Hindawi

Advances in Materials Science and Engineering

Volume 2022, Article ID 1712207, 10 pages
https://doi.org/10.1155/2022/1712207

Research Article
Extraction of Cellulose from Sugarcane Bagasse Optimization
and Characterization

Getu T. Melesse,1 Fekadu G. Hone ,2 and Mulualem A. Mekonnen 1

1
Faculty of Materials Science and Engineering, Jimma Institute of Technology, Jimma University, P. O. Box: 378, Jimma, Ethiopia
2
Department of Physics, Addis Ababa University, P.O. Box: 1176, Addis Ababa, Ethiopia

Correspondence should be addressed to Mulualem A. Mekonnen; [email protected]

Received 1 July 2022; Revised 31 August 2022; Accepted 26 September 2022; Published 10 October 2022

Academic Editor: Jirapornchai Suksaeree

Copyright © 2022 Getu T. Melesse et al. (is is an open access article distributed under the Creative Commons Attribution
License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is
properly cited.
In this study, cellulose was extracted from sugarcane bagasse (SCB) through a convenient five-step treatment, and procedures
were performed. During the alkaline curing process of the extraction of cellulose, NaOH has a concentration of (0.5, 1.5, 2.75, and
4%) and the extraction time (15, 30, and 45 min) at a constant temperature of 120°C were taken as variables and perfectly
optimized by response surface methodology (RSM) for cellulose with the highest product. (e optimum conditions were found to
be 2.75% NaOH, 120°C, and 45 min with a cellulose yield of 73.71 ± 0.67% cellulose, 17.22 ± 0.82% hemicellulose, and 9.07 ± 0.95%
lignin. (ough most of the lignin was eliminated during the alkaline and dilute acid pretreatment process, the remaining lignin
was removed by a solution treatment of 4% NaOH, and 21.92% H2O2 at 121°C for 44.97 min where the cellulose yield was found as
89.75 ± 0.64%, hemicellulose was 6.15 ± 0.83%, and lignin was 2.65 ± 0.66%. Morphological analysis revealed that the average
diameter of the cellulose was 12.06 µm. (ermal and XRD diffraction analysis showed that the cellulose is thermally stable and has
a crystallinity index of 31.63%. FTIR spectra demonstrate that cellulose was successfully extracted due to the removal of
noncellulose components.

1. Introduction Furthermore, hemicelluloses can form hydrogen bonds with

cellulose and lignin, which is why they are called “cross-
(e main constituent of plant biomass is lignocellulosic linking glucans” [12]. (e chemical structure of hemicel-
materials such as lignin, hemicellulose, and cellulose. Ag- lulose is shown in Figure 1.
ricultural byproducts from plant biomass can serve as Lignin is composed of phenylpropane polymeric units,
sustainable, renewable, and inexpensive raw materials for which has high resistance to chemical and physical influ-
the production of industrial biopolymers [1]. For example, ences and is insoluble in water. (e main function of lignin is
the cellulose content of SCB is around 40–50% [2]; isolated to hold fibers together. (e major components of lignin are
cellulosic fibers and their derivatives have attracted attention p-hydroxyphenyl, guaiacyl, and syringyl as shown in
for their applications ranging from paper, packaging, sen- Figure 2.
sors, water purification, and textiles to biomedical devices Cellulose is the largest and most important natural
and drug delivery due to their advantageous properties such biopolymer present in plants in the form of microfibrils and
as low density, high surface area, and good mechanical is known for its turnover capacity, biocompatibility, and
strength [3–9]. Hemicellulose is an amorphous polymer biodegradability [15]. (e molecular structure of cellulose
usually composed of different types of C6 and C5 sugars: consists of hydroxyl groups in the chain, which can easily
D-glucose, D-xylose, D-mannose, D-galactose, L-arabinose, form chemical bonds with various compounds to create
D-glucuronic acid, and L-fucose. Hemicellulose is amor- many derivatives [16], shown in Figure 3. (is leads to
phous [10] and a large and complex carbohydrate molecule multiple technological uses of cellulose including trans-
that helps cross-link cellulose fibers in plant cell walls [11]. portation of drugs [17], polymer fillers [18], gases,
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2 Advances in Materials Science and Engineering

HO3C
O
H3CO
HO H Xilose
OH H

OH O OH
HO O HO
O
O HO O
O OH O n

Figure 1: Chemical structure of hemicellulose [13].

CH2OH CH2OH CH2OH biomass sources to reach the diverse needs of the community
CH CH CH [22]. In the broadest sense, a biorefinery can be defined as a
CH CH CH facility that produces a large area of different products
through the use of different biomass feedstocks.
Numerous pretreatment methods for biomass deligni-
fication have been reported, including physical, biological,
OCH3 H3CO OCH3 chemical, and combined methods (ammonia fiber blast and
OH OH OH vapor) [23–29]. In fact, each pretreatment process has its
p-Hydroxyfenyl Guaiacyl Syringyl pros and cons; For example, physical pretreatment such as
Figure 2: Structure of the main subunits of lignin precursors [14].
grinding and milling requires fewer chemicals but con-
sumes a lot of energy, especially in large-scale production
[19], while the biological treatment process reduce lignin
and hemicellulose, but the hydrolysis process needs over-
consumables, meals, papermaking, fabrics, and many more. long time [29–31]. (e chemical pretreatment process is a
(is provides a compelling starting material for a wide range well-studied pretreatment technique which produces a
of industrial applications and has generated considerable myriad of harmful chemicals, such as hydrogen sulfide [32].
research interest. Cellulose is a polymer consisting of (e dilute acid pretreatment method can get rid of hemi-
anhydro glucose fractions bonded to carbon atoms four and cellulose, but corrodes instruments and harms the envi-
one through b-glycosidic bonds. (is is corroborated by the ronment [33]. Alkaline pretreatment process is to a greater
existence of 3 hydroxyl groups with reactivity, OH secondary extent appropriate for enzymatic hydrolysis as it effectively
to C-2, OH secondary to C-3, and OH number one to C-6, removes lignin and limits carbohydrate degradation com-
and therefore by the establishment of numerous van der pared to other similar methods [34]. (is method incor-
Waals, and hydrogen bonds within solid molecule [19]. It is porates sodium hydroxide, lime, ammonia, and alkaline
organized into fibrils surrounded by a matrix of lignin and hydrogen peroxide (AHP) chemicals for pretreatment
hemicellulose. Currently, it seems to be common knowledge process [34, 35]. Among the alkali-based pretreatments,
that cellulose I has a parallel chain orientation, while in hydrogen peroxide (H2O2) is widely utilized in the pulp firm
cellulose II, the chains are antiparallel [20]. to whiten and enhance the transparency of the paper. (e
(ere is no doubt that the natural resources available to usage of H2O2 causes the production of hydroperoxyl anion
the world population are limited. Society is currently facing a at an alkaline pH (pH 11.5), which is the main cause of the
number of ecological and social challenges such as global dissolution of lignin and hemicellulose [36]. Many re-
population growth, climate change, and the destruction of searchers help in the development of AHP pretreatment to
ecosystems, which require the definition of new production enhance the enzymatic hydrolysis of lignocellulosic raw
and consumption patterns that are economically, socially, materials [37–39]. For example, Su et al. fractionated
and ecologically sustainable. In this context, the bioeconomy hemicellulose and lignin from corn cobs with a pull out
can provide a clear answer, contributing to the equitable ratio of 38.7% and 75.4%, respectively, after 6 h of treatment
supply and distribution of food, to mitigate the effects of with AHP [39].
climate change and to reduce the use of fossil fuels. Fur- We report a simple five-step process which is an efficient
thermore, it can offer new opportunities for economic de- and environmentally advantageous method for extracting
velopment and employment. (e biorefinery strategy has cellulose from SCB. In addition, the properties of the
been identified as a key element in fostering the arising extracted cellulose were characterized and analyzed. (e
bioeconomy by providing a broad variety of products from a extracted cellulose has a good index of crystallinity, very
large collection of biomass sources to meet diverse society good thermal stability, and high cellulose content under
demands [21]. Biorefineries are a crucial instrument for the alkaline AHP bleaching conditions. (is study reports the
development of the bioeconomy, with the aim of providing a utility of sugarcane bagasse and its cellulose as reinforcing
wide range of product collections from a broad span of fillers for polymers composites.
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Advances in Materials Science and Engineering 3

OH OH
OH HO OH HO OH
O O
HO O O HO O O
O O HO O O n
O OH
OH
OH OH OH
Figure 3: Chemical structure of cellulose molecule [14].

2. Experiment method developed by Chesson (2016) and the results are

compiled in Table S1 in Supporting Information (SI).
2.1. Materials. (e SCB sample was taken and left air dried
for 24 hours. (e dried SCB was kept in an oven at 100°C for
8 h to bring the moisture content to 8–10%. (e dried SCB 2.2.3. Optimization for Dilute Acid Treatment Conditions.
was physically fractionated with 4 mm and 3 mm mesh (e experimental trials were determined using GFD sta-
particle sizes and stored in an airtight polyethylene plastic tistical methodology. (e experimental design had two
bag to keep the sample dry for further research phase. (e factors: concentrations of dilute sulfuric acid (A) (0.5, 2.5,
macromolecular composition of fractionated dried SCB is and 5%) and reaction times (B) (15 and 30 min.) with a total
referred in Table 1. (e chemicals used are purchased from of 3 ∗ 2 � 6 main treatment combinations and a QM con-
the local representatives of Merck and Sigma-Aldrich, sisting of 12 serial experiments used, including duplicate
Ethiopia, the chemicals are sodium hydroxide (NaOH) (AR, replicates for each of the treatment conditions. (e treat-
Assay 98%), sodium hypochlorite (NaOCl), acetic acid, ment of the same solid charge (5%) of sugarcane bagasse was
sulfuric acid (H2SO4) (AR, 98% Assay), hydrogen peroxide carried out in a water bath (Sr.N. 106544116, Germany)
(H2O2) (the 30% ACS reagent contains inhibitors), ethanol under reflux at a constant temperature of 100°C while the
(AR, C2H5OH) (>99%). amount of solid became liquid (H2SO4), the ratio was kept
constant at 1:10 (g/ml). (e contents are separated from the
solid fraction by vacuum filtration. (e remaining solids
2.2. Optimization and Extraction of Cellulose were washed thoroughly with warm DI water to neutral pH
and oven-dried at 105°C overnight. (e sample moisture was
2.2.1. Pretreatment Stages: Dewaxing, Boiling, and Washing. maintained at approximately 8–10% (dry basis). (en, the
(e physically fractionated SCB, first dewaxed for about 4 h data on the composition analysis of the amount of SCB
using an ethanol/DI water mixture (1:1 v/v), and the mixture treated with dilute sulfuric acid of extracted cellulose,
is boiled for 1.5 h, this process is repeated twice to wash and hemicellulose, and lignin were collected by gravimetry based
dirt, dust, Earth, marrow, sugar extracts and those water- on the method developed by Chesson [40], and the results
soluble impurities. are summarized in Table S2 in SI. (e percentage of each of
(e dewaxed SCB powder was washed thoroughly with the collected data was calculated using a general factorial
DI water at a temperature of 95°C, followed by cold DI water design from Design-Expert software (Stat-Ease Inc., version
to remove some of the residual sugar and surfactants. It was 7.0) for statistical analysis to determine an optimal treatment
air dried for 24 h and then dried in an oven (model 30–1060, combination. Furthermore, a regression model was devel-
GmbH, Germany) to constant weight at 85°C for 16 h. (e oped between the optimal response (as a dependent variable)
humidity of the sample is maintained at about 10% (on a dry and the optimal treatment combination (as independent
basis) with a moisture analyzer (SARTOTIUS AG GER- variables).
MANY, MA 35 M-000230V2) for subsequent chemical
treatments and characterization applications. (e chemical
composition of dewaxed SCB is given in Table 1. 2.2.4. Optimization for First-Step Bleaching Treatment
Conditions. In addition to the alkaline pretreatment, the
insoluble residue was refined and washed with distilled
2.2.2. Optimization of Alkali Treatment Conditions. water. Although most of the lignin was eliminated during the
NaOH-alkali treatments were carried out on the dried, alkaline pretreatment process, the remaining lignin was
crushed, ground, and sieved sample obtained after the extracted using 1% NaOCl solution at 95°C for 60 minutes.
completion of the pretreatment steps and after the deter- (is step was repeated twice, then, the cellulose was sieved
mination of the experimental tests using a statistical general and rinsed with distilled water until the pH of the filtrate
factorial design (GFD) methodology. (e experimental became neutral. Finally, the resulting cellulose was dried in a
design had two factors: concentrations of NaOH (A) (0.5, hot air oven at 50°C for 24 hours. (e RSM methodology was
1.5, 2.75 and 4%) and reaction times (B) (15, 30 and 45 min.) used using Design-Expert software to optimize effective
at a constant temperature of 120°C, for a total of 4 ∗ 3 � 12 parameters in the first stage bleaching process, which re-
treatment combinations. (e quadratic model (QM) was covers cellulose and hemicellulose and lignin concentrations
used and comprised of 24 experimental runs, incorporating are minimized, shown in Table 2. (ree factors and a QM
double replication for each of the treatments. Computational consisting of 20 combinations of experimental procedure
analysis data were collected gravimetrically based on the were used for the first-stage bleaching pretreatment process,
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4 Advances in Materials Science and Engineering

Table 1: Chemical composition of untreated and dewaxed sugarcane bagasse determined by the Chesson method of gravimetric analysis.
SN Sample Sample kind Moisture (%) Cellulose (%) Hemicellulose (%) Lignin (%) Ash (%) Extractives (%) Total
1 A Untreated 6 42.40 25.20 19.70 3.01 9.69 100
2 B Dewaxed 6 58.86 18.79 17.60 2.25 2.50 100

Table 2: Description of the first four optimized predicted solutions of the RSM quadratic model Design matrix for the first-step bleaching
treatment.
Model parameter Yields
Factors used in ANOVA Y1, cellulose Y2, hemicellulose Y3, lignin
(%) (%) (%) Desirability Rank
2B: Time 3C: Temp
1A: Acidified NaOCl (%) Pred. Pred. Pred.
(min) (°C)
1 5 75.00 86.86 ± 0.35 7.90 ± 0.48 5.01 ± 0.25 0.969 1st
1 5 75.12 86.79 ± 0.74 7.89 ± 0.64 5.017 ± 0.93 0.966 2nd
1 5 75.00 86.80 ± 0.81 7.88 ± 0.86 5.022 ± 0.69 0.966 3rd
1 4.98 75.00 86.75 ± 0.77 7.89 ± 0.90 5.019 ± 0.75 0.962 4th

of which 6 replicates were performed. (e design variables the QM consisting of 50 combinations of experimental
considered the lower and higher levels of 5 individual runs in treatments were employed for investigation. (e design
each of the three factors, such as concentration of NaOCl parameters were the high and low levels of 5 individual runs
acidified to pH 3–5 (adjusted with 1 M glacial acetic acid) in each of the five factors of NaOH concentration, H2O2
(1A) (0, 1, 1.5, 2, and 2.34% by %), extraction temperatures concentration, temperature required for extraction, ex-
(2B) (68, 12, 75, 85, 95, and 101.82 in °C) and extraction time traction time, and extraction pressure, while the response
(3C) (2.99, 3.5, 4.25, and 5.51 in hours), while the ratio of variables were the yield of cellulose, hemicellulose, and
solids (sugarcane bagasse) to liquid (acidified NaOCl) was lignin. (e second bleaching solution treatment was carried
kept constant at 1:10 (g/ml). out in a vertical autoclave (VSL series, equipped with digital
(e first stage of bleach solution processing was ac- temperature, pressure, and time control) while maintaining
complished in a vertical autoclave furnished with digital the solid to liquid ratio (mixtures of NaOH–H2O2) con-
temperature and time controls while reaction variables such stant at 1:10 (g/ml). After boiling, the insoluble residue was
as cellulose yield, hemicellulose, and lignin of sugarcane collected under vacuum filtration and washed heavily with
bagasse were evaluated. (e samples with the highest cel- deionized water at neutral pH to take away all soluble
lulose concentrations and with the lowest lignin and materials. (e left over white paste residue was oven-dried
hemicellulose concentrations were selected from the dilute at a temperature of 105°C for 24 h and referred to as
sulfuric acid pretreatment process. After boiling, the liquid “purified cellulose.” (e humidity of sample was sustained
contents were separated from the solid parts through vac- around 8–10% (dry basis) for the next chemical treatments
uum filtration. (e remaining solids were washed thoroughly and characterizations and stockpiled in fasten polythene
with warm deionized water to neutral pH and oven-dried at bags at room temperature. Subsequently, the data for the
105°C for 15 h. Sample humidity maintained at approximately compositional analysis of the amount of cellulose, hemi-
8–10% (dry basis) for later chemical treatments and char- cellulose, and lignin extracted from the sugarcane bagasse
acterizations and kept in sealed polythene bags at room treated in the second bleaching step were collected gravi-
temperature. Subsequently, the compositional analysis data metrically according to the method developed by Chesson.
from the first bleaching process for the extracted cellulose, Percentages of all data collected from the gravimetric
hemicellulose, and lignin were collected gravimetrically analysis were calculated in STATISTICA Design-Expert
according to the method [40]. software and used for statistical and graphical analysis to
determine the optimal treatment mix.
(e X-ray diffraction of the powder was carried out
2.2.5. Optimization for Second-Step Alkaline Hydrogen using Drawell XRD 7000 with the Johanson monochromator
Peroxide (AHP) Bleaching Treatment Conditions. (e in the incident beam to remove the Cu-Kα2 radiation.
bleaching process was completed by evaluating the effect of (e crystallinity index (CI) was calculated using equation
second stage alkaline hydrogen peroxide (AHP) solutions (1), [41].
at pH 11–12.5 under the conditions of the bleaching
process. It was performed to remove hemicellulose and I002 − Iam 􏼁
CI(%) � 􏼢 􏼣 × 100, (1)
lignin from SCB with a small modification of the method I002
described by Sun et al. [26]. (e RSM design was used to
optimize the best combination of second stage bleaching where I002 is the maximum intensity of the (002) diffraction
process parameters for cellulose extraction as reported in at 2θ value of about 22.2°, while Iam is the intensity dif-
Table 3. (e study used five factors as a parameter used in fraction at 2θ value of around 18°.
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Advances in Materials Science and Engineering 5

Table 3: Description of the first three optimized predicted solutions of the RSM quadratic model design matrix for the second-step
bleaching treatment.
Model parameter Yields
Y2,
Factors used in ANOVA Y1, cellulose Y3, lignin
Hemicellulose Rank for the
(%) (%) Desirability
(%) selection
2B: Conc. 3C: 4D: 5E:
1A: Conc. Of
Of H2O2 Time Temp Pressure Pred. Pred. Pred.
NaOH (%)
(%) (min) (oC) (Psi)
4.00 21.92 44.97 121.0 15.0 89.75 ± 0.64 6.14 ± 0.83 2.65 ± 0.66 0.97 1st
4.00 20.94 45.00 120.9 15.0 89.70 ± 0.58 6.17 ± 0.73 2.69 ± 0.96 0.97 2nd
3.89 20.52 45.00 120.9 15.0 89.75 ± 0.67 6.20 ± 0.40 2.73 ± 0.87 0.97 3rd

3. Results and Discussion

3.1. Cellulose Extraction. (e chemical compositions of SCB E2
at the beginning are 42.40% of cellulose, 25.20% of hemi-
cellulose, and 19.70% of lignin, 3.01% of ash and 9.69% of E1

Intensity (a.u.)
extractives as raw materials in this study. (is result is in
good harmony with the work of Bruna et al. reported that D
42.20% of cellulose, 27.60% of hemicellulose, 21.60% of C
lignin, 2.84% of ash, and 5.83% of extractives [42]. (e
chemical composition of the SCB after dewaxed with a 1:1
ratio of ethanol to water mixture, boiled, washed, and dried B
was 58.86% of cellulose, 18.79% of hemicellulose, 17.60% of
A
lignin, and 2.25% of ash. (e yields of the cellulose extracted
from the SCB after treatment with NaOH-alkali were 15 20 25 30
73.57%, hemicellulose 17.225%, and lignin 9.075%. (e 2θ (Degree)
content of cellulose in the sample through the dilute acid
Figure 4: XRD pattern of extracted cellulose for (A) untreated, (B)
pretreatment stage was 82.73% and the hemicellulose and
dewaxing, (C) alkali, (D) dilute acidic, (E1) first bleaching, and (E2)
lignin components were obtained with a minimum amount second bleaching-treated sugarcane bagasse.
of 9.21% and 7.955%, respectively, where concentration of
diluted sulfuric acid was 0.50%, extraction temperature was
100°C, and extraction time was 15 minutes. After first-step Table 4: Crystallinity index of the samples.
bleaching treatment, we obtained the cellulose extracted Sample Crystallinity index (%)
from the sugarcane bagasse with a maximum expected yield A 23.68
of 86.86% and the hemicellulose and lignin components B 24.82
were obtained in a minimum amount of 7.89% and 5.01%, C 26.03
respectively, using with an acidified NaOCl concentration of D 26.34
1.00% by weight, a reaction time of 5:00 hours, and a re- E1 29.23
action temperature of 75°C. (e result of cellulose content in E2 31.63
the sample through the second step bleaching treatment
were 89.76%, and hemicellulose and lignin components were
extracted at the lowest levels of 6.15% and 2.66%, 83.03%, 86.86%, and 89.76% when the sample is untreated,
respectively. dewaxed, alkali-treated, dilute H2SO4-treated, first bleaching
treatment, and second bleaching treatment, respectively.
(e result shows CI and cellulose content has direct
3.2. X-ray Diffraction (XRD). In all the samples, the dif- relationship, which was in a very good agreement with the
fraction peaks are observed around 2θ � 15.3 and 22.7°. (ese work of Morais et al. reported a perfect linear relationship
peaks are characteristic peaks of cellulose I, designated by the between the CI and cellulose content [44].
(100) and (002) planes [43], as clearly observed in Figure 4. It has been reported that crystallinity is one of the most
Table 4 shows the crystallinity index of cellulose. (e CI powerful factors in the efficiency of enzymatic hydrolysis for
for the untreated (A) SCB is 23.68%, while the CI for the the reason that giant crystallinity of cellulose makes the
treated cellulose materials shown increment with a value of biomass unreachable to enzymatic attack [45, 46]. (e
24.82%, 26.03%, 26.34%, 29.23%, and 31.63% in the treat- crystallinity of cellulose derived from inter- and intra-
ment of dewaxing (B), alkali, dilute H2SO4 (C), first-step molecular hydrogen bonding between cellulose chains and
bleaching (E1), and second-step bleaching (E2), respectively. can be modified using biomass pretreatment technologies
(is is due to the increment of cellulose contain in the [47, 48]. Determining the cellulosic crystallinity of modified
treated materials with values of 42.4%, 58.86%, 73.71%, solids is not simple; however, because lignocellulosic
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6 Advances in Materials Science and Engineering

biomass consists of disordered cellulose and various non- Figure 5(d). From Figure 5 (E2), the produced cellulose
crystalline compounds such as hemicellulose and lignin [49]. fibers are evenly distributed and their average width is about
From the findings, it was concluded that the fraction- 12.06 μm. (erefore, the surface morphology produces the
ation based on the five-step process modifies the chemical higher quality cellulose exhibited by cellulosic products have
bonding, the structure, and the crystallinity of the cellulosic to fulfill the following treatment stages: dewaxing, alkaline,
materials, but exclusively by the significant elimination of dilute acid, first stage, and second stage bleaching processes.
lignin since delignification contributes to increasing the Figure 6 demonstrates the reduction of average diameter
crystallinity of the reclaimed materials. of cellulose, conforming the removal of waxes, lignin, and
hemicelluloses, as the sample treatment continuous to dif-
ferent chemicals and methods, the noncellulosic compo-
3.3. Scanning Electron Microscope Analysis. (e SEM image nents are gradually decreased to process defibrillation,
of cellulose extracted from untreated (A) sample and resulting in a reduction in diameter.
extracted through dewaxing stage (B), alkaline stage (C),
dilute acidic stage (D), first bleaching stage (E1), and second
bleaching stage (E12) process are shown in Figure 5. 3.4. Fourier-Transform Infrared (FTIR) Spectroscopy.
(ere are significant changes in the morphological Figure 7(a) and 7(b) shows the FTIR spectra of the cellulose
structure of cellulose that occurred in treated SCB samples extracted from sugarcane bagasse. All spectra showed a band
compared to untreated SCB samples due to the removal or in the range 3530–3050 cm−1, which is ascribed to the free
lesser amount of noncellulose components such as pectin, OH stretching vibration of the −OH group of the intermolecular
lignin, and hemicellulose. and intramolecular hydrogen bonds in the cellulose molecules
Figure 5(a) shows the surface morphology of untreated [45]. (e spectra in Figure 7(b) manifested an absorption band
SCB with an average cellulosic diameter of 35.23 μm sur- around 902 cm−1 due to glycosidic C-H stretching vibration in
rounded with residual materials and firmly bound together cellulose molecules, representing β-glycosidic bonds and the
in a stack, which could be because of the existence of the wax noncrystalline portion of the cellulose [46]. (e FTIR spectrum
layer and intact lignocellulosic parts [43, 44]. SEM images of of lignin and hemicellulose indicated by peaks in the wave
the deparaffinized cellulose shown in Figure 5(b) have an number around 1515 and 1732 cm−1 have been related to the
average cellulose diameter of 28.41 μm after removal of C�C aromatic skeletal vibration of the aromatic ring in lignin
waxes as well as dirt, dust, soil, pith, sugar extracts, and such and the C�O stretching vibration of hemicellulose and lignin in
water-soluble impurities. (ere are significant differences the structure, respectively [47, 48]. However, the various peaks
between cellulose treated through alkaline, shown in associated with hemicellulose and lignin in addition to the C-H
Figure 5(c) compared to cellulose that was treated through curvature of the hemicellulose and lignin structures and to the
acid hydrolysis as shown in Figure 5(d)). Based on C�C vibration of the aromatic ring of lignin around 1437 cm−1
Figure 5(c), the distribution of celluloses appeared uniform [49] as well as the peak at 1249 cm−1 attributed to out-of-plane
with an average diameter of 24.35 μm, while the alkaline- C-O-C stretches of aryl alkyl ethers in lignin [50] decreased and
treated samples followed by acid hydrolysis produced cel- almost completely disappeared in some spectra after treatment
lulose with an average cellulose diameter of 17.44 μm and of cellulose fibers (Figure 7(b)). (is was due to the reduction of
quite a large number of long rod-like structures, as shown in hemicellulose and lignin after alkaline, dilute acid, and bleaching

10 12
8 10
6 8
6
4 4
Number of Cellulose Radius (Count)
Number of Cellulose Radius (Count)

2 2
0 0
0 10 20 30 40 50 60 0 10 20 30 40 50 60
10 10
8 8
6 6
4 4
2 2
0 0
0 10 20 30 40 50 60 0 10 20 30 40 50 60
10 14
8 12
10
6 8
4 6
4
2 2
0 0
0 10 20 30 40 50 60 0 10 20 30 40 50 60
Cellulose Diameter (μm) Cellulose Diameter (μm)

Figure 5: SEM micrographs of cellulose extracted from sugarcane bagasse.

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Advances in Materials Science and Engineering 7

treatments [51]. (ese spectra were not observed in the E2 3.5. >ermal Analysis. (e thermogravimetric analysis
cellulosic fibers with the exception of the peak around 902 cm−1 (TGA) and differential thermal analysis (DTA) curves of the
which characterizes the cellulosic structure. (e outcome of the cellulose extracted by the different techniques are shown in
spectra illustrates the chemical treatment getting rid of most of Figure 8. (e thermogram showed the different stages
the lignin and hemicellulose. (represented by a circle in Figure 8) of degradation that takes
place in the cellulose due to the differences in degradation
temperature of each component of the cellulose. As shown in
40 Figure 8(a), the initial decomposition happened at tem-
perature between 60 and 150°C due to the evaporation of
Average Cellulose

35
Diameter (μm)

30 water molecules and low molecular weight components that

25 were broken down [52].
20 (e studied cellulosic fibers became thermally stable in
15 the range of 220–310°C, which is associated with the onset of
10 thermal degradation of cellulosic materials [53]. As shown in
A B C D E1 E2 Figure 8(a), the TGA curve of all samples A, B, C, D, E1, and
Type of Treatment E2 started to decay at 232, 264, 268, 302, 310, and 312°C,
Figure 6: Average diameter of cellulose extracted from sugarcane respectively. (e decomposition temperature at 0% weight
bagasse. loss for the examined samples was 347, 347.2, 360.7, 382.4,
2898 cmʹ
3347 cmʹ

E2

E1

D
Transmittance (%)

4000 3500 3000 2500 2000 1500 1000 500

Wave number (cm-1)
902
1049

E2
1372

E1
1317

D
Transmittance (a.u)

C
1437

A
1600
1739

1520

1249

2000 1500 1000 500

Wave number (cm-1)

Figure 7: (a, b) FTIR spectra of the extraction of cellulose from sugarcane bagasse.
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8 Advances in Materials Science and Engineering

Table 5: (e onset thermal decomposition (Ton ) and the maximum

100 (a)
thermal decomposition (Tmax ) of all samples as collected from the
(I) (II) DTA curve.
80
(III) sample Ton (°C) Weight loss (%) Tmax (°C) Weight loss (%)
60
Weight (%)

A 310 24.56 345 48.33

B 318 15.04 348 47.51
40
C 320 13.25 352 34.04
20 D 321 6.10 353 19.79
E1 324 4.31 344 7.30
0 E2 328 3.42 352 10.00

-20
(b)
(II)
-1.5 thermal stability reported in related studies such as Arzu
et al. [55]. (e main thermal decomposition took place at
Derivative (wt(%))

350–600°C. A similar result has also been obtained by other

-1.0 researchers where cellulose acetate undergoes a strong
degradation between 330°C and 450°C [55].
-0.5
(III) 4. Conclusion
(I)

0.0
Cellulose was efficiently extracted from sugarcane bagasse
through a five-step process. (is study showed that a large
100 200 300 400 500 600 700 amount of hemicellulose and lignin was removed with
Temperature (°C) optimal solutions of alkaline hydrogen peroxide (AHP) at
A C E1 pH 11–12.5 under the conditions of the bleaching process
B D E2 that allow for maximum cellulose yield, which has been
confirmed by FTIR spectra. As a result of SEM analysis, the
Figure 8: (a) (e thermogravimetric analysis and (b) the differ-
ential thermal analysis curves of cellulose extracted from the dif- average diameter of cellulose was 12.06 μm. TGA and XRD
ferent methods. analysis showed that cellulose is thermally stable and has the
highest crystallinity index of 31.63%. (erefore, the applied
procedures are successful for getting to the appropriate
443.5, and 494.7°C, respectively. (is was consistent with the properties of cellulose. (e cellulose will be highly recom-
fact that as the purity of cellulose increased, its thermal mended for use as fillers for polymeric composites.
stability also increased. It is the result of the pyrolytic de-
composition of the cellulose acetate polymer chain followed Data Availability
by deacetylation as well as the removal of the less stable
lignin and hemicellulose polymer from the SCB during (e data used to support the findings of this study are in-
treatment processes [54]. (e thermograph showed the cluded within the article.
different stages of temperature degradation of each com-
ponent of the cellulose, which are marked with a circle in the Conflicts of Interest
figure. (e temperature at which a 50% weight loss occurred
for E1 and E2 cellulose was evident in the third stage or (e authors declare that they have no conflicts of interest.
phase of degradation. Table 5 shows the onset of thermal
decay (Ton ) and the maximum thermal decay (Tmax ) of all Acknowledgments
samples taken from the DTA curve (Figure 8(b)).
(e decomposition temperature of Sample-B with (e authors would like to acknowledge the support provided
Tmax �348°C is higher than that of Sample-A with 345°C by by the Faculty of Materials Science and Engineering at the
3°C, but Sample-A showed higher weight losses than Jimma Institute of Technology.
Sample-B as tabulated in Table 5. (is is due to the reduction
of the content of hemicellulose and lignin after the dewaxing Supplementary Materials
pretreatment process. (e Ton of dewaxed cellulose in-
creased from 310 to 318°C, while cellulose-B increased Supporting Information (SI) contains the experimental
slightly from 318 to 320, 321, 324, and 328°C for cellulose-C, section and additional information regarding the three
cellulose-D, cellulose-E1, and cellulose-E2. In general, all optimized predicted solutions of the General Factorial
samples show an increase in trend Tmax , while they show a quadratic model design matrix for NaOH-alkali treatment
decrease in weight loss. (is corresponds to the fact that and dilute sulfuric acid treatment conditions with experi-
thermal stability of cellulose is directly proportional to its mental values of response variables. (Supplementary
purity. (is work’s thermal stability is better than the Materials)
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Advances in Materials Science and Engineering 9

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