2021). An approach to address this issue
involves the design of filler materials that possess minimal toxicity, are
biocompatible, and are environmentally sustainable (Trache et al.,
2016). Cellulose-based fillers, notably microcrystalline cellulose (MCC),
are among the materials that can be produced. MCC is a natural polymer
with the molecular formula (C6H10O5)x obtained from the depolymer­
ization of cellulose. MCC generally has a linear structure with an
arrangement of β-D-glucopyranose units connected by (1,4)-glycoside
bonds. As a filler in membranes, MCC can increase the strength, hy­
drophilicity, and performance of the membrane, including its flux and
rejection of pollutants. In their study, Pramono et al. (2022) found that
incorporating 1 % MCC into the PVDF membrane resulted in a signifi­
cant improvement in water flux, increasing it from 16.76 L⋅m− 2⋅h− 1 to
around 27 L⋅m− 2⋅h− 1. Additionally, this modification enabled the
membrane to effectively reject humic acid, with a rejection rate of up to
99 %. These findings agree with the studies of Nazri et al. (2021), who
reported the performance of a composite membrane made of PES with
commercial MCC filler. This membrane was able to enhance water flux
by up to 115.67 LMH and achieve a maximum rejection of 97.16 %. In
addition to enhancing performance, incorporating MCC as a filler in the
polymer matrix can also lower the fabrication expenses of composite
membranes and enable the development of eco-friendly membrane
materials by utilizing natural cellulose fibers or other lignocellulosic
biomass (Vatanpour et al., 2022b).
Currently, cellulose is recognized as the most abundant biopolymer
in nature (Dufresne, 2020), with annual production ranging from 1.0 ×
1011 to 1.0 × 1012 tons (Suryanto et al., 2023). The natural profusion of
cellulose makes it a renewable material that ensures the availability of
raw materials without reliance on fossil fuels. However, compared to
commercial cellulose, the utilization of natural cellulose remains insig­
nificant (Fan et al., 2010). Several lignocellulosic biomasses that have
been studied previously as sources of MCC are water hyacinth (Semachai
et al., 2018), sengon wood (Trisant et al., 2020), cotton fiber (Yulina
et al., 2020), corncob (Singh et al., 2020), bagasse (Katakojwala and
Mohan, 2020), rice husk (Bhandari et al., 2020), and cotton waste (Yuen
et al., 2021). Among these sources, water hyacinth (Eichhornia crassipes),
sengon wood (Albizia chinensis), and kapok (Ceiba pentandra) fiber are
suitable natural fibers for use as MCC sources due to their high cellulose
and low lignin content (Pratama et al., 2020; Sartika et al., 2019;
2
Bioresource Technology Reports 25 (2024) 101728
Trisanti et al., 2021). Trache et al. (2016) reported that each type of
lignocellulosic source has different characteristics that affect the char­
acteristics of the MCC obtained. Therefore, this research focuses on
exploring lignocellulosic biomass as the best source to produce MCC
with good characteristics as a filler for cellulose acetate membranes to
make composite membranes with high hydrophilicity, tensile strength,
and water flux, as well as high performance for MB removal in pro­
cessing wastewater. Economic analysis was also studied in this research
to obtain information on the production costs of MCC insulation from
lignocellulosic biomass and the manufacture of composite membranes
with MCC filler from biomass.
2. Experimental
2.1. Materials
The materials used in this study were water hyacinth (Eichhornia
crassipes), sengon wood (Albizia chinensis), and kapok fiber (Ceiba pen­
tandra), MCC Avicel PH 10, toluene (C7H8, 99 %, Smartlab), ethanol
(C2H5OH, 96 %, Smartlab), sodium hydroxide (NaOH, 99 %, Merck),
hydrogen peroxide (H2O2, 30 %, Merck), hydrochloric acid (HCl, 37 %,
Smartlab), cellulose acetate ((C6H7O2(CH3COO)3)x, 99 %, Sigma-
Aldrich), dimethylformamide ((CH3)2NCH, 99.5 %, Merck), and meth­
ylene blue (C16H18ClN3S, 99.99 %, Merck).
2.2. Isolation of microcrystalline cellulose from biomass
The cellulose isolation step was carried out according to the pro­
cedure reported by Holilah et al. (2021). The first stage is to prepare
each biomass, including water hyacinth (WH), sengon wood (SW), and
kapok fiber (KF). Biomass dried in the sun for ±2 days. Then the fiber is
crushed and sieved to get fine fiber. In the second stage, biomass fibers
were extracted using a Soxhlet apparatus with 450 mL of toluene-
ethanol (2:1) solvent for 6 h at 80 ◦ C to remove wax compounds from
the three biomasses. Then the raffinate was dried for 16 h in an oven to
remove the solvent. Next, the fibers were washed with 400 mL of aqua
DM and stirred vigorously for 30 min. Then, the fiber is filtered using
filter paper. In the third stage, the alkalinization process was done by
dissolving the dewaxed fiber in 5 % NaOH (1:20) and stirring at 90 ◦ C for
2 h. The fiber was then filtered and neutralized using aqua DM. In the
fourth stage, the three alkalized fibers were dissolved in a mixture of 5 %
NaOH and 3 % H2O2 (1:1) with a solid/liquid ratio of 1:40, stirred for 90
min at 55 ◦ C, and filtered. The process was repeated two times to obtain
minimal cellulose in lignin. The bleached cellulose fibers were then
neutralized using aqua DM and dried in an oven at 50 ◦ C for 6 h. The
final stage is the hydrolysis process to convert cellulose into micro­
crystalline cellulose. The bleached cellulose was hydrolyzed with 3.5 N
HCl solution at a ratio of 1:20 (w/v) and stirred for 90 min at 70 ◦ C,
filtered, and neutralized with aqua DM. The resulting MCC was then
dried at 60 ◦ C for 24 h. The synthesized dry MCC is used as a filler to
manufacture composite membranes. In summary, the MCC synthesis
process from biomass is presented in Fig. 1. The yield of cellulose ob­
tained after bleaching is calculated using Eq. (1), and the MCC yield
after the hydrolysis process is calculated using Eq. (2).
w1
Yield of cellulose (%) = × 100% (1)
w2
where w1 is the mass of cellulose obtained after the bleaching process
and w2 is the initial mass of WH, SW, and KF.
w1
Yield of MCC (%) = × 100% (2)
w2
where w1 is the mass of MCC obtained after and w2 is the mass of cel­
lulose obtained before the hydrolysis process.
R. Abdullah et al. Bioresource Technology Reports 25 (2024) 101728

Fig. 1. Isolation process of microcrystalline cellulose from biomass.

2.3. Synthesis of CA-MCC composite membrane 2.4. Characterizations

Synthesis of composite membranes begins by weighing each isolated
MCC with a weight percent of 0.5, 1.0, and 1.5 % by weight of cellulose
acetate. The MCC was subsequently dispersed in dimethylformamide
(DMF) using ultrasonication for a duration of 30 min. This process aimed
to disintegrate the MCC aggregates and achieve a uniform distribution of
MCC in the suspension. After 30 min, the cellulose acetate polymer with
the optimum concentration obtained from the previous step was added
to the suspension. The mixture was stirred at 80 ◦ C for 24 h, so the
cellulose acetate powder was wholly dissolved in the DMF. The prepared
dope solution was subsequently allowed to stand for 12 h in order to
eliminate any air bubbles. In the final stage, the membrane is printed
following the procedure described in the previous stage. Membranes
with MCC from water hyacinth, sengon wood, and kapok fiber were each
coded with CA-MCC_WH, CA-MCC_SW, and CA-MCC_KF, as shown in
Table 1. In summary, the manufacture of composite membranes in this
study is presented in Fig. 2.
2.4.1. X-ray diffraction (XRD)
XRD characterization was carried out to determine microcrystalline
cellulose’s structure and crystalline phases by an X-ray Diffraction
Phillips XPert MPD Diffractometer. The XRD instrument used is an
X’Pert PANalytical with Cu Kα source (λ = 1.5406 Å). Measurements
were made at 2θ between 5 and 50◦ with a step size of 0.01◦ . The
crystallinity index (CrI) of MCC was calculated using Eq. (3).
I002 − Iam
CrI (%) = × 100% (3)
I002
I002 is the maximum crystalline intensity at 2θ = 22.50◦ and Iam is the
amorphous minimum intensity at 2θ = 18◦ .
2.4.2. Fourier transform infrared (FTIR)
FTIR characterization was carried out to determine the bonds and
functional groups present in microcrystalline cellulose and composite
membranes. FTIR spectra were observed at wave numbers from 500 to
4000 cm− 1 with Thermo Scientific Nicolet IS10.

2.4.3. Thermal gravimetric analysis (TGA)

Table 1 TGA characterization was carried out to determine the thermal sta­
Composition of cellulose acetate-MCC composite membrane. bility of microcrystalline cellulose using the PerkinElmer Pyris 1 TGA
MCC Membranes Concentration of MCC CA DMF Thermogravimetric Analyzer. Approximately 10 mg of the sample was
sources MCC (wt%) (g) (g) (g) placed in the sample holder, and then the sample was heated at
Water CA-MCC_WH 0.5 0.012 2.388 17.6 10 ◦ C⋅min− 1 from room temperature to 600 ◦ C.
hyacinth (0.5)
CA-MCC_WH 1.0 0.024 2.376 17.6 2.4.4. Scanning electron microscopy (SEM)
(1)
CA-MCC_WH 1.5 0.036 2.364 17.6
SEM characterization was carried out to determine the surface
(1.5) morphology of microcrystalline cellulose, composite membranes, cross-
Sengon CA-MCC_SW 0.5 0.012 2.388 17.6 sections of composite membranes, and their distribution and pore size
wood (0.5) using Hitachi Flex SEM100. The preparation was done by placing a small
CA-MCC_SW 1.0 0.024 2.376 17.6
sample coated with gold metal (Au) on copper tape, then placed on the
(1)
CA-MCC_SW 1.5 0.036 2.364 17.6 sample holder to be analyzed with an SEM instrument.
(1.5)
Kapok CA-MCC_KF 0.5 0.012 2.388 17.6 2.4.5. Water contact angle membrane test
fiber (0.5) Contact angle characterization was carried out to determine the
CA-MCC_KF 1.0 0.024 2.376 17.6
(1)
hydrophilicity of the cellulose acetate-MCC composite membrane using
CA-MCC_KF 1.5 0.036 2.364 17.6 3D OM vhx-500. The membrane was cut to a size of about 2 × 2 cm, then
(1.5) water was dripped on the surface of the membrane, and the contact

3
R. Abdullah et al.
Fig. 2. Composite membrane synthesis process.
angle formed was observed with a digital microscope.
2.4.6. Tensile strength membrane test
The tensile test was characterized to determine the tensile strength of
the cellulose acetate membrane against the tensile force using Gotech
Testing Machines AI-7000-LAU. In the testing process, both ends of the
specimen are clamped on the clamp with mechanical test equipment,
and then the tensile strength (N⋅mm− 2) is observed.
2.4.7. Membrane porosity test
The membrane porosity test determined the number of pores formed
on the cellulose acetate-MCC composite membrane. The method used in
this test is gravimetry. Tests were conducted by immersing a 50 cm2
membrane in aqua DM for 24 h at room temperature. The membrane
was then removed from the aqua DM, the dripping liquid was wiped
before being weighed, and the obtained weight was recorded as W1.
Next, the membranes were dried in an oven for 48 h at 40 ◦ C. The dry
membrane was then weighed again, and the weight obtained was
recorded as W2. The membrane porosity is then calculated by Eq. (4).
w − w2
ε= ( 1 ) × 100% (4)
ρw w1ρ− w2 + ρw2
w md
with: ε = Porosity (%), w1 = Mass of wet membrane (g), w2 = Mass of dry
membrane (g), ρw = Density of water (g⋅mL− 1), and ρmd = Density of
cellulose acetate (g⋅mL− 1).
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2.4.8. Composite membrane performance testing
The performance of the composite membrane was tested to evaluate
the permeability and rejection of the composite membrane to methylene
blue dye. The ultrafiltration test process is carried out on a laboratory
scale with a crossflow system, as shown in the scheme in Fig. 3. The
performance of the composite membrane was evaluated through an
analysis of water flux and its rejection of MB. The water flux obtained is
calculated by Eq. (5).
V
Jv = (5)
Axt
with: Jv = Flux (L⋅m− 2⋅h− 1), V = Permeate volume (L), A = Surface area
of the membrane (m2) and t = Time (hours).
The performance against MB dye rejection was evaluated using a
concentration of 5 mg⋅L− 1 of MB solution. The composite membrane
performed best and was used as the test medium, with a higher MB
concentration variation. The resulting permeate was analyzed for con­
centration with UV–Vis at a wavelength of 664 nm. Membrane rejection
ability is calculated by Eq. (6).
( )
Cf − Cp
R= × 100% (6)
Cf
with: R = Rejection percentage (%), Cf = Feed concentration (mg⋅L− 1),
and Cp = Permeate concentration (mg⋅L− 1).
R. Abdullah et al. Bioresource Technology Reports 25 (2024) 101728

Fig. 3. Membrane separation performance testing scheme.

3. Result and discussion
3.1. Isolation and characterization of MCC
The MCC isolation process using the alkalization method causes a
mass reduction in each of the WH, SW, and KF, as presented in Table 2.
The mass reduction in the dewaxing process shows that the wax content
in WH is greater than that in SW and KF. This is caused by the charac­
teristics of WH plants, which generally contain wax on the surface of
their stems and leaves to maintain the water content in them (Arivendan
et al., 2022). In addition, the reduction in mass after the delignification
and bleaching processes indicates a decrease in the content of lignin and
hemicellulose compounds caused by NaOH alkalization. Among the
three, cellulose from KF shows the highest yield, which is caused by the
high cellulose content in KF. However, the overall MCC yield from WH,
SW, and KF produced was 73.76 %, 89.46 %, and 91.21 %, respectively.
These results are higher than those of several previous studies regarding
MCC isolation, as reported by Bhandari et al. (2020) with an MCC yield
from rice husks of 25.05 %, Bhandari et al. (2022) with an MCC yield
from wood waste of 24.09 %, Kasim and Asben (2022) with an MCC
yield from empty palm fruit bunches of 31.22 %, and Shao et al. (2020)
with an MCC yield from corn cobs of 41.90 %.
XRD analysis was carried out to determine the nature of the MCC
crystals and observe whether other crystals were formed or remained
after the isolation process. Fig. 4a presents the diffractogram of cellulose
raw material, isolated MCC, and commercial MCC. The results indicate a
diffractogram difference between the raw material and the isolated
MCC. The presence of inappropriate peaks and low intensity on the raw
material diffractogram indicates that other substances besides cellulose
are contained therein. On the other hand, the isolated MCC diffracto­
gram has shown a typical MCC peak at 2θ = 15–16, 22.5, and 34.5◦
(Sainorudin et al., 2018) with crystallographic fields (110), (200), and
(040), respectively (Khenblouche et al., 2019). This is also supported by
the compatibility of the third MCC diffractogram with commercial MCC.
The three MCCs isolated from WH, SW, and KF showed a type I cellulose
polymorph structure (Lu et al., 2015) and did not form type II cellulose
polymorphs, as evidenced by the absence of double peaks at 2θ = 22.6◦
(Rosa et al., 2012). Type I cellulose polymorph is the original structure
of cellulose, which is more abundant than other cellulose polymorphs
and is found in plant cell walls. In this study, low concentrations of
NaOH were the reason for not forming type II cellulose because type II
cellulose can be obtained by using a high concentration of NaOH,
namely 18 % (He et al., 2021). Holilah et al. (2021) reported that an
increase in intensity at the peak of 22.6◦ is the primary indicator to
confirm the formation of MCC. This suggests that the MCC obtained
from the three lignocellulosic sources in this investigation has been
generated with an enhanced MCC intensity at peaks of 22.4 and 22.5◦ .
The XRD analysis revealed that the crystallinity index (CrI) of WH_MCC,
SW_MCC, and KF_MCC was 80.49 %, 79.67 %, and 67.81 % respectively.
The commercial MCC had a crystallinity index of 83.08 %. In this work,
the produced MCC exhibited high crystallinity, as indicated by Moha­
mad Haafiz et al. (2013), who defined MCC as having high crystallinity
when the CrI is between 55 % and 80 %. The CrI MCC results from each
biomass were higher than several previous studies, as reported by
Semachai et al. (2018) with CrI MCC from water hyacinth of 76.44 %,
Trisant et al. (2020) with CrI MCC from sengon wood of 75.98 %, and

Table 2
Mass balance in MCC isolation process.
MCC Initial Mass (g) Dewaxing Delignification Bleaching Hydrolysis Cellulose yield (%) MCC yield (%)

w (g)a wl (%)b w (g)a wl (%)b w (g)a wl (%)b w (g)a wl (%)b

WH 10 8.52 14.80 5.23 32.90 3.43 18.00 2.53 9.00 34.30 73.76
SW 10 9.28 7.20 5.46 38.20 4.27 11.90 3.82 4.50 42.70 89.46
KF 10 9.57 4.30 8.89 6.80 7.85 10.40 7.16 6.90 78.50 91.21
a
w = weight.
b
wl = weight loss.

5
R. Abdullah et al.
Fig. 4. a) X-ray diffractogram, b) FTIR spectra, and c) thermogram of isolated and commercial MCC.
Sartika et al. (2020) with CrI MCC from kapok fiber of 57.90 %.
FTIR analysis was conducted to identify the functional groups and
chemical bond interactions present in natural fibers and MCC, as well as
to assess any alterations in functional groups following the alkalization
of the raw materials. Fig. 4b shows the FTIR spectra of each raw mate­
rial, isolated MCC, and commercial MCC. The three absorption bands of
the raw materials indicate the presence of cellulose contained in WH,
SW, and KF, with absorption peaks at wave numbers 1029, 1315, 1428,
2895, and 3332 cm− 1. In addition, the appearance of solid absorption
peaks at wave numbers 1615 and 1732 cm− 1 indicates the occurrence of
stretching vibrations in the carbonyl group (C– –O), which proves the
presence of lignin and hemicellulose compounds, which are still present
in the three natural lignocellulosic fibers (Boukir et al., 2019; Cogulet
et al., 2016). When compared with the MCC FTIR spectra, the weakening
of the absorption peak at wave number 1615 cm− 1 on WH and the loss of
the absorption peak of 1732 cm− 1 on SW and KF indicate a reduction in
lignin compounds due to the alkalization process by 5 % NaOH. In
addition to the loss of the typical lignin absorption peaks, the success of
the MCC isolation process was also seen through its compatibility with
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Bioresource Technology Reports 25 (2024) 101728
commercial MCC FTIR spectra. The three isolated MCCs showed ab­
sorption peaks at wave number 1029 cm− 1, indicating asymmetric
C–O–C stretching vibrations in the pyranose ring units in the cellulose
structure (Jindal and Singh, 2016). In addition, the absorption peaks at
wave numbers 1315 and 1428 cm− 1 indicate CH2 bending vibrations
with the types of vibrations, namely wagging and scissoring, respec­
tively. The appearance of an absorption peak at wave number 2895
cm− 1 indicates the occurrence of symmetrical strain on the C–H bond.
The presence of hydroxyl groups (O–H) in the cellulose structure was
identified by the appearance of an absorption peak at wave number
3332 cm− 1. The hydroxyl group comes from the glucose structure,
which is the monomer that makes up the MCC structure. Therefore,
glucose was identified as a type of carbon source during the isolation
process of microcrystalline cellulose.
TGA analysis was conducted to assess the thermal stability of MCC
produced from the three biomasses and identify the presence of
decomposition processes at certain temperatures. The testing was con­
ducted at a 25–600 ◦ C with a heating rate of 10 ◦ C⋅min− 1 in the air. The
results of the TGA analysis of the three MCCs showed a similar
R. Abdullah et al.
decomposition pattern to commercial MCCs. The three MCCs show the
occurrence of three stages of decomposition, as shown in Fig. 4c. The
first decomposition occurs at 50–100 ◦ C, caused by removing physically
adsorbed water from the MCC. The second decomposition occurs at a
temperature range of 200–325 ◦ C, indicating cellulose degradation. The
final decomposition process occurs at a temperature of 325–500 ◦ C,
indicating an oxidation process in the carbon residue resulting from the
degradation of cellulose. The patterns are similar to a report by Holilah
et al. (2021). The three isolated MCCs showed different initial decom­
position temperatures. WH_MCC is a material with better thermal sta­
bility than the other two MCCs, even when it is compared to commercial
MCC. This is demonstrated by the fact that cellulose has a higher
decomposition temperature at WH_MCC, reaching up to 317 ◦ C. In
contrast, SW_MCC, KF_MCC, and C_MCC experienced cellulose degra­
dation at temperatures of 308, 313, and 313 ◦ C. On the other hand, the
MCCs synthesized in this work exhibited a characteristic breakdown
temperature of cellulose. Carrier et al. (2011) reported that cellulose
typically decomposes within the temperature range of 300 to 350 ◦ C.
SEM analysis was used to see the morphology of the isolated raw
materials and MCC, as shown in Fig. 5. These results provide informa­
tion about the morphological changes after the alkalinization process.
Before treatment, SEM images of water hyacinth fiber and sengon wood
showed a rough and aggregated surface. This indicates the presence of
hemicellulose and lignin in natural fibers, whereas kapok fibers clearly
show fibers in the form of fibers. The MCC synthesis results showed a
small and irregular structure and size of MCC. However, compared to
Fig. 5. Raw material morphology and MCC of (a, b) water hyacinth, (c, d) sengon wood and (e, f) kapok fiber.
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Bioresource Technology Reports 25 (2024) 101728
WH_MCC and SW_MCC, KF_MCC shows a longer and more stable
structure with finer fibers. The change in fiber size before and after
treatment was due to the hydrolysis process using acid, which had an
impact on breaking the β-1,4-glycosidic bond that connected the cellu­
lose chains (Zhao and Chung, 2018). The isolated MCCs showed cellu­
lose fibers with low lignin and hemicellulose. A comparison of fiber size
before and after treatment shows that the shape of the fiber gets smaller
after the alkaline treatment, bleaching, and hydrolysis using acid. Based
on the results of SEM analysis, the three MCCs obtained showed dif­
ferences in fiber diameter sizes. The size of the WH_MCC, SW_MCC, and
KF_MCC were up to 5.38, 7.01, and 7.82 μm, respectively, with average
diameters of 58.74, 38.31, and 14.44 μm. The sizes of the three MCCs are
similar to commercial MCC sizes, ranging from 13.33 to 166.67 μm
(Yugatama et al., 2012). Trache et al. (2014) and Adel and El-shinnawy
(2012) reported that the average diameter of commercial MCC is
generally higher than that obtained from the isolation of lignocellulosic
biomass.
3.2. Isolation and characterization of composite membranes
3.2.1. Functional group analysis of composite membranes
The FTIR spectra of the cellulose acetate (CA)-MCC composite
membrane, as depicted in Fig. 6, exhibit absorption peaks similar to
those observed in the cellulose acetate membrane. In other words, it can
be said that there are no new absorption peaks after adding MCC to the
cellulose acetate polymer matrix. This is influenced by functional
R. Abdullah et al.
Fig. 6. FTIR spectra of cellulose acetate membranes and composite membranes.
groups, which are found in cellulose acetate and are mostly the same as
those in MCC. Based on the chemical reaction, cellulose acetate is a
polymer that can be obtained from the acetylation of cellulose, where
the hydroxyl groups present in cellulose will be replaced by acetyl
groups so that they can form cellulose acetate polymers. This causes the
appearance of a peak in the CA absorption band with wave number
1737 cm− 1, which indicates the occurrence of symmetrical and asym­
metric stretching vibrations of the carbonyl group (C– –O) of the ester
group in the CA polymer (Cherifi et al., 2022). The same thing can be
seen in the absorption band of the composite membrane, but with
sharper peaks than in the absorption band of the CA membrane. In
addition, the entire FTIR spectra showed several absorption peaks
typical of cellulose, such as the appearance of a peak at wave number
901 cm− 1, indicating the presence of C–O vibrations in the 1,4-glyco­
side bonds that connect between cellulose monomer units (Jamil
et al., 2020). In addition, the appearance of an absorption peak at wave
number 1035 cm− 1 indicates the occurrence of asymmetric C–O–C
stretching vibrations in the pyronase ring unit, forming the cellulose
structure framework (Xu et al., 2020). The appearance of absorption
peaks at wave numbers 1367 and 1434 cm− 1 indicates CH2 bending
vibrations, one of the functional groups in the cellulose structure with
vibrational types, namely wagging and scissoring, respectively. The
presence of hydroxyl groups (O–H) in the structure of CA and MCC was
identified by the emergence of absorption peaks at wave numbers be­
tween 3401 and 3522 cm− 1 (Akturk, 2023; Kokot et al., 2002). The FTIR
analysis revealed a distinct disparity in the absorption peaks between
the CA membrane and the composite membrane. Specifically, all ab­
sorption peaks exhibited enhanced sharpness on the CA-MCC composite
membrane.
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3.2.2. Analysis of tensile strength, hydrophilicity, and porosity of
membrane composite
Tensile strength analysis was carried out to determine the strength of
the membrane before and after the addition of MCC to the CA matrix.
Fig. 7a shows the influence of the source and weight percent of MCC on
the membrane strength. The results of the tensile strength analysis
proved that adding MCC to the CA membrane increased the tensile
strength of the resulting membrane. This increase was due to the
excellent compatibility between CA and MCC, as well as the efficient
transfer of stress from the CA matrix to MCC, which increased the tensile
strength of the composite membrane, as explained by Yousefian and
Rodrigue (2016). The three types of composite membranes with
WH_MCC, SW_MCC, and KF_MCC fillers showed the same tendency to­
wards the optimum tensile strength at 1 % MCC addition. The tensile
strength is lower when 0.5 % MCC is added. It seems that the increase in
MCC addition will also increase the tensile strength of CA-MCC com­
posites. However, when the concentration of MCC was increased to 1.5
%, the tensile strength of the membrane decreased. This might be caused
by a lower dispersion of MCC in the CA polymer matrix that may trigger
MCC agglomeration, leading to a decrease in the membrane’s tensile
strength (Bai et al., 2012).
Contact angle analysis was carried out to determine the hydrophi­
licity of the membrane before and after the addition of MCC to the CA
matrix. The surface of the membrane, which has hydrophilic properties,
will trigger the formation of bonds between water molecules and the
molecules that make up the membrane (Yin and Zhang, 2021). Fig. 7b
shows the three composite membranes, with each MCC filler isolated
from WH, SW, and KF showing the same trend towards the membrane
contact angle. The addition of 1 % MCC produced the lowest contact
angle. Additionally, it demonstrates that the CA membrane containing 1
R. Abdullah et al.
Fig. 7. a) Tensile strength, b) contact angle, and c) porosity of cellulose acetate membrane and composite membrane.
% MCC exhibits greater hydrophilicity. As described by Salehian et al.
(2022), this hydrophilicity is inversely related to the contact angle. The
increase in hydrophilicity is influenced by the presence of the –OH
group in MCC, one of the functional groups that make up cellulose and
can form interactions with water molecules. These results are in line
with research reports by Pramono et al. (2022), who reported that the
addition of MCC to PVDF membranes also showed optimum hydrophi­
licity with a weight percent of 1 % MCC. A different thing was seen in the
membrane with a weight percentage of 1.5 %, where the addition of
excess MCC could increase the contact angle and reduce its hydrophi­
licity. This outcome is attributed to the elevated viscosity of the dope
solution due to the surplus MCC content. Bai et al. (2015) observed that
increased viscosity slows down the rate at which the solvent and non-
solvent interchange occurs during the phase inversion process. This
hinders the filler from quickly moving to the surface of the membrane.
The objective of the membrane porosity investigation was to eval­
uate the alterations induced by the incorporation of MCC into the CA
matrix. Fig. 7c presents the results of this porosity analysis, indicating
the impact of MCC concentration on the composite membrane. For both
WH_MCC and SW_MCC fillers, a 1 % MCC concentration yielded the
highest porosity. Pramono et al. (2022) have also reported that the
addition of 1 % MCC in the PVDF matrix was able to produce a higher
membrane porosity than 0.5 % MCC. However, a different trend was
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Bioresource Technology Reports 25 (2024) 101728
observed in the composite membrane synthesized with KF_MCC filler,
where a 0.5 % MCC concentration resulted in the highest porosity. The
addition of 1 % MCC in CA-MCC_WH and CA-MCC_SW significantly
improved the hydrophilicity of the membrane, which promoted a rapid
exchange of solvent and non-solvent during phase inversion, leading to
enhanced pore formation. These results are consistent with the findings
of Barzegar et al. (2020), which indicate that the incorporation of hy­
drophilic materials enhances both the hydrophilicity and porosity. In
addition to hydrophilicity, the porosity of a membrane can be affected
by the viscosity of the fluid used to create it. The incorporation of 1 %
MCC in CA-MCC_KF resulted in a membrane that exhibited enhanced
hydrophilicity, albeit with reduced porosity compared to the addition of
0.5 % MCC, which obtained a porosity of 85 %. The difference was
ascribed to the presence of excessive KF_MCC (1 and 1.5 %), which
caused an increase in the molecular weight of cellulose in the solution,
leading to a high viscosity. As a result, the rate at which the solvent and
non-solvent interchange occurred decreased during phase inversion,
which aligns with the findings of Tu et al. (2022). This suggests that
when the viscosity of the dope solution increases, the porosity of the
membrane reduces. Matveev et al. (2022) have also reported similar
findings.
R. Abdullah et al.
3.2.3. Composite membrane morphology analysis
The effect of adding MCC to the CA matrix on the changes in the
membrane’s surface morphology and pore structure is characterized by
SEM. Fig. 8 shows SEM images of the membrane surface, pore size, and
pore distribution. The figure shows that the pure CA membrane has a
smoother surface with a smaller pore size and is more evenly distributed
than the CA-MCC membranes. Differences in MCC sources affect the
pore structure on the surface of the membrane, where the composite
membrane synthesized with WH_MCC fillers shows a larger pore size
with more distribution. In contrast, the composite membrane with fillers
SW_ MCC and KF_MCC showed a surface pore structure with less pore
Fig. 8. Membrane Surface Morphology and Pore Size Distribution (a–c) CA, (d f) CA-MCC_WH(1), (g–i) CA-MCC_SW(1) and (j–l) CA-MCC_KF(0.5).
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distribution and a smaller size. The results of the analysis of the surface
morphology of the membrane with SEM were in line with the results of
membrane porosity, where the addition of MCC in the CA matrix was
able to influence the formation of the pore structure of the membrane to
produce a membrane with higher porosity. Overall, the synthesized
membrane shows an asymmetrical pore structure with differences in the
pore structure of the upper and lower parts of the membrane.
The cross-sectional section of the membrane was also analyzed using
SEM, as shown in Fig. 9. The figure shows that a finger-like pore
structure is visible at the top of the membrane, while at the bottom,
there is a sponge-like pore structure. In addition, the SEM analysis of the
R. Abdullah et al.
Fig. 9. Cross section morphology of membranes: (a–b) CA, (c–d) CA-MCC_WH
(1), (e–f) CA-MCC_SW(1) and (g–h) MCA-MCC_KF(0.5).
membrane cross-section also indicated that adding MCC to the CA
membrane affected the formation of cavities in the membrane pores.
The presence of MCC aggregation can affect the development of cavities
in the membrane. Specifically, a greater amount of agglomeration leads
to bigger cavity sizes (Wang et al., 2016).
3.2.4. Pure water flux analysis
The augmentation of water flux in the composite membrane exhibits
an inverse relationship with the reduction in contact angle and the
augmentation in porosity with the addition of MCC to the CA matrix
(Fig. 10). The decrease in the contact angle indicates the high hydro­
philicity of the composite membrane due to the presence of –OH groups
present in the MCC structure, which increases the interaction of the
membrane with water molecules through hydrogen bonds. Hydrogen
bonds are interactions between hydrogen atoms and elements with high
electronegativity, such as oxygen in water. In addition, the –OH group
in MCC also accelerates the exchange of DMF and water during the
phase inversion process, causing a higher porosity of composite mem­
branes with MCC compared to CA membranes without MCC. The high
porosity of the membrane is known to increase the diffusion rate of
water molecules during the filtration process. This aligns with research
by Wahab et al. (2019), who reported that an increase in membrane
porosity produced a higher water flux.
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Fig. 10. Pure water flux of composite membrane.
3.2.5. Membrane performance analysis on methylene blue separation
The enhancement in membrane performance in resisting methylene
blue (MB) dye was evaluated by comparing the results of water flux and
the membrane’s ability to reject MB molecules, as depicted in Fig. 11.
The water flux results in the MB separation process using the three types
of composite membranes exhibited a similar pattern to the pure water
flux test. Notably, the CA composite membrane with 1 % WH_MCC and
SW_MCC fillers demonstrated the highest water flux after the MB sep­
aration process, indicating optimal performance. The water flux test
results are in line with the reports of Nazri et al. (2021) and Pramono
et al. (2022), who reported that the addition of 1 % MCC to PES and
PVDF membranes was able to produce optimal water flux. In contrast,
the composite membrane with MCC_KR showed optimal water flux
when 0.5 % MCC was added. These results are affected by the lower
contact angle values and higher membrane porosity. Among the three,
CA-MCC_WH showed the most increased water flux compared to other
composite membranes, while CA-MCC_KF showed the lowest. The SEM
analysis supported these results, which showed a more significant dis­
tribution and pore size in the CA-MCC_WH membrane compared to the
CA-MCC_SW and CA-MCC_KF membranes. Compared with pure CA
membranes, the entire composite membrane produced a higher water
flux than the membrane without adding MCC. The increase in water flux
was due to the addition of MCC in the CA matrix, which was able to
increase the number of –OH groups on the surface and inside of the
membrane, increasing the interaction of hydrogen bonds between –OH
groups and water molecules (Zhang et al., 2020).
The results of the rejection of the MB molecule showed that the three
types of composite membranes that produced the optimum water flux
could only have a lower rejection percentage. The small pore size of CA-
MCC_KF(0.5) compared to CA-MCC_WH(1) and CA-MCC_SW(1) is the
cause of the high selectivity to MB. Furthermore, the larger and more
uniform size of the KF_MCC compared to WH_MCC and SW_MCC results
in a reduced amount of free space within the composite membrane. As a
result, the passage of MB molecules through the membrane becomes
more challenging. At a higher MCC concentration of 1.5 %, the three
composite membranes showed excellent rejection of up to ≥90 %. This is
because adding excess filler to the membrane matrix can cause
agglomeration, which triggers the closing of the membrane pores to
become smaller and denser (van den Berg and Ulbricht, 2020). Overall,
the three composite membranes have shown good separation perfor­
mance. This is because adding MCC can increase the –OH group on the
membrane, which causes the binding of MB molecules by the membrane
through the interaction of hydrogen bonds. On the other hand, the
R. Abdullah et al.
Fig. 11. Water flux and MB rejection of the composite membranes.
formation of aggregates of fellow MB molecules is also a possible cause
of the retention of MB by the composite membrane because the
appearance of aggregates causes the size of the MB molecule to become
more significant (Colomba et al., 2017).
3.2.6. Effect of MB concentration on membrane performance
Membrane configuration studies were conducted to examine the
effects of different concentrations of MB in the solution. This was done to
see the performance of the membrane at higher MB concentrations. The
CA-MCC_KR(0.5) membrane, which had an optimal performance on the
results of water flux and rejection of MB, was used as the test membrane
in the breakdown of MB with concentrations of 10 and 15 mg⋅L− 1.
Fig. 12 shows that the CA-MCC_KR(0.5) membrane has excellent per­
formance in finishing MB up to 15 mg⋅L− 1 with a rejection proportion of
92 %. In addition, experiments with various MB concentrations showed
a decreasing trend of water flux and MB rejection as the MB concen­
tration increased. The decrease in water flux is caused by the concen­
tration polarization phenomenon, where the higher the MB
Fig. 12. Flux and MB rejection with variation of MB concentration.
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concentration, the more MB molecules are present in the feed. It will
result in an increase in MB molecules or an increase in excess MB con­
centration on the membrane surface. Increasing the MB concentration
will cause a significant difference between the feed solution concen­
trations and the permeate. This difference in concentration makes it
difficult for water molecules to get to the permeate side, or it can be said
that there is a back-diffusion of water molecules to the feed side to form
an equilibrium (Ezugbe and Rathilal, 2020). This phenomenon is one of
the reasons for the decrease in water flux when the MB concentration
increases. In addition, an increase in the concentration of the bait also
influences the phenomenon of fouling.
The fouling phenomenon indicates that pore blockage by MB mole­
cules can occur during the filtration process. The pore blockage affects
the water flux, as Wei et al. (2013) reported that blockage of membrane
pores by pollutants can reduce the air flux resulting from the filtration
process. In addition, the decrease in membrane rejection of MB is caused
by the phenomenon of fouling through pore narrowing, which occurs
due to the larger pore size of the MB molecule. The pore-narrowing
process is caused by chemical interactions between the membrane and
the pollutant molecules to be separated. In this study, MB molecules
were known to be able to form interactions with –OH groups on the
membrane (Cheng et al., 2020), as presented in Fig. 13. An increase in
MB concentration accompanied by an increase in the number of MB
molecules in the feed solution will cause a high probability of MB
molecules escaping due to the limited –OH groups on the surface or in
the membrane. This is supported by the report of Goosen et al. (2009),
who explained that an increase in the number of pollutant molecules on
the surface of the membrane could form a layer that causes the closure of
the active part of the membrane, which can bind pollutants. In addition,
the decrease in membrane rejection of increasing MB concentrations
may also be due to a decrease in the dissolving capacity of the dye in
water, resulting in seepage of the insoluble dye onto the permeate side,
which causes absorption of the membrane retention of the MB dye. This
is also like the study reported by Parakala et al. (2019), who stated that
an increase in MB concentration was able to decrease membrane
rejection of MB dyes. Table 3 shows that the CA-MCC membrane syn­
thesized in this study has good performance compared to the cellulose
acetate-based composite membranes that have been developed
R. Abdullah et al. Bioresource Technology Reports 25 (2024) 101728

Fig. 13. Schematic of the interaction of the composite membrane with the MB molecule

Table 3
Comparison of cellulose acetate based membrane in dye processing.
Membrane Dyes pollutants Dyes concentration (mg⋅L− 1) Membrane performance Reference
− 2 − 1
CA-MCC Methylene Blue 5 Flux = 84 L⋅m ⋅h , Rejection = 99 % This work
2 1
10 Flux = 60 L⋅m− ⋅h− , Rejection = 96 %
2 1
15 Flux = 48 L⋅m− ⋅h− , Rejection = 92 %
CA/NAC Methylene Blue 10 Rejection = 53 % (Koriem et al., 2022)
CA/p-MWCNTs Methylene Blue 10 Rejection = 40 % (Silva et al., 2020)
2 − 1
CA/AC Acid Blue 60 Flux = 62 L⋅m− ⋅h (Zhao et al., 2019)
2 − 1
CA/MOFDPC Methylene Blue 10 Flux = 76 L⋅m− ⋅h , Rejection = 94 % (Tahazadeh et al., 2021)
CA/SnO2 Methylene Blue 5 Rejection = 95 % (Costantino et al., 2020)
Methyl Orange 5 Rejection = 92 %
CA + CNC Victoria Blue 5 Rejection = 98 % (Nair and Mathew, 2017)

previously in dye processing. The production costs for producing a single flat sheet composite mem­
brane with MCC filling using water hyacinth, sengon wood, and kapok
fiber are $12.64, $12.88, and $14.74, respectively. This outcome is
3.3. Economic analysis of composite membrane manufacturing
regarded as highly economical in comparison to composite membranes
employing commercial MCC as a filler, which can cost as much as
One approach to achieve cost-effective membranes with high per­
$419.20. Furthermore, the composite membranes containing MCC
formance is by incorporating lignocellulosic biomass-based fillers into
fillers derived from the three lignocellulosic biomasses offer several
composite membranes. An economic analysis was conducted by quan­
advantages over commercially available cellulose acetate polymer
tifying the expenses associated with utilizing chemicals for the extrac­
membranes, which can be priced as high as $148.29. These advantages
tion of MCC from lignocellulosic biomass and manufacturing composite
include lower cost and improved performance.
membranes. These costs were then compared to those incurred when
using commercially available MCC. The cost of separating MCC from
4. Conclusions
water hyacinth, sengon wood, and kapok fiber is reduced due to their
abundant natural availability. In addition, its abundance ensures that
The alkalinization method has successfully obtained MCC isolated
these three biomasses can serve as a reliable source of MCC. The isola­
from the lignocellulosic biomass of water hyacinth, sengon wood, and
tion method involves several phases, including dewaxing, delignifica­
kapok fiber. The MCC diffractogram obtained has shown typical in­
tion, bleaching, and hydrolysis. The production costs for MCC from
tensity peaks of cellulose. The isolated MCC also showed a low lignin
water hyacinth, sengon wood, and kapok fiber sources are $8.82, $9.06,
content, as evidenced by the loss of absorption peaks indicating the
and $10.92, respectively. The disparity in expenses arises from varia­
presence of lignin compounds. Based on the results of the TGA charac­
tions in the extent of mass reduction during the separation process of
terization, the three MCCs showed good thermal stability up to 317 ◦ C.
each biomass, hence necessitating distinct production costs. Neverthe­
In addition, composite membranes with MCC-based fillers have also
less, the total cost is considerably lower than the retail price of com­
been synthesized by the phase inversion method. The addition of MCC
mercial MCC, which is quoted at a maximum of $415.38. These
increased the tensile strength of the membrane from 1.13 to 3.05
differences impact the fabrication expenses of composite membranes.

13
R. Abdullah et al.
N⋅mm-2, but it also reduced the membrane contact angle from 65 to 52◦ .
This shows an increase in the hydrophilicity of the membrane. Along
with the increase in hydrophilicity, the porosity of the composite
membrane also increased from 82 to 88 %. In the separation of MB, the
entire membrane synthesized in this study has shown better perfor­
mance than the pure cellulose acetate membrane, which has a water flux
of 43 L⋅m− 2⋅h− 1 and an MB rejection of 64 %. Composite membranes
with MCC fillers can increase water flux to 82–88 L⋅m− 2⋅h− 1 with the
order WH_MCC > KF_MCC > SW_MCC. In addition, it is also able to
increase MB rejection by up to 76–99 % in the order KF_MCC >
WH_MCC > SW_MCC. Furthermore, the utilization of lignocellulosic
biomass as a filler in composite membranes exhibited promising per­
formance in dye separation. This research emphasized the advantageous
aspect of converting biomass waste into functional materials as opposed
to using synthetic materials for membrane production.
CRediT authorship contribution statement
Romario Abdullah: Data curation, Formal analysis, Methodology,
Writing – original draft. Dinia Astira: Data curation, Investigation.
Utari Zulfiani: Data curation. Alvin Rahmad Widyanto: Methodology,
Writing – original draft. Alvin Romadhoni Putra Hidayat: Data cura­
tion. Dety Oktavia Sulistiono: Formal analysis. Zeni Rahmawati:
Formal analysis, Methodology, Supervision, Validation. Triyanda
Gunawan: Methodology, Validation, Visualization. Yuly Kusumawati:
Conceptualization, Formal analysis, Supervision. Mohd Hafiz Dzarfan
Othman: Methodology, Resources, Supervision. Hamzah Fansuri:
Conceptualization, Formal analysis, Funding acquisition, Methodology,
Project administration, Resources, Supervision, Validation, Writing –
review & editing.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
Acknowledgements
The authors express their appreciation for the research funding
provided by the Ministry of Education, Culture, Research, and Tech­
nology of the Republic of Indonesia for the Penelitian Magister Menuju
Doktor Sarjana Unggul research scheme, with contract No. 009/E5/
PG.02.00.PL/2023 and 1245/PKS/ITS/2023.
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