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Fibers and Polymers 2016, Vol.17, No.

5, 687-694 ISSN 1229-9197 (print version)


DOI 10.1007/s12221-016-5416-0 ISSN 1875-0052 (electronic version)

Extraction of Natural Cellulosic Fibers from Cornhusk and Its


Physico-Chemical Properties
Nishant Kambli1,2, Shantanu Basak2, Kartick K. Samanta2,3, and Rajendra R. Deshmukh1*
1
Department of Physics, Institute of Chemical Technology, Mumbai 400019, India
2
Institute of Chemical Technology, Matunga, Mumbai, Mumbai 400019, India
3
Chemical and Bio-chemical Processing Division, ICAR-National Institute of Research on Jute and Allied Fiber Technology,
Kolkata 700040, India
(Received May 29, 2015; Revised March 5, 2016; Accepted April 17, 2016)

Abstract: A natural long staple ligno-cellulosic fibers have been extracted from the cornhusks using an alkali treatment.
Physico-chemical properties such as chemical composition, length, fineness, crystallinity, surface properties, etc. measured by
standard methods are reported in this paper. The physico-chemical and morphological properties of the extracted cornhusk
fibers are discussed in detail and compared with other cellulosic like cotton and ligno-cellulosic fibers such as jute. Scanning
electron microscopy was used to study the morphological and cross-sectional view and energy dispersive X-ray and FTIR
were used for the identification and quantification of elements, groups present in the cornhusk and other cellulosic and ligno-
cellulosic fibers. In addition, fibers are characterized by thermo-gravimetric analysis. Results showed that morphological and
physico-chemical behavior is more or less similar to other multicellular ligno-cellulosic fibers like jute.
Keywords: Cornhusk fibers, Physico-chemical properties, Ligno-cellulosic fibers, XRD, SEM

Introduction prepared yarns by blending cornhusk fibers with cotton fiber


and polyester fiber for getting more strength, and adequate
Ligno-cellulosic fibers are being utilized in various areas elongation [7]. However, physico-chemical, cross-sectional,
like building, packaging, home textile, home furnishing thermal characterization of cornhusk fiber is still not reported
purpose, etc. From last few decades, various natural ligno- deeply in the literature. Here, in this paper we have extracted
cellulosic fibers like flax, sisal, jute, kenaf, hemp have been and characterized the cornhusk fibers thoroughly using
playing a major concern in fiber research domain. However, various techniques such as SEM, AFM, EDX, FTIR, and
there is a tremendous scope on research on agricultural waste TGA and compared it with other two valuable common
materials like wheat and rice straw, cornhusk, pineapple, cellulosic and ligno-cellulosic fibers, cotton and jute.
banana fibers [1-3]. Study on these underutilized fibers will
not only support the rural community by value addition of Experimental
these waste products, but also be helpful as far as the
environment friendliness is concerned. Materials
Among all the above mentioned agricultural waste Cornhusks (Maize Cob Sheaths), collected from local
materials, a very limited research work has been carried out market, Mumbai, India, were used for the fiber extraction.
on extraction and characterization of cornhusk fibers [1,4-6]. Cornhusks were peeled from maize cobs. The collected
Cornhusk fiber, a multicellular long length ligno-cellulosic cornhusks were manually cleaned to remove foreign materials,
fiber, is available around 9 million tons every year in the followed by air drying and were subjected to cellulosic fiber
world fiber market [6]. It is the second largest source of extraction. For the experiment, sodium hydroxide (98 %,
natural fibers preceded by cotton and followed by jute. Merck Specialties Private Limited, India) was used.
As cornhusk fiber is the cheapest source of natural
cellulosic fiber, it has great potential to be used as apparel Procedure for Fiber Extraction
and value added unique products like carpets, rugs, cordage, Experiments were carried out to standardize the suitable
etc., making purpose depending on the staple length of the conditions for extraction of fibers from cornhusks. The
fiber. Fibers extracted from cornhusk also have potential for experiments were carried out for 60 min at four different
high value textile applications and have better processibility temperature levels viz. 100, 120, 140, and 160 oC by using
than natural fibers extracted from other agricultural byproducts 10 % w/w concentrations of sodium hydroxide (as an alkali
such as pineapple and banana leaves [4]. Besides, the material for degumming and releasing the fibers from
process of the fiber extraction from cornhusk requires less cornhusks) 5 g/l with the material:liquor ratio of 1:20. The
energy, and is eco-friendly compared to the regenerated and extracted fibers were washed thoroughly in tap water to
the synthetic fiber production process. Researchers have also remove the dissolved substances. The extracted fibers were
then neutralized with dilute acetic acid 0.1 % (w/v), rinsed
*Corresponding author: rr.deshmukh@ictmumbai.edu.in with water and finally dried under ambient condition.

687
688 Fibers and Polymers 2016, Vol.17, No.5 Nishant Kambli et al.

Fiber Composition Determination of Ash Content


The fiber compositions like lignin content, cellulose The ash content was determined using ASTM (E 1755-01)
content, hemicellulose content, etc., were determined using test method by heating the sample in a muffle furnace. Test
Halliwell’s method [8]. It gives the percentage of components specimen of about 5 g was placed in a tared silica crucible
present in the fiber. According to this, cornhusk fibers were and weighed accurately. The specimen in the crucible was
extracted with petroleum ether in a Soxhlet apparatus for then ignited over a Bunsen flame until it was carbonized.
6 h, and then boiled with 0.5 % ammonium oxalate solution The crucible was then transferred to a muffle furnace and the
to remove lipids from the fibers. Most of the lignin was ashing was continued at 575±25 oC, until it attained a
removed by bleaching with 1.0 % sodium chlorite solution constant weight. The oven dry weight of the material taken
in 0.05 N acetic acid in a boiling water bath for 1 h. This for ashing was found by measuring the moisture content in
residue was treated with 5.0 % and then with 24.0 % KOH the sample through a separate experiment (as mentioned in
which removed hemicellulose. Finally, the residue was moisture determination method). From the weights so
treated with 20-fold volume of phosphoric acid (90.0 %) for measured, the percentage ash content was determined on the
2 h at 1 oC (iced bath), washed with 1.0 % Na2CO3, and then original dry weight basis.
washed with water till pH becomes neutral to obtain pure
cellulose percentage. Determination of Moisture Content
Moisture content of the fibers was determined according
Fiber Length, Diameter, and Fineness to ASTM (D 2495-01) test method. A fiber sample of 2 g (A)
Fiber length was directly measured by using calibrated was taken in a tared weighing bottle. It was dried in an oven
scale. Fiber diameter was measured by using optical for 2 h at 105±3 oC and then cooled in desiccator. The
microscope (Nikon) fitted with 10× objective. stopper was momentarily opened to equalize the air pressure
and weighed again. Once again the bottle was returned to the
Determination of Crystallinity oven for 1 h, cooling and weighing and this action was
The degree of crystallinity of cornhusk fibers was determined repeated for successive hourly periods until a constant
using the X-ray diffractometry technique (Philips PW 1877). weight (B) was obtained. The moisture content (%) was
calculated using the formula:
Tensile Properties
The tensile tests of the fibers, i.e., tenacity, elongation, Moisture content (%) = [(A − B)/A] × 100
modulus of rigidity, and work of rupture were performed
using a vertical table top Instron tensile testing machine Determination of Moisture Regain
(INSTRON-4400R) according to ASTM (D 2654) test Moisture regain of the fibers was determined according to
methods. The fibers were cut into about 6 cm length. The ASTM D 2654-89a. The samples were dried in an oven at
test was carried out at a cross head speed 18 mm/min and the 105 oC for 4 h and then allowed to absorb water vapour
gauge length was 25 mm. The relative humidity of 65 % and under standard test conditions (21 oC and 65 % relative
temperature of 21 oC was maintained throughout the testing. humidity) for 24 h. The moisture regain was calculated as
The measurement was taken for minimum of 100 fibers. the ratio of the amount of water vapour absorbed to the dry
weight of the sample.
Linear Mass Density
Linear density was determined using ASTM (D 1577-96) FTIR Spectroscopy
test methods by weighing a predefined length of the fibers. The FTIR spectroscopy was used to determine the
functional groups and chemical structure of cornhusk fibers.
Determination of Absorbency It was carried out on a Shimadzu IR Prestige 21 analyzer.
The absorbency was determined using IS (2369-1967) test Cornhusk fiber powder (0.5 mg) was mixed with 200 mg
method. 1 g of test specimen collected from ten different KBr (spectroscopy grade, 200 mesh dried at 110 oC for 2 h
portions of extracted fibers was used for the absorbency test. and stored in desiccators) and pelletized in a KBr press, with
Before performing test, the sample was conditioned for 24 h a pressure of approximately 8 tons to form transparent
at 27 oC and the relative humidity of 65 %. This condition 13 mm diameter pellets. Similarly, IR pellets were prepared
was maintained throughout the testing. The conditioned 1 g for the other fibers. Degassing was performed to eliminate
of fiber was placed on the surface of water with a pair of air and moisture from the KBr powder. FTIR was recorded
forceps. The stop-watch was started when the test specimen in the range of 500 to 4500 cm-1.
touched the surface of water and the stop-watch was stopped
when the test specimen sank under the surface of water. This EDX Analysis
time interval was noted. The same experiment was repeated EDX analysis of cornhusk, cotton, and jute samples was
ten times. The average time in seconds was calculated. carried out in a Field Emission Gun Scanning Electron
Extraction of Fibers from Cornhusk and Its Properties Fibers and Polymers 2016, Vol.17, No.5 689

Microscope (FEG-SEM) to determine the quantity of the 100 oC is insufficient for extraction of fibers from cornhusk,
elements present on the fiber surface and expressed in whereas the cornhusk fibers extracted from 100 g cornhusks
atomic and weight percent. at 120, 140, and 160 oC are 32.01, 23.02, and 22.953 g
respectively. However, cornhusk fibers extracted at higher
Morphological Structure temperatures (140 and 160 oC) is brownish in nature and
The morphological structure of the fibers and its cross very harsh and brittle as depicted in Figure 1(B) and (C). It
section were studied using a scanning electron microscope may be due to the removal of lignin present in the cornhusk
(SEM), Philips XL-30, with an accelerating voltage of fiber. Therefore, further technical experiments were carried
12 kV. Each sample was coated with a thin layer of conducting out with the yellowish cornhusk fibers extracted at 120 oC,
material (gold/palladium) using a sputter coater before SEM as shown in Figure 1(A). Some part of extracted fibers were
measurement. further bleached with 6 % hydrogen peroxide (H2O2) to
impart whiteness to the fibers. The bleaching process was
TG Analysis in N2 Atmosphere carried out for 60 min at 85 oC using 1 g/l concentrations of
Thermogravimetry measures the gradual weight loss of a sodium hydroxide (NaOH) with the material:liquor ratio of
sample with respect to time at a constant heating rate. The 1:20. NaOH is used to bring the pH up to 9-10 because H2O2
TG curves of the cornhusk fibers were obtained using a becomes active at this pH. High pH and temperature lead to
thermogravimetric analyzer (METTLER TOLEDO TG-50/ the faster decomposition of peroxide bleaching liquor and
MT5) in a nitrogen atmosphere with 2 ml/min flow rate and degradation of cellulose. To overcome this problem sodium
a constant heating rate of 10 oC/min. silicate (1.5 g/l) is used as a stabilizer to control or regulate
these effects.
AFM Analysis of Cornhusk Fiber Cornhusk fiber extraction parameters such as % weight
The AFM analysis of cornhusk fiber was carried out using loss and % fibers recovered are given in Table 1. It was
an Innova AFM (Veeco, Santa Barbara, CA, US) equipped found from the table that at 10 % NaOH with 120 oC is an
with a 90 μm scanner. A cornhusk fiber was placed onto a ideal condition for the extraction of the cornhusk fibers.
freshly cleaved mica surface and air dried. All images were
obtained using a tapping mode at room temperature. The Properties and Fiber Composition
silicon nitride cantilever with a spring constant of 40 Nm-1 Fiber composition affects appearance, structure, properties,
was used. The scan rate of 1.0 Hz and 512 lines per 5 μm and processability of the fiber. The composition and properties
was used for optimum contrast. No filtering was used during of the extracted cornhusk fibers are evaluated and compared
scanning. with cellulosic cotton and ligno-cellulosic jute fiber (Table
2). The parameters of cotton and jute fibers reported here in
Results and Discussion Table 2 for comparison purpose are taken from the literatures
[9,10]. The cornhusk fiber contains 50-55 % cellulose,
Fiber Extraction whereas cotton and jute fibers contain around 85-90 and 51-
Different experiments were carried out to standardize the 72 % cellulose, respectively. Lignin, the binding substituents
suitable conditions for extraction of fibers from cornhusks. which hold the individual cells together, is present in jute
The experiments were carried out for 60 min at four different and cornhusk fibers. As far as the crystallinity is concerned,
temperature levels viz. 100, 120, 140, and 160 oC using 10 % cornhusk fiber is less crystalline (56.9 %) than the cellulosic
w/w concentrations of sodium hydroxide (as an alkali cotton fiber, which might be due to the presence of more
material for degumming and releasing the fibers from amorphous hemi-cellulose and lignin in it. The crystallinity
cornhusks) 5 g/l with the material:liquor ratio of 1:20. As far of cornhusk fiber is comparable with that of jute fiber.
as the extraction temperature is concerned, it was found that Crystallinity of cornhusk fiber has been confirmed by X-ray

Figure 1. Cornhusk fibers extracted from cornhusks at (A) 120 oC, (B) 140 oC, and (C) 160 oC and (D) extracted at 120 oC and bleached.
690 Fibers and Polymers 2016, Vol.17, No.5 Nishant Kambli et al.

Table 1. Extraction of the cornhusk fiber at different temperatures and alkali concentrations
NaOH (%) on Temperature % wt. loss of
Sr. no. % fibers recovered Remarks
wt. of fibers (oC) cornhusk
1 7 120 - - Non extractable
2 8 120 - - Non extractable
3 9 120 65.0 35.0 Extractable
4 10 120 68.0 32.0 Extractable (good quality)
5 7 140 - - Non extractable
6 8 140 69.1 30.9 Extractable
7 9 140 69.9 30.1 Extractable
8 10 140 77.0 23.0 Extractable
9 7 160 66.5 33.5 Extractable
10 8 160 70.8 29.2 Extractable
11 9 160 70.9 29.1 Extractable
12 10 160 77.0 23.0 Extractable
Note: M:L=1:20, wetting agent=1 g/lit, incubation period=1 hr.

Table 2. Fiber composition and properties of cornhusk fiber and its comparison with other fibers
Sr. no. Parameters Cornhusk Jute Cotton
1 Length (mm) 40-180 150-360 10-35
2 Diameter (µm) 130-140 (33.0) 15-25 11-22
3 Lignin (%) 7.5 5-13 0
4 Cellulose content (%) 50-55 51-72 85-90
5 Hemicellulose content (%) 39.39 12-20.4 4-6
6 Holocellulose content (%) 89.72 - -
7 Crystallinity (%) 56.9 50-55 65-70
8 Tenacity (g/den) 1.3 (30.6) 4-5 3-5
9 Elongation (%) 19.7 (31.1) 0.9-1.2 5-10
10 Modulus of rigidity (g/den) 128.9 (24.7) 180-200 50-60
11 Work of rupture (g·cm/den) 0.39 (26.3) 0.03 0.11
12 Linear mass density (tex) 29.7 1.25-5 0.1-0.3
13 Absorbency (sec) 0.92 Absorbent Absorbent
14 Ash content (%) 1.16 0.9-1.1 1.1-1.8
15 Moisture content (%) 11.4 12-14 6-8
16 Moisture regain (%) 12.9 13.8 7.0-8.5
Note: Figures in the parenthesis indicate C.V. (%).

diffraction represented in Figure 2. Because of less presence of encrusting substances that give cornhusk a
crystallinity as compared to cotton fibers, cornhusk fiber is rough and irregular appearance. On the contrary, grey ligno-
more accessible to water, dyes, and other finishing chemicals. cellulosic jute and banana fibers showed comparatively
In regards to fineness cornhusk fiber is coarser than cotton smooth, regular surface appearance. Cotton fibers showed
and jute fibers. The diameter of the cornhusk fiber is also even cleaner and smoother surfaces. Non-cellulosic material
larger than cotton and jute fibers. present at the fiber surfaces may be responsible for this kind
of morphological observations. Those encrusting non-
SEM Analysis cellulosic substances may be carbon based, which has been
SEM images of the chemically extracted cornhusk fiber further confirmed by EDX analysis in the later part of this
showed rough, distorted, honeycomb nest like cellular paper. As far as the morphology of the cross-sectional view
structure with the presence of small micropits on the fiber of the cornhusk fiber (Figure 4(A1)) is concerned, it showed
surface as depicted in Figure 3(A). It may be due to the central hollow regions like banana fiber. This hollow regions
Extraction of Fibers from Cornhusk and Its Properties Fibers and Polymers 2016, Vol.17, No.5 691

help to reduce the bulk density of the cornhusk fiber and


make it suitable for composite and thermal insulator materials
[5]. However, other ligno-cellulosic fibers like jute and coir
do not contain any lumen like hollow spongy appearance in
cross-sectional morphology, whereas cellulosic cotton fiber
showed kidney bean shaped appearances.

FTIR Analysis
FTIR spectra of cornhusk, jute, and cotton fibers were
recorded to understand the chemical groups present in each
fiber (Figure 5). FTIR spectra of cornhusk and cotton fibers
(Figure 5(A) and (C)) show a broad absorption band around
3200-3498 cm-1 corresponding to the OH stretching of
hydroxyl group of cellulose. However, jute contains less
amount of hydroxyl groups as seen in Figure 5(B). Peak
Figure 2. X-ray diffraction pattern of the extracted cornhusk corresponding to the CH stretching at 2875 cm-1 is more
fibers. intense in cotton and cornhusk fibers, which may be due to

Figure 3. SEM images of (A) cornhusk, (B) jute, (C) cotton, (D) banana, and (E) coir fiber.

Figure 4. Surface morphology of the cross-section of (A1) cornhusk, (B1) jute, (C1) cotton, (D1) banana, and (E1) coir fiber.
692 Fibers and Polymers 2016, Vol.17, No.5 Nishant Kambli et al.

the presence of more cellulosic -CH2OH groups, whereas the EDX Analysis
broad peak at 1650 cm-1 is attributed to the C=O stretching EDX analysis of chemically extracted cornhusk fibers,
of the carbonyl group present in it and the 1425 cm-1 peak is ligno-cellulosic jute and cellulosic cotton fibers is given in
assigned to CH2 symmetric bending. However, the peak at Table 3. It showed that chemically extracted cornhusk fibers
1425 cm-1 is more prominent in case of cotton fiber, which contain almost 62 % weight of carbon, which is more than
may be because of more cellulose content. The absorption the jute fiber and cotton fiber. It may be due to the presence
peak at 1637 cm-1 is due to the anti-symmetric deformation of more non-cellulosic materials in the cornhusk fiber. On
of C-O-C band in cellulose and hemi-cellulose. It is more the other hand amount of oxygen present is around 36 %,
prominent in cornhusk and cotton fibers, but less prominent which is less than the jute and the cotton fiber. However
in jute fiber. Since the two peaks (1650 and 1637 cm-1) are after bleaching both carbon and oxygen weight percentage
very close, we get a sharp and broad peak due to combined (%) was reduced by 7.8 % and 9.1 % respectively. It might
effect of C=O groups and C-O-C groups. The broad peak be due to the removal of lignin and other non-cellulosic
around 1050 cm-1 is due to C-O and O-H stretching found in materials during bleaching. Further extracted cornhusk fiber
all the fibers, whereas the shoulder peak at 1000 cm-1 found also contain magnesium, silicon, calcium elements, which is
in case of cornhusk fiber is interpreted as C-O-C stretching not present in jute and the cotton fibers. These elements
at the β (1-4) glycoside linkage of cellulose. come from the non-cellulosic cell wall material of the
cornhusk fibers.

AFM Analysis of the Cornhusk Fiber


AFM analysis helps us to measure the surface texture
parameters of the fiber quantitatively. The surface of the
cornhusk fiber contains irregular non-uniform ups and
downs as shown in Figure 6(A), whereas the jute fiber
surface is comparatively smoother as shown in Figure 6(B).
In general cotton fibers are smooth [11]. It means that ligno-
cellulosic cornhusk fiber surface is rougher compared to the
cellulosic cotton fiber. As far as the quantitative measure of
the roughness is concerned, cornhusk fiber showed average
roughness of 189.74 nm and RMS roughness of 250.46 nm,
whereas for jute fiber these values are 84.3 nm and 109.2 nm
respectively. Canetta et al. have reported average roughness
of 76 nm and RMS roughness 156 nm for cotton fiber [11].
Thus cellulosic cotton fiber is smoother as compared to the
other two ligno-cellulosic fibers. Therefore it is clear that
Figure 5. FTIR spectra of (A) cornhusk, (B) jute, and (C) cotton cornhusk fibers are coarse as compared to other two fibers.
fiber. Regarding the roughness value, henequen fiber (77 %

Table 3. Atomic and weight percentage of cornhusk, jute and cotton fibers using EDX
Cornhusk fiber (A) Jute fiber (B) Cotton fiber (C)
Elements
Weight (%) Atomic (%) Weight (%) Atomic (%) Weight (%) Atomic (%)
C 62.54 69.17 55.68 62.72 46.1 53.2
O 36.80 30.56 43.89 37.11 53.9 46.8
Na 0 0 0 0 0 0
Mg 0.13 0.07 0 0 0 0
Al 0 0 0 0 0 0
Si 0.20 0.10 0.11 0.06 0 0
P 0 0 0 0 0 0
Cl 0 0 0 0 0 0
K 0 0 0 0 0 0
Ca 0.33 0.11 0 0 0 0
S 0 0 0.18 0.08 0 0
Extraction of Fibers from Cornhusk and Its Properties Fibers and Polymers 2016, Vol.17, No.5 693

surface may be responsible for more roughness.

TGA Analysis
TGA curves of cotton, jute, extracted cornhusk, and
bleached cornhusk fibers are represented in Figure 7. It was
observed from the Figure 7 that the TG curve of the cotton
fiber (C) showed sharp fall at 370 oC and less amount of char
mass remained at higher temperature, whereas jute and
cornhusk fibers showed fall at 350 oC ((B) and (A)), but here
the rate of fall, i.e., the weight loss rate is lower compared to
the only cellulosic cotton fiber. This particular temperature is
reported as pyrolysis or decomposition temperature of the
cellulose. It means that lignin and non-cellulosic matter
present in jute and cornhusk fibers are responsible for
lowering down the pyrolysis, i.e., (decomposition) temperature
compared to the cotton fiber by 20 oC. Another interesting
observation from the Figure 7 is that the amount of char
mass remained at higher temperature is slightly lower in
case of jute fiber than cornhusk fiber, this might be due to
less amount of lignin present in the jute fiber.
Figure 6. AFM images of (A) cornhusk and (B) jute fibers.
Conclusion

Cornhusk fibers are the only fibers obtained from the by-
product of a food crop with large availability and low cost. It
has low crystallinity and rough surface with hollow cross-
sectional view like ligno-cellulosic banana fibers, which
makes it suitable for more chemical and dye absorption.
SEM topography of the cornhusk fiber showed rough,
encrusting surface due to the presence of non-cellulosic
materials. As far as the thermal stability and chemical
composition is concerned, it showed almost similar properties
like jute. As far as the strength of the cornhusk fiber is
concerned, it showed less tensile strength and more elongation
than jute and cotton fibers.

Acknowledgement

The authors would like to acknowledge the support from


the Institute of Chemical Technology (ICT), Mumbai and
Central Institute for Research on Cotton Technology (CIRCOT),
Mumbai, ICAR. Thanks are also expressed to the staff
members of CIRCOT for their help to carry out various
characterizations of cornhusk fibers.

Figure 7. Thermogravimetric curves of cotton (C), jute (B), References


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