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COVALEN, 4(1): 41-52, April 2018 e-ISSN: 2477-5398

MANUFACTURING OF CELLULOSE ACETATE MEMBRANE FROM TREE HAND CELLULOSE

BANANA

[The Production of Cellulose Acetate Membrane from Stem of Banana Cellulose]

Dina Apriana Putri Husni1*, Erwin Abd. Womb1, Ruslan1

1Department of Chemistry, Faculty of Mathematics and Natural Sciences, Tadulako University

Jl. Soekarno Hatta Km.9, Earth Campus Tadulako Tondo Palu, Tel. 0451- 422611
* ) Corresponding author: dinaapriana26@gmail.com

Accepted December 17, 2017, Approved February 13, 2018

ABSTRACT

The aim of this research is to find out the ratio of polyethylene glycol in cellulose cetate that produces the
best cellulose acetate membrane. Cellulose was produced by extracting stem of banana. Cellulose acetate
was obtained in cellulose synthesis. The membrane was templated by dissolving cellulose acetate in the
acetone at ratio of 1:45 (w/v) by adding PEG as plasticizer (0; 2; 4; 6; and 8%). Thickness, tensile strength,
and elongation of the membrane were tested by using a micrometer and universal testing machine,
respectively. The rendement of cellulose was 62.5%, while the synthesized cellulose acetate had rendement
of 50%. The molecular weight of cellulose acetate was 24,961.48 g/mol. The best membrane characteristic
was obtained at 8% of PEG with thickness of 0.0206 mm, tensile strength of 20.29 Mpa, and elongation of
3%.
Keyword :Cellulose, Cellulose Acetate, Membrane, PEG

ABSTRACT
This study aims to determine the addition of the ratio of polyethylene glycol to cellulose acetate which
produces the best characteristics of cellulose acetate membranes. Cellulose is obtained from the process of
extracting the banana tree midrib. Cellulose acetate is obtained from the synthesis of cellulose. Membrane
printing was done by dissolving cellulose acetate into 1:45 (w/v) acetone solvent and adding PEG plasticizer
with a variation of 0; 2; 4; 6; and 8%. Membranes were tested for thickness usingmicrometerwhile for
tensile strength and elongation tested withUniversal Testing Machine. The cellulose yield obtained was
62.5%. The yield of cellulose acetate from the synthesis is 50%. The molecular weight of cellulose acetate is
24,961.48 g/mol. The best membrane characteristics were obtained from the addition of 8% PEG which had
a thickness of 0.0206 mm, a tensile strength of 20.29 MPa, and an elongation of 3%.

Keywords:Cellulose, Cellulose Acetate, Membrane, PEG

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COVALEN, 4(1): 41-52, April 2018
BACKGROUND
Renewable technology is a
technology that is growing rapidly and is
the center of world attention today. One
of the renewable technologies that is
being developed is separation technology
using membranes that utilize renewable
materials, namely natural polymers
(Lankaster, 2002).
Separation with
is technology which
developed as
replacement process separation
conventional. This technology has
advantages compared to conventional
techniques, such as low energy required,
can take place continuously, the process
can be combined
with
other separations, do not require a lot of
additives, are suitable for compounds that
are not heat resistant, and do not produce
waste (Nunes, 2001). With these advantages,
membrane technology has been widely
applied in various fields, including in the
industrial, chemical and pharmaceutical
fields, in the field of sewage treatment and
environmental technology in the field of oil
processing, namely the processing of oil and
gas.vegetable oil (Coutinho, 2009). However,
in Indonesia the development of membrane
technology is not as fast as in other
countries because membrane materials still
have to be imported.
Basically, membrane materials can
be derived from ceramics, silica, zeolites,
Dina Apriana Putri Husni et al.
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metal, glass, or polymer (Drioli,et al.,
2010). Biopolymers are generally widely
developed as membrane base materials,
such as chitosan (Astuti, 2008), agar
(Setyaningrumet al.,2017), and cellulose
(Yuanet al.,2009). Cellulose in particular
has great potential as an alternative to
membrane materials or its derivatives
such as cellulose acetate. Indonesia has a
wealth of natural resources as potential
membrane cellulosic materials, including banana tree
many waste fiber which is
alternative
contain up to 63% cellulose (Small,
1954inWijaya, 2002). Referring to the lack
of utilization of banana stems, the banana
tree waste fiber can be used as an
alternative raw material for the
manufacture of cellulose acetate.
process Cellulose acetate has advantages as
a basic material for making membranes
because it has an asymmetric structure
with a very thin active layer, can hold
dissolved materials on a rough support
layer, is resistant to precipitation,
produces a balance of hydrophilic and
hydrophobic properties (Kumano &
Fujiwara, 2008). Cellulose acetate
membrane from banana tree midrib waste
has the following properties:
biodegradable, but the mechanical
properties are less than optimal so that
the useful life of the membrane becomes
short. Because of this, additives are
needed to improve their properties, such
as plasticizers or compounds that enable
the resulting plastic
42
COVALEN, 4(1): 41-52, April 2018
not easily brittle and stiff (Darniet al.,
2009). One of the plastics that is often
used is polyethylene glycol (PEG) because
it is non-toxic, biocompatible, hydrophilic,
has high flexibility, antifoaming agent,and
antifouling
(Apriliani, 2010 and Suet al., 2009). The
addition of PEG to the membrane can
produce membranes with smaller and
more regular pores, Muliawati (2012) and
can increase the value of the membrane
flux (Whichet al.,2001).
Apriliani (2010) used PEG on
chitosan membranes and showed an
increase in membrane permeability of PEG
2:1 and 3:1 respectively giving a value of
0.805 L/m2hours and 2,617 L/m2
hour at a pressure of 1 atm. Fadillah
(2003), Mohammadi and Saljoughi (2009)
and Saljoughi (2010) reported that the
permeation rate of commercial cellulose
acetate membranes will increase with the
addition of PEG. Rini et al (2007) also
reported that the more PEG was added,
the smaller the pores of the rice husk silica
membrane, so it was more effectively
used in batik wastewater decolorization.
Based on these results, it is necessary to
study the cellulose acetate membrane
based on banana stem cellulose with the
addition of PEG.
RESEARCH METHODS
Materials and Equipment
The material used is the waste of the
outer kepok banana tree midrib,
Dina Apriana Putri Husni et al.
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sodium hydroxide, sodium hypochlorite,
sulfuric acid, glacial acetic acid, anhydrous
acetic acid, aquades, acetone,
polyethylene glycol.
The equipment used in this study
were reflux apparatus, blender, 60 mesh
sieve, FTIR spectrophotometer, Ostwald
viscometer,hot plateWiseStir MSH 20-D,
stirrer, Memmert oven, Adventure TM
Ohaus brand analytical balance, filter
paper, desiccator,micrometerKrisbow,
gegep, oven, glass plate 25x30 cm and
glassware commonly used in the
laboratory.
Work procedures
Sample Preparation (Ningsih et al., 2014)
The midrib of the kepok banana tree
is washed with running water. Then
drained, then cut into small pieces until
the sample of the kepok banana midrib is
dry. The dry samples were ground and
sieved through a 60 mesh sieve.
Extraction of cellulose (Rosli et al., 2013)
Samples of banana tree fronds as much
as 10 grams were added with 250 mL of 4%
(w/v) sodium hydroxide and refluxed at 700C
for 2 hours. Then washed with distilled
water until the pH is neutral. After that, the
bleaching process was carried out using 250
mL of 1.7% sodium hypochlorite (v/v) at a
temperature of 700C for 4 hours. Then
washed with distilled water until the pH is
neutral. The ratio of sample in solution is
1:25 (g/mL). Each sample treatment was
carried out twice and
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COVALEN, 4(1): 41-52, April 2018 e-ISSN: 2477-5398

samples were washed using distilled Determination of Cellulose Acetate Molecular

Weight
water. Then dried in the oven at a
Determination of the molecular weight of cellulose
temperature of 700C for 4 hours. Then
acetate using an Oswald viscometer.
grind it using a mortar and pestle. So that
Cellulose acetate solution was prepared
the cellulose dry powder is obtained. The
with a concentration of 0.0; 0.05; 0.1; 0.15;
resulting sample then
0.2 and 0.25 g/25 mL acetone solution. A
tested characterization
volume of the solution was put into an
using FTIR.
Oswald viscometer and the flow time was
Synthesis of cellulose acetate (Bahmid et determined by repeated measurements.
al., 2014) Khaswar and Tutus, 2014)
Molecular weight can be calculated using
15 grams of cellulose added 150
the Mark-Houwink equation:
mL of glacial acetic acid (1:10) and stirred
at 380C for 60 minutes. Cellulose was
Relative Viscosity r=/ o t/to sp=r -
added 2% (v/v) sulfuric acid pa and stirred
Specific viscosity 1
at 380C for 45 minutes. The result of
Intrinsic Viscosity [η] = (ηsp/c)
activation is added 100 mL of acetic
=KMa
anhydride pa then stirred at 380C for 45
where: K=1.49 x 104ml/g =
minutes. The results of acetylation were
0.82
added with 10 mL of distilled water and 20
= viscosity of the substance
mL of glacial acetic acid and stirred at 500C
0=solvent viscosity
for 30 minutes. The solution was then
t = time of flow of substance (in
centrifuged. The precipitate obtained was seconds) t0= solvent flow time

put into 500 mL of distilled water to form

white cellulose acetate flakes. The Manufacture of cellulose acetate membrane
(Modification of Pasla method, 2006)
cellulose acetate flakes were then filtered
Fabrication of membranes through phase
using a funnel and washed with distilled
inversion by immersion. The first step is
water until the sour smell disappeared.
10 grams of cellulose acetate dissolved in
Then dried in the oven at a temperature of
45 mL of acetone and stirred using a
550C for 4 hours. In order to obtain a dry
stirrer until well mixed. Polyethylene
powder of cellulose acetate. The resulting
glycol (PEG) plasticizer was added to the
sample was then tested for
solution with a variation of 0 ; 2 ; 4 ; 6 and
characterization using FTIR and
8% by weight of cellulose acetate. Prepare
determined the molecular weight of
a glass measuring 20 x 15 cm which has
cellulose acetate.
been tapered on both opposite sides.
polymer solution is poured over

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COVALEN, 4(1): 41-52, April 2018 e-ISSN: 2477-5398

The cross section of the glass is then Elongation (%) = x 100%

printed as a thin layer by pressing it with a
Information :
rodstainlessthen withdraw the polymer : membrane elongation (cm) :
L initial length of membrane (cm)
solution, until a thin layer is obtained. This
thin layer sticks to the glass and is left for
RESULTS AND DISCUSSION
1 minute. Then, the glass cross-section is
Banana Leaf Cellulose Extract Tree
immersed in water until the thin film that
sticks out is separated from the glass The cellulose extraction process is carried out

cross-section. Next, the thin layer is dried by refluxing a sample of banana tree
fronds with 4% NaOH. The crystalline
structure of lignin and the amorphous
structure of hemicellulose can be
Membrane characteristic testing.
damaged by NaOH so it is very suitable to
1. Thickness Test (Akiliet al., 2012)
be used to remove lignin at a time
Thicknessfilmmeasured using
extract hemicellulose. Generally
micrometer(accuracy of 0.001 mm) by
the fiber product produced in the
placingfilmbetween jaws micrometer. For
delignification process by NaOH is white
each samplefilmto be tested, the thickness
but in this study it is still brown. So that
is measured at five different points, then
the bleaching process is carried out so
the average is calculated.
that the color of the fiber becomes
brighter or white.
2. Mechanical Properties (ASTM 882-91,
Process extraction cellulose
1996) Determination of tensile
produces a white dry powder which is
strength and elongation were tested using
coarse cellulose. The cellulose yield of
Universal Testing Machine. Specimenfilm
banana midrib was 62.5%. The pure
cut (8 cm x 0.5 cm) from each sample and
cellulose IR spectrum gives an absorption
installed between the grips of the
peak in the wavenumber region at 3350
machine. The tensile strength is
cm-1where the peak is between 3400 cm-1–
determined based on the maximum load
3500 cm-1indicates the presence of OH
atfilmrupture and elongation percentage
stretch, 2800 cm-1– 2900 cm-1
is based on elongationfilmmomentfilm
break. Mathematically this relationship
shows the presence of CH stretching, 1160
can be written as follows:
cm-1indicates COC stretching, and 1035 cm
Tensile strength(N/m²) = -1 – 1060 cm-1
Information : indicates the presence of CO stretching. In
F: tensile strength (N) A:
the fingerprint area, cellulose gives a peak
cross-sectional area (m2)
around 1300 cm-1

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COVALEN, 4(1): 41-52, April 2018 e-ISSN: 2477-5398

indicates the presence of CH bending and 5-10% excess anhydride (Mc.Ketta, 1982).
about 1400 cm-1indicates the presence of In this acetylation process, most of the
CH2bending (Marchessault and hydroxyl groups are replaced by acetyl
Sundararajan, 1983). The results of the IR groups. In complete esterification, the
spectrum of banana midrib cellulose majority of the remaining hydroxyl groups
showed a peak at 3423 cm-1, 2854 cm- are bound to the primary dihydroxyl
1, 1431 cm-1, 1323 cm-1, 1161 cm-1, and groups of the cellulose.
1020 cm-1. These results have similar IR
spectra with pure cellulose.
According to Kamalet al., (2014)
characterization of cellulose bonds in
absorption board spectrum at 3300-3500 cm
-1 corresponding stretching
shows the OH group. Absorption bond at
2700-2900 cm-1characterized by the Figure 1 Mechanism of acetylation reaction

presence of –CH . group2(CH stretching) .

The weight of cellulose before being
Bond characterization at 1065 cm-1for the
synthesized was 10 grams and after the
COC (ether linkage) of the glycoside unit.
synthesis process the sample weight was
5 grams. So that the yield of cellulose
Table 1 Wave Number (cm-1) cellulose acetate from banana midrib is 50%. The
Wave Number (cm-1)
yield of cellulose acetate obtained in this
Cellulose Cellulose Group
No Cellulose study was higher than the yield of
Results (Kamalet Function
Pure
Study al., 2014) cellulose acetate from waste cellulose
1 3350 3423 3300 OH Ulur agar by Nurhayati and Rinta (2014), which

2 2800 2854 2700 CH Ulur obtained a yield of 26.19%.

3 1400 1431 - CH2Buckling

4 1300 1323 - CH Bend

Results analysis group function

5 1035 1020 1065 CO Stretch using FTIR showed an absorption peak of

Synthesized Cellulose Acetate
The acetylation process aims to
produce cellulose acetate. The solution for
this acetylation is obtained by heating and
stirring the cellulose by adding the acetate
mixture
the carbonyl group, C=O (1749-1622 cm-1)
and the CO ester group of the acetyl
group (1377cm-1) each at a wave number
of 1749 cm-1and 1377 cm-1. This indicates
the formation of cellulose acetate
compounds with a sharp peak at

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COVALEN, 4(1): 41-52, April 2018 e-ISSN: 2477-5398

wavenumber 1749 cm-1and a decrease in membrane manufacture (Habibahet al.,

the intensity of the OH group due to being 2013).
substituted by an acetyl group. Looks Based on results study
similar, only the OH group at wave The molecular weight of cellulose acetate
number 3406.29 cm-1from commercial from the synthesis of cellulose from
cellulose acetate has a higher absorption banana midrib was 24,961.48 g/mol.
than the synthesized cellulose acetate. These results are greater when compared
Typical absorption peaks of commercial to previous research by Wijoyo (2002) with
and synthetic cellulose acetate can be a sample ofEucalyptus Albawhich is 17,746
seen in Table 2. g/mol, but smaller than the molecular
weight of pure cellulose acetate of 30,000
g/mol.
Table 2 Wave Number (cm-1) cellulose
acetate
According to Wijoyo (2002), several factors
Wave Number (cm-1) that affect the molecular weight of cellulose
Cellulose
Cellulose acetate are the length of the fiber from the
Cellulose acetate Group
No acetate
Acetate (Nurhayati Function cellulose/base material, the time of the pre-
results
commercial and Rinta,
synthesis treatment process, the time of the acetylation
2014)
1 3486.97 3632.20 3391.59 OH stretch process and the hydrolysis time, the composition

2 2960.38 2961.62 2901.7 CH alkanes of the materials used in the manufacture of

3 1754.63 1755.90 1636.49 C=O stretch cellulose acetate.

4 1383.89 1372.53 1027.02 COC stretch
Cellulose Acetate Membrane

Cellulose Acetate Molecular Weight Cellulose acetate is applied to

Determination of the molecular weight making membrane with

(BM) of cellulose acetate was carried out by the adding plasticizer with the aim of

capillary or Ostwald method. The principle of this increasing the elasticity of the membrane.

method is to measure the time required for the The addition of PEG plasticizer needs to be

liquid being measured to pass through the two done because the cellulose acetate

boundary marks due to the gravitational force on membrane produced without plasticizer is

the Ostwald viscometer. very fragile so it cannot be peeled off from

Molecular weight from biopolymer the mold (Khaswar and Tutus, 2014).

cellulose acetate is an important

parameter to determine its properties. In The resulting membrane is transparent

general, polymers with high molecular white like plastic. In this study, the physical

weights have more distinctive properties properties of the membrane were tested by

with benefits that are more likely to measuring the thickness of the membrane,

tensile strength and elongation tests.

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COVALEN, 4(1): 41-52, April 2018 e-ISSN: 2477-5398

1. Thickness membrane could influence

Thickness membrane be measured characterization of the filtration membrane (Mulder,

use micrometer (accuracy 1996).

0.001 mm). Thickness membrane 2. Tensile Strength

influenced by the thickness of the duct tensile strength (tensile strength)

tape used in the printing process. The is the maximum tensile force that a film
thickness of the tape used is 0.036 mm. can withstand until it breaks (Astuti, 2008).
The average membrane thickness using The greater the tensile strength, the
different PEG concentrations can be seen better the membrane
in Figure 2 in withhold damage
0.03 mechanical. Average tensile strength

0.025 membrane with addition

Thickness(mm)

0.02 different PEG concentrations are shown in

0.015 Figure 3
0.01 25
0.005
20
0
0% 2% 4% 6% 8%
15
Tensile Strength

PEG concentration

10
Figure 2 Graph of PEG . Concentration Relationship
Against Membrane Thickness
5

Membranes formed with variations 0

in PEG concentrations have various 0% 2% 4% 6% 8%

thicknesses. The results of the average PEG concentration

thickness measurement (Figure 2) show Figure 3 Graph of PEG . Concentration Relationship

Against Membrane Tensile Strength
that enhancement

concentration PEG tend

Figure 3 shows that the highest tensile
increase the membrane thickness. The
strength of the membrane was 20.29 MPa
result of the highest membrane thickness
obtained at 8% PEG concentration and the
test was 0.0077 mm at 2% PEG
lowest was 12.61 MPa at 13.3% glycerol
concentration and the lowest was 0.0059
concentration, while the control had a
mm at 0% PEG concentration. This
tensile strength value of 12.61 MPa. The
membrane is thinner than the agar-agar
results of this tensile strength test do not
polymer-based membrane (0.0167 mm)
meet the minimum standard of tensile
(Setyaningrumet al.,2017). Thickness
strength. According to Harrisonet al., (2006),
tensile strength for cellulose membranes

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COVALEN, 4(1): 41-52, April 2018
acetate is 30 Mpa, while the tensile
strength for polyvinyl chloride membrane
is 20 Mpa.
Enhancement score strong
influenced by the size of the fiber making
up cellulose acetate. The smaller the size
of the fiber making up cellulose acetate,
the higher the tensile strength value
produced.
This is in accordance with the
statement by Lu and Kessler (2013), that
nanoparticles have a specific surface area
larger than micron size particles, other
polymer molecules will be adsorbed to
cover the surface of nanoparticles of the
same mass thereby reducing voids in the
material.
3. Elongation
Elongation obtained
comparison increase
maximum length of the membrane with its
initial length (Pasla, 2006). The average
value of membrane elongation with the
addition of different PEG concentrations can
be seen in Figure 4.
Elongation percentage shows how
wide the membrane can be stretched,
elongation shows the flexibility of the
membrane (Yuanet al.,2009). The average
elongation of the membranes produced
by treatment with PEG concentration was
1-3%. However, this result still does not
meet the standard of membrane
elongation value according to ASTM
(1996), where the maximum membrane
has an elongation value of 30-45%. The
results obtained are also lower
Dina Apriana Putri Husni et al.
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compared to using glycerol as a plasticizer
on an agar membrane, which is 12.75%
(Setyaningrumet al.,2017).
pull 3.5
3
2.5
Elongation (%)
2
1.5
1
0.5
0
0% 2% 4% 6% 8%
PEG concentration
Figure 4 Graph of PEG . Concentration Relationship
Against Membrane Elongation
The increase in elongation is caused
by the increase in the number of
hydrogen bonds formed due to the
from plasticizer filling the pores in the
long membrane. The higher the hydrogen
bond, the higher the viscoelasticity
response. (Bahmidet al., 2014).
CONCLUSION
Based on the results obtained, it can
be concluded that the yield of cellulose
obtained from the extraction is 62.5% and
the yield of cellulose acetate obtained
from the synthesis is 50% with a molecular
weight of 24,961.48 g/mol. The formation
of cellulose acetate was indicated by the
results of the FTIR identification in the
form of absorption of the C=O carbonyl
group at a wave number of 1749.44 cm-1
and CO ester of acetyl group 1377cm-1
. The highest membrane thickness
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COVALEN, 4(1): 41-52, April 2018
obtained at a concentration of 2% PEG
was 0.0258 mm. The concentration of PEG
on cellulose acetate that produces the
best membrane characteristics is PEG 8%
with a tensile strength of 20.29 Mpa and
an elongation of 3%.
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