Hindawi

Advances in Materials Science and Engineering

Volume 2022, Article ID 7163359, 13 pages
https://doi.org/10.1155/2022/7163359

Research Article
Chemical Composition and Extraction of Micro Crystalline
Cellulose from Outer Skin Isolated Coffee Husk

Nehemiah Mengistu Zeleke ,1 Devendra Kumar Sinha ,1 and Getinet Asrat Mengesha 2

1
School of Mechanical, Chemical and Materials Engineering, Department of Mechanical Engineering, ASTU, Adama, Ethiopia
2
School of Mechanical, Chemical and Materials Engineering, Department of Materials Science and Engineering, ASTU,
Adama, Ethiopia

Correspondence should be addressed to Devendra Kumar Sinha; devendrasinhame@astu.edu.et

Received 14 October 2022; Revised 21 November 2022; Accepted 29 November 2022; Published 13 December 2022

Academic Editor: Sheraz Ahmad

Copyright © 2022 Nehemiah Mengistu Zeleke et al. Tis 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.
Cofee husk (CH) is a sustainable and abundantly available cellulosic waste material. Its fber consists of cellulose as the major
structural part which leads to potential utilization for the manufacturing of microcrystalline cellulose (MCC) products that can be
utilized for diferent industrial applications. In the present study, chemical composition of outer skin-isolated cofee husk was
determined and sequential treatments of various untreated (UT) sample, ethanol—toluene treated sample through dewaxed (DW)
treatment, sodium hydroxide (NaOH)—treated sample through alkali (AT) treatment, and sulfuric acid (H2SO4)—treated sample
through bleaching (BL) treatment have been carried out. Te Micro Crystalline Cellulose (MCC) has been extracted through
hydrogen peroxide (H2O2) after BL treatment. Te BL treatment for MCC extraction process was conducted without chlorine and
additional harsh acid treatment, respectively. Te characterization of chemically treated samples was carried out to investigate
their morphological, physico-chemistry, and thermal behavior through a scanning electron microscope (SEM), Fourier transform
infrared—ray (FTIR), X-ray difraction (XRD), thermo gravimetric analysis (TGA), and diferential temperature analyzer (DTA).
From the chemical composition analysis; the cellulose, hemicellulose, lignin, and extractive content were determined and its
values were (52.9%), (12.5%), (24.3%), and (9.4%), respectively. In the morphological examination, the great untreated (UT) fber
sample was greatly reduced into a micro-sized BL sample, revealing that (from FTIR analysis) the lignin and hemicellulose
contents were greatly removed during chemical treatments and the presence of a micro crystalline cellulose region with 54.7%
yield. Also, the sample AT and BL showed the lowest amorphous region in X-RD due to the removal of hemicellulose and lignin.
Te highest crystallinity index has been determined for the BL sample, i.e., 89.9%. Additionally, the thermal analysis shows that the
AT and BL sample has great thermal stability than other (UT and DW) samples at high temperature. Terefore, the outer skin
separated cofee husk was prepared from agricultural waste was subjected to eco-friendly chemical treatments to yield MCC. Tus,
the extracted MCC is expected to be reliable for replacing other plant materials for the production of crystalline nanomaterial and
reinforcing constituent for the fabrication of bio composite.

1. Introduction million of 60 kg bags per year [4]. Basically two varieties of

Cofee is one of the most widely held commercial commodities
next to petroleum [1]. Ethiopia is the frst in Africa and sixth of
the globe’s largest producers and exporters of cofee [2], and a
large amount is consumed by local consumers [3]. Currently,
according to the International Cofee Organization report, over
2.3 billion cups of cofee are used up every day across the world,
and the world’s cofee yield has reached an average of 171.9
cofee called as Robusta and Arabica are responsible to support
100% production in the world. Tey vary typically in their
chemical constituents, and on the other hand, produce com-
parable volumes of waste [5]. Cofee cherry produces 30–50%
cofee husk based on the processing method [6]. Currently, an
estimated 400,000 to 550,000 metric tons of cofee has been
produced per year in Ethiopia [7]. Among these, more than
100,000 tons are estimated to be cofee husks [8, 9].
2 Advances in Materials Science and Engineering
Cofee husk is the cofee industry residue that is pro-
duced during the dry processing method [10], which con-
tains cellulose, hemicellulose, and lignin in unlike
proportions based on the geographical location and cofee
hulling process [11]. Te efects of these diferent conditions
afect the chemical composition and physical properties of
natural fbers [12]. Additionally, the cafeine and tannins
contents, which are toxic in nature of this waste are disposed
of by the environment and contaminate the land and rivers
[13]. Furthermore, they are not used for animal food because
of tannins which are considered as antinutritional com-
pounds and other applications in Ethiopia [14]. So, due to
disposal problems and lack of reutilization, these husks are
traditionally burned in the felds leading to pollution or
smoke which is identifed as the cause of major health-
hazardous [15]. Cofee wastes can be made up of husks, pulp
and skin, cofee parchment, cofee mucilage, cofee silver
skin, and spent cofee grounds [16]. Studies are under
progress on the reprocessing of these by-products of cofee
industries as these are important for environmental friendly
motives and for the hopeful real purpose of this enormous
extent of lignocellulose material. In processing, the cofee
parchment and pulp separation are dissimilar in wet and dry
processing. In wet processing, the pulp and outer skin are
removed from cherries, and parchment is removed after
drying. However, in the dry processing, the dried green
cofee cherries and the skins (outer skin, pulp, and parch-
ment) are isolated in a single process.
Enormous natural materials have received increased
attention from the research community due to their
properties, including rice husk [17], cotton products [18],
bagasse [19], and wastes of oil palm fruit [20], peanut hulls
[21], and wheat straw [22]. Te literature reveals that the use
of these natural resources is sustainable for countries with
sufcient amount. Ethiopia has various agricultural residues
such as wheat, barley, tef, maize, chat, sugarcane, enset, and
cofee. Tese wastes are mainly exploitable for energy
consumption in the country [9] and other reutilization areas
further require investigations. Te residues of these crops
have a high environmental impact and health hazards due to
poor disposable problems. Te demands are increasing for
wood based products, including cellulose, MCC, wood-
based reinforcing material, and their composite products for
various industries such as medical and automotive. Cellulose
is a highly crystalline and ordered structure which forms
strong material with excellent properties [23]. Its derivative
MCC is a microsized and tasteless naturally available sub-
stance found from purifed and partially depolymerized
cellulose. Due to its exceptional properties such as biode-
gradability, chemical inactivity, high surface area for
bonding with resins, high sorption, absence of toxicity, and
great hygroscopicity, MCC has gained attention for various
applications such as cosmetics, pharmaceutical, bio com-
posite reinforcement, and beverage[24, 25]. Te extraction
techniques for MCC particles are several including me-
chanical treatment, biological treatment, and chemical
treatment. Among these techniques, chemical treatment
(e.g. acid hydrolysis) is the conventional method for ex-
traction of MCC [26]. Te stringent environmental
protocols concerning the utilization of protected forests
drive the investigation of cellulose, MCC, wood-based
reinforcing materials, and their composite products from
agricultural residues to satisfy the demand of the industries.
Terefore, to lessen deforestation and utilize efciently
agricultural residues (wastes), overlooking available re-
newable resources ofers the commercial product through
the production process. Interestingly, few researchers have
focused on the use of agricultural residues to extract cel-
lulose and fber to fabricate paper, paperboard, and bio
composite materials. Additionally, researchers have inves-
tigated agricultural residues, such as wheat straw [27],
peanut hull [21], and rice husk [28], in the fabrication of
particleboard, fbers, biomass energy, and composite ma-
terial. Till now, numerous studies on diferent areas of cofee
industry residues/cofee husk have been reported for various
industrial applications. Some of the recently reported re-
search works are presented in Table 1. From Table 1, it is
palpable that cofee industry residues can yield diferent
products and compounds.
Te previous literature reveals that there is almost no
report on the extraction of MCC and chemical composition
analysis from outer skin-isolated cofee husk. Te current
study has been conducted to systematically determine the
potential of outer skin-isolated cofee husk fber for sup-
plementing environmental protection and health. Te major
objective of this research is to explore the chemical com-
position and potential of microcrystalline cellulose extracted
from outer skin-isolated cofee husks through a modifed
user-friendly procedure for industrial utilization. Te re-
sultant microcrystalline cellulose properties were studied in
terms of structure, morphology, crystallinity, and thermal
stability.
2. Materials and Methods
2.1. Materials. Cofee husk fbers were collected from bale
zone Dello Menna, the southern part of Ethiopia, in the form
of short fber, in 2022. Te reagents used were toluene,
ethanol, sodium hydroxide, hydrogen peroxide, and sulfuric
acid. All reagents were purchased from techno tech, Addis
Ababa, Ethiopia, and were used without further purifcation.
2.2. Preparation of Samples. From the collected cofee husk
fber part, the pulp and parchment were separated from the
outer skin via strip (manually). Te cofee husk (pulp and
parchment) isolated from the outer skin was washed away
with distilled water and dried up in an oven at 70°C intended
for 2 days, then cooled in a desiccator for 30 minutes to
prevent moisture absorption of the fber. Finally, it was
crushed with a grinding machine and put through a sieve
using a sieve dimension of 2 mm. Figure 1 confrms the
collected cofee husk, outer skin-isolated cofee husk, and
sieved outer skin-isolated cofee husk.
2.3. Chemical Composition Analysis. Te chemical compo-
sition investigation of the lignocellulosic components
present in the outer skin isolated cofee husk fbers was
Advances in Materials Science and Engineering 3

Table 1: Recently reported research work conducted on cofee industry residues.

Materials
Cofee silver skin
Parchment
CH/thermoplastic starch flms
Spent cofee ground/poly (vinyl alcohol)
CH/starch/polylactid acid
CH/polypropylene
Ground cofee waste/oxobiodegradable
high density polyethylene
CH/linear low-density polyethylene
CH/poly lactid acid
Cofee husk/polybutylene adipate
terephthalate
Cofee hull/high-density polyethylene
CH/high-density polyethylene
Objective Application Reference
Bio-nanocomposite flm development
Nanocellulose extraction [29]
for food packaging
Micro fbrillated cellulose extraction Composite reinforcement [30]
Composite development Food packaging material [31]
Composite flm development — [32]
Termoplastic starch composite flm
Food packaging [33]
development
Building materials (roofng and ceiling
Bio-based composite development [34]
tile)
Internal automotive parts and
Composite material development [35]
lightweight furniture
Polymer composite material
— [36]
development
Rigid packaging (food tray, cups and
Green composite material development [37]
containers)
Development of polybutylene adipate Substitute neat poly butylene adipate
[38]
terephthalate composite terephthalate
High-density polyethylene composite — [39]
Polyethylene composite — [40]

(a) (b) (c)

Figure 1: (a) Waste cofee husk. (b) Outer skin isolated waste cofee husk (cofee pulp and parchment). (c) Ground outer skin isolated cofee
husk.

carried out in three steps, which follow the conventional Wi − Wf

methods of the Technical Association of Pulp and Paper
Industry (TAPPI) and standards which involves an ana-
lytical approach (gravimetric method) to fnd extractive,
hemicellulose, lignin, and cellulose contents. For a piece of
sample, three replicates were conducted to determine the
average value. Tis step was then followed for microcrys-
talline cellulose extraction.
Step 1. Te extractive content was investigated through the
TAPPI standard technique (T-264 om-82) [30]. In a Soxhlet
extraction, about 20 g of dry outer skin isolated cofee husk
was added to a beaker flled with 750 mL of the solution
combination (1 : 1, ethanol: toluene). Te extract was col-
lected and placed in an oven at 110°C with the aim of drying
up for precede weighing. Tis extractive-free dried cofee
husk was considered as a base for the subsequent processes.
Te yield of extractive was determined by expression (1).
% of Extractives � x 100, (1)
Wi
where Wi —is the weight (gm) of oven-dried sample before
extraction and Wf —is the weight (gm) of the oven-dried
sample after soxhlet.
Step 2. Te content of the lignin sample was calculated by
putting in the residue in a sulfuric acid solvent of 72% as
per TAPPI approach (T-222 om-83) methodology [41].
About 3 gram of extraction-free sample was immersed in
a beaker, to the 51 mL of sulfuric acid (72%) solvent was
placed, rigorously stirred in electromagnetic stirrer at
room temperature for 8 hours. Ten, this hydrolyzed
sample was washed away using distilled water till the PH
became neutral and was dehydrated in an oven for 3 hours
at 105°C. Te lignin content was determined by expres-
sion (2).
4 Advances in Materials Science and Engineering
Wi − WL
% of Lignin � x 100,
Wi
where wi is the weight of oven-dried sample before ex-
traction and wL is the weight of oven-dried sample after
extraction.
Step 3. Te content of hemicellulose was studied according
to the technique broadly mentioned in the literature [42].
Extraction process was carried out using 4 gm extractive-free
and dehydrated sample which were placed in a 200 mL
boiling fask at a ratio of 20/1 (liquid/solids) by the use of
10% NaOH solvent for 24 h at room temperature with
stirring. Te extracted samples were washed away by dis-
tilled water until the pH was neutral and dried up in an oven
for 3 h at 110°C. Te yield of the extracted hemicellulose was
determined by expression (3).
Wi − Wb
% of Hemicellulose � x 100,
Wi
where Wi is the weight of the oven-dried sample before
extraction and Wb is the weight of the oven-dried sample
after extraction.
Ten, the cellulose percentage was calculated by
% Cellulose � 100 − (% hemicellulose + % lignin + % extractive).
2.4. Micro Crystalline Cellulose Extraction and Yield. Te
extraction and yield of microcrystalline cellulose were car-
ried out using chlorine fully and a harsh acid-free extraction
procedure, which was proposed according to the method
reported by Khenblouche et al. [43] with minor modifca-
tion; the method overcomes the environmental impacts. Te
process is taken out with chemical treatment with execution
in dewaxing (removal of extractives), alkali, and bleaching
treatment procedures.
2.5. Dewaxing. It was carried out to remove tannins, sugars,
fatty acids, wax, and extractives from powder material (outer
skin separated cofee husk) using toluene-ethanol (2 : 1, v/v)
in a Soxhlet setup at 65°C for 8 hours as per TAPPI standard
(T264 om-97). After dewaxing, the sample was dried in an
oven at 50°C for 2 days and then cooled in a desiccator to
take away traces of residual reagents and moisture
absorption.
2.6. Alkali Treatment. It was performed for an extractive-
free (dewaxed) sample to remove hemicellulose and insig-
nifcant amount of lignin. It was done at 70°C for 4 hours
with electromagnetic stirring using a 7 wt% NaOH with an
extractive-free sample to solvent ratio of 1 : 10. Tis action
was conducted twice, and after a piece of action, the sample
was fltered and washed away with distilled water till the pH
became neutral. Finally, the sample was dried at 80°C for 24
hours in an oven.
2.7. Bleaching. For the removal of lignin and remaining
(2) amount of hemicelluloses, extracting MCC was carried out
with the dewaxed and alkali-treated sample placed in sul-
furic acid (7 wt%) solvent for 3 h at room temperature under
stirring with 1 : 20 fber to liquid ratio (g/mL). Further
purifed cellulose was treated with hydrogen peroxide
(H2O2) solvent (11%, v/v), and the pH was tuned to 11 by 8
wt% NaOH. Te solution was forcefully agitated constantly
for 4 hours at 50°C temperature and a 1 : 25 sample to a
solvent ratio. Te microcrystalline cellulose sample obtained
from this bleaching process was fltered and washed away
with distilled water till the pH reaches neutral. Te treatment
of each process is carried out twice in the same settings and
weighed for taking the sample yield. Te outer skin-isolated
CH, MCC extraction, and chemical composition analysis has
been illustrated in Figure 2.
2.8. Fourier Transform IR-Spectroscopy. Infrared spectros-
(3) copy investigation was carried out to obtain the existence of
chemical variations which occurred in the intended (UT,
DW, AT, and BL) samples. Te peaks were obtained with
Jasco FT/IR-6600typeA analyzer (Easton, Maryland, USA),
at scanning speed of 2 mm/sec in the range of
400–4000 cm− 1 (standard) and 4 cm− 1 resolution.
(4) 2.9. X-Ray Difraction (XRD). Te XRD pattern of untreated
and chemically treated samples was recorded using MAX-
ima_X XRD-7000 X-ray Difractometer (Japan) with Cu Kα
radiation. Te X-ray was operated at 30 mA and 40 kV with a
scan rate of 3 min− 1 and in the range of 5 –60 . Te crys-
tallinity index (CI) was investigated by the XRD amorphous
subtraction method developed by Ruland for the frst time
and states the ratio of the sum of areas under the peaks of the
crystalline component Icry to the overall area under all peaks
Itot [44].
Icry
crystalline index(%) � x 100. (5)
Itot
2.10. Scanning Electron Microscope (SEM). Surface mor-
phology of cofee husk-derived cellulose and microcrystal-
line cellulose was observed through JOEL, JCM-6000 plus
scanning electron microscope (JOEL Ltd., Tokyo, Japan),
operating under 10 KV accelerating voltage.
2.11. Termo Gravimetric (TG) and Diferential Termal (DT)
Analyzer. Te thermal endurances of the samples were
carried out using BJHENVEN thermo gravimetric analyzer,
HCT-1 model. For analysis, the samples were heated be-
tween 0 and 500°C under a nitrogen atmosphere at 10°C/
min.
2.12. Determination of Average Molecular Weight and Degree
of Polymerization. Te average degree of polymerization,
DP, of extracted MCC was determined by the viscometry
method at 25°C in 6 wt% NaOH/4 wt% urea solvent using
Advances in Materials Science and Engineering
Coffee husk Strip
Outer skin isolated CH
MCC Extraction
Dewaxing (toluene/ethanol)
Alkali treatment (NaOH)
Bleaching (H2SO4 and H2O2)
Figure 2: Schematic diagram of MCC extraction and chemical composition of outer skin-isolated cofee husk.
Ostwald viscometer [45, 46]. Te fow time was recorded and
relative viscosity, ηr , was determined based on recorded fow
time (ratios of time fow of extracted MCC solution and
CED solvent). Ten, intrinsic viscosity, η, was determined
according to the following equation in cm3 g− 1 . Te result
shows an average of three measurements.
η − 1
log􏼔 r 􏼕 � log[η] + 0.13[η]C, (6)
C
where C is solution concentration of the sample in gmL− 1 .
Average degree of polymerization was then determined
from the following formula:
DP0.905 � 0.75[η].
3. Results and Discussion
3.1. FTIR and Chemical Composition. Te chemical com-
position of outer skin-isolated cofee husk was determined
using the gravimetric method and was determined to be
9.4% extractives, 12.5% hemicellulose, 24.3% lignin, and
52.9% of cellulose yield. Tis yield value is higher than the
cellulose yield of wheat straw (32.5%) [47], cofee husk
(24.5%) [48], and parchment (22%) [30] and lower than the
yield values of cellulose extracted from cofee husk through
chlorine-based extraction techniques (61.8%) [49] reported
in the literature. Furthermore, the yield value is comparable
to yield values of cellulose extracted from bagasse (55.2%)
[50] and kenaf fber (53%) [51]. Te obtained cellulose from
outer skin isolated CH is compared with other renewable
source and has been summarized in Table 2 and Figure 3
which shows diferent samples of outer skin-isolated cofee
husk in order to determine their chemical composition and
changes.
3.2. FTIR. Infrared spectroscopy is a simple technique used
to obtain information continually on chemical changes that
takes place throughout chemical treatments. Figure 4 shows
5
Grinding Ground outer skin isolated CH
Chemical
Composition
% of extractives
(toluene/ethanol)
% of lignin (H2SO4)
% of hemicellulose (NaOH)
the IR spectra of untreated (UT) sample (a), dewaxed sample
(b), alkali-treated sample (c), and bleached sample (d).
Table 3 exhibits all IR spectra of detected peaks and their
representations.
FTIR analysis shows UT sample and DW sample spectra
exhibited matching absorption bands. Te spectra at
1030 cm− 1 shows the O–H and C–O stretching vibration of
polysaccharide occurred in cellulose, and the peak at
1630 cm− 1 is may be caused by water absorption of the
samples [58]. Te spectrum at 1739 cm− 1 is a typical be-
havior of the carbonyl C�O stretching of the uronic ester
and acetyl groups of polysaccharides. It is moreover as-
(7) sociated to the p-coumaric acids of hemicellulose or/and
lignin [59], and the removal of this spectra after continuous
chemical treatments shows the elimination of excessive
content of hemicellulose and lignin from the samples.
Additional sign of hemicellulose and lignin elimination
through the treatment is the substantial reduction in the
absorption of the small spectra at 1220 cm− 1 which is as-
sociated to the C-O stretching of the aryl group in
hemicellulose and lignin. A small spectra exhibited at
1430 cm− 1 can be associated to the CH2 symmetric bending
of cellulose [57]. Te absorption in the range of
3600–3100 cm− 1 is associated to the O–H stretching vi-
bration and hydrogen bonds of the hydroxyl groups. Te
absorption at 2920 cm− 1 is a typical characteristic of the
C–H stretching frequency in cellulose [57]. Furthermore,
typical FTIR spectra of AT sample shown in Figure 4 ex-
hibits the peaks observed at 1516 cm− 1 which are associated
to aromatic ring stretching frequencies of lignin [59]. Te
alkali treatment removes this peak apparently from the
cellulose so that these spectra was eliminated from the AT
sample spectrum. Te absorption at 3440 cm− 1 is correlated
to the –OH stretching vibration of cellulose [60]. Te
cellulose did not show the absorption band located at
1739 cm− 1, which is a typical behavior of the stretching
vibration of C�O and C-O. Te alkali treatment removed
these groups from the spectra.
6 Advances in Materials Science and Engineering

Table 2: Cellulose obtained from diferent renewable sources.

S. No. Renewable source Cellulose content (%) Reference
1 Wheat straw 32.5 [47]
2 Cofee husk 24.5 [30]
3 Parchment 22 [30]
4 Bagasse 46 [50]
5 Kenaf 53 [51, 52]
6 Giant reed 35.52 [53]
7 Jute 60 [54]
8 Sisal 73.5 [52]

(a) (b) (c) (d) (e)

Figure 3: (a) Untreated sample. (b) Extractive free sample. (c) Alkali-treated sample. (d) Bleached sample. (e) Acid-treated sample (to
determine the lignin content).

250
BL

200

898
AT
Trasmittance (%)

150

DW
100

UT
50
1141
1030
1220
3440

2920

1430
1739

1516
1630

0
4000 3500 3000 2500 2000 1500 1000
Wavelength (cm ) -1

Figure 4: Infrared spectra of UT, DW, AT, and BL samples.

Finally, the FTIR spectra of BL sample shown in Figure 4
shows the delignifcation process of sample and further
extraction of MCC. In this spectra, the elimination of almost
the remaining lignin was proven by the removal of peak at
1516 cm− 1, and the peak band around 3440 and 2920 cm− 1 is
related with the characteristic values of purifed cellulose and
the broadened peak and sharp peaks in the BL sample
implying enhanced cellulose content and increasingly ex-
posed cellulose content in the sample [60]. In addition, the
spectra around 1430 cm− 1 are connected to the crystallinity
of cellulose and are related to CH2 symmetric stretching.
Additionally, the spectra at 898 matching to the C–O–C
pyranose ring skeletal stretch, β-glycosidic bond stretch, and
C–H asymmetric deformation [61]. Tis peak appearance on
Advances in Materials Science and Engineering 7

Table 3: Te IR spectra of detected peaks and their representations.

Wave number (cm− 1) Spectra Represents Reference
1030 All C-O-C pyranose ring skeletal vibration [43]
1141 BL C-O-C stretching at the b-(1⟶4)-glycosidic linkages [55, 56]
1220 UT C–O stretching of the aryl group in hemicellulose and lignin. [56]
1430 AT, BL C-H bond of cellulose [57]
1516 UT, DW C-C aromatic ring stretching vibrations of lignin [55]
1630 AT, BL OH bending of the absorbed water [58]
1739 UT, DW C�O stretching in hemicellulose [59]
2920 AT, BL C-H stretching [57]
3440 AT, BL -OH groups stretching of cellulose [60]

9000

22.2

44.0
16.12

7500

34.6
BL
6000
Intensity (a.u)

4500

AT
3000

DW
1500

UT
0
10 20 30 40 50 60
2θ (Degree)
Figure 5: X-ray difraction pattern of untreated (UT), dewaxed (DW), alkali-treated (AT), and bleached (BL) sample of outer skin isolated
cofee husk.

Table 4: Crystalline index of UT, DW, AT, and BL samples.

Sample Te total area of crystalline peaks Areas of all peaks Crystalline index (CI %)
UT 5207.2 7462.2 69.7
DW 6611.9 8667.5 76.2
AT 6386.1 7863.2 81.2
BL 8394.4 9328.3 89.9

the BL sample spectra confrms the breaking of cellulose
chains and extraction of MCC.
3.3. X-Ray Difraction Measurements. It is an important
method to characterize the structure of crystalline material.
Figure 5 represents the XRD patterns of chemically-un-
treated and treated outer skin-isolated cofee husk samples.
Te samples showed outstanding peaks around 16.7°, 22.4°,
34.6°, and 44.1°, which match all peaks with standard dif-
fraction data (JCPDS Card Number: 00-003-0192) that
corresponds to the crystallographic plane of (110), (200),
(004), and (100) [55, 62]. Tis JCPDS Card Number: 00-003-
0192 refers to coated cellulose-II type structure, and these
planes reveal that each cellulose sample has a cellulose type
structure [63], and the bleached (BL) sample shows coated
cellulose-II type structure. Te peak observed at 16.12° was
related to the cellulose crystals domain, and it has increased
intensity for alkali-treated (AT) and bleached (BL) samples.
It was suggested that the two-cycle NaOH—alkali treatment
and H2SO4 and H2O2—based bleaching processes promote
highly ordered coated cellulose-II crystallites in outer skin-
isolated cofee husk through improving intra and inter-
molecular hydrogen bonding. Te peak 22.2° 34.6 and 44.0
8 Advances in Materials Science and Engineering
were observed to be sharpened gradually and also had high
intensity for both ATand BL samples as compared to UTand
DW samples. Tis was likely due to the alkali treatment and
bleaching processes that removed residual compounds and
produced coated cellulose-II crystalline structure with 54.7%
yield. Accordingly, the highest crystalline index of cellulose
possessed 89.9% with the BL sample, followed by the AT
with 81.2%, DW with 76.2%, and lastly UT with 69.7% as
shown in Table 4. Tus, the outer skin-isolated cofee husk-
bleached sample could ofer it as a promising agent in bio
composite reinforcement application.
3.4. Morphological Properties of Chemically Untreated (UT)
and Treated (DW, AT, and BL) Samples. Figure 6 exhibits
SEM micrograph of CH fber subjected to dewaxing, alka-
line, and bleaching treatment. Figures 6(a) and 6(b) show the
feature of any typical lignocellulosic fber characteristics
which clearly shows surface impurities. Te dewaxed sample
Figure 6(b) further exhibits the microfbers in pack form
more densely with a rough surface, and the alkali-treated
sample in Figure 6(c) exhibits less dense microfbers with a
smooth surface, and fbers try to isolate each other. Tis
indicates partial hemicellulose, lignin, and surface impurity
removal at this stage, while the smooth structure of cellulose
was still preserved [50]. Te two-cycle bleaching process in
Figure 6(d) causes the fber to split into isolated cellulose
microcrystalline. According to reported pieces of literature,
the acidic attack disintegrates the cellulose structure into
individual small microcrystalline size, and penetration of
acidic ions into the inner part of fber could depolymerize
the cellulose by degrading the amorphous regions [60]. Te
chemically-treated cellulose microcrystalline average di-
ameters are about 2-3 μm but the exact length is difcult to
determine. Te reduction in diameter refers to the disap-
pearance of hemicellulose, lignin, and other impurities [64].
Tis extracted CH cellulose microcrystalline is less in di-
ameter than those extracted from various sources such as
sisal [65], coconut [66], and wheat straw [67] with diferent
extraction methods which uses harsh acid and chlorine-
based extraction methods.
3.5. Termal Stability. Figures 7(a) and 7(b) exhibit the
TGA and DTA curve, respectively, and environmentally
friendly chemical treated and untreated outer skin-sepa-
rated cofee husk samples. Initially, all samples, mainly UT
and DW samples, demonstrated a decreased weight curve
in the range of 30–135°C, which is a typical characteristic of
adsorption of water and disappearance of constituents of
low molar mass [68]. However, AT and BL samples showed
increase in the same way with a fattened curve, and the
weight loss was also relatively low. Tis was probably
caused by water adsorption of the high amount of cellulose
content in both samples. Consequently, AT and BL samples
exhibit higher decomposition temperatures than UT and
DW samples for the reason of the existence of micro-
crystalline cellulose structure that increases the thermal
endurance of samples from high temperatures [63]. Te
second range 135–250°C is associated with the degradation
of hemicellulose which contains numerous saccharide types
that form amorphous structures and thermally less stable
lignocellulosic components [30]. Te third range
250–375°C corresponds to a portion of hemicellulose and
cellulose. Cellulose is a highly crystalline and ordered
structure that forms strong material with thermal stability
[69]. Finally, the degradation takes place at the range of
375–520°C related to lignin, which is more thermally stable
and difcult to degrade [70]. Te DTA curve tries to show a
slight an endothermic reaction at the initial stage of the
curve due to the sample’s dehydration around 100°C, then
undergoes a sharp exothermic reaction between temper-
ature around 270°C–375°C. Te sharp exothermic reaction
at this temperature range indicates the degradation of
cellulose and remaining hemicellulose. Variation in the
structure of cellulose due to heat primarily takes place
through depolymerization (begins at 310°C due to breaking
the chain at 1,4 glycosidic bond), dehydration (occurs at
initial range of degradation temperature, 280°C), and the
formation of Glucosan [71]. Additionally, the exothermic
peak around the temperature of 410°C and above indicates
the release of lignin from the samples. Finally, the curve BL
sample shows that the temperature resistance is highly
relative to other samples. Tis indicates that the two stage
bleaching process highly improves the thermal resistance of
the sample. Te weight loss in each range of the samples is
summarized in Table 5. Te weight loss of sample BL in the
range initial, second, and fnal was lower than other
samples, and in the third range AT sample, the loss was low.
3.6. Average Molecular Weight and Degree of Polymerization.
Te η and extracted MCC average DP was determined to
study the efect of H2O2 treatment on the cellulose
structure. During the frst bleaching cycle using H2SO4, the
η and DP are 901 and 1340, respectively. For the second
bleaching cycle, using H2O2 for preparation of MCC, the η
and DP signifcantly reduced to 365 and 281, respectively.
Tis could be described by the degradation of amorphous
region for the extracted MCC. Te result shows that the
DPs of extracted MCC are in the range (150–300) of
currently available commercial MCC, and the DPs of
extracted MCC higher is than DPs of commercial MCC
i.e.117.2 and MCC extracted from bacterial cellulose has
DP250 [72]. Te molecular weight (Mw) of extracted MCC
from outer skin isolated CH was determined by multi-
plication of DP of extracted MCC with (Mw) of unit cel-
lulose, 162 [73], then the (Mw) of extracted MCC is around
21,300 g/mol. With considering to the plenty of cofee husk
waste material, large scale fabrication of MCC with ade-
quate DP and (Mw) could be realized.
Advances in Materials Science and Engineering 9

(a)

(b)

(c)

(d)

Figure 6: SEM micrograph of untreated (a), dewaxed (b), alkali-treated (c), and bleaching (d) sample of outer skin-isolated cofee husk fber.
10 Advances in Materials Science and Engineering

3.29 %

0.91 %
100

Third range
80

Final range
Second range
Initial range

46.98 %
Mass loss (%)

60

17.94 %
40

20

0
100 200 300 400 500 600
Temperature (°C)

BL DW
AT UT
(a)
50

40

30
DTA (µV)

20

10

100 200 300 400 500 600

Temperature (°C)

BL DW
AT UT
(b)

Figure 7: (a) TGA and (b) DTA curves of UT, DW, AT, and BL samples.
Advances in Materials Science and Engineering
Table 5: Weight loss of the samples at each range.
(%) of weight loss in each ranges UT
Initial range 7.7
Second range 3.4
Tird range 48.0
Final range 20.1
4. Conclusion
In this study, the systematic extraction of MCC from outer
skin-isolated cofee husk was carried out using an envi-
ronmental-friendly extraction method. Te extraction was
conducted efectively by means of the cooperative chemical
treatment method of dewaxing (toluene, ethanol), alkali
(NaOH), bleaching (H2SO4), and chlorine and harsh acid
free—MCC extraction (H2O2). FTIR results showed the
cellulosic structure which refers to the elimination of a
signifcant quantity of hemicellulose and lignin throughout
the chemical treatments. Extracting MCC by means of
weak acid and chlorine-free treatment shows the extraction
process to be environmentally kind with ensuing protec-
tion of harm chemicals. Terefore, this process can be
further realized to other lignocellulosic materials as well.
Te XRD analysis had demonstrated the crystalline
structure of the extracted microcrystalline cellulose, though
TGA ofered clarity in terms of stability in its thermal
property. Te morphological examination confrmed the
rod-shape-like fbers of the separated cellulose, and addi-
tional homogeneity in the structure of microcrystalline
cellulose was realized after the bleaching process. From the
present investigation, it is possible to conclude that outer
skin-isolated cofee husk is excellent source for the fabri-
cation of MCC in abundance with excellent thermal
property and great crystallinity index through this envi-
ronmentally friendly and economically feasible procedure.
Tese extracted MCCs could be reliable for replacing other
plant materials for the production of crystalline nano-
material and for diferent industrial applications such as
hygroscopic agents in cosmetics, fllers, and binders in
medicine formulations, reinforcing elements for the pro-
duction of bio composite for building and automotive
industries.
Data Availability
Te datasets used and/or analyzed during the current study
are available from the corresponding author on reasonable
request.
Conflicts of Interest
Te authors declare that they have no conficts of interest.
Authors’ Contributions
Nehemiah Mengistu: Investigation, writing original draft,
Devendra Kumar Sinha: Writing, review and editing,
Getenet Asrat: Supervision.
11
DW AT BL
6.1 3.5 3.3
4.0 3.4 0.9
60.8 45.2 46.9
26.2 22.3 17.9
Acknowledgments
No funding has been done for this research work.
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