Superficial modification of cellulose microfibers
obtained from sugarcane bagasse, by
silanization
Modificación superficial de micro fibras de celulosa obtenidas a partir de
bagazo de caña de azúcar usando silanización
Fernando Luna Vera, Ph.D 1
Harold Arturo Melo Cortés 2
Claudia Viviana Murcia 3
Italo Charry Galvis 4
1 Colombian PhD Researcher Centro ASTIN- SENA Cali,
Colombia, flna29@misena.edu.co
2 Apprentice Tecnologists Centro ASTIN- SENA Material
Analysis for the Industry Program. Cali, Colombia.
3 Apprentice Tecnologists Centro ASTIN- SENA Material
Analysis for the Industry Program. Cali, Colombia.
4 Apprentice Tecnologists Centro ASTIN- SENA Material
Analysis for the Industry Program. Cali, Colombia.
106
Receipt: 07- 10 - 2014 Accepted: 28-11-2014
Abstract
Water- repellent sugar cane bagasse fibers were produced
after their pretreatment and superficial
modification with hexadecyltrimethosiloxane. Three pretreatments were
studied to carry out delignification, hemicellulose removal and
superficial exposure of cellulose: treatment with 3% hypochlorite (HP),
acetic acid and sodium chlorite mix and an oxidizing solution composed
of hypochlorite-hydrogen peroxide followed by alkaline treatment
(OX-B). The lignine and the hemicellulose were effectively removed
from the bagasse fibers with the OX-B treatment, which yielded
deaggregated fibers of 567 + 115 µm long and an aspect ratio of 32.
Other treatments such as HP yielded less fibers, with reduced length,
297 + 32. The effectiveness of the selected treatment, OX-B, permitted
the obtention of a lignocellulosic material from sugar cane bagasse,
easily modifiable and waterproof, whose characteristics suppose an
advantage as a reinforcement element for polymer-matrix composite
materials.
Keywords: Sugarcane bagasse; silanes; silanization; TGA; FTIR;
hydrophic; Natural fibers.
Introduction
A significant Increase in hydrophobicity of sugar cane bagasse
was Obtained microfiber production Obtained through surface
modification ITS With chain aliphatic silanes. Several delignification
methods of the microfibers, Were Analyzed for Their capacity to
produce fibers With high cellulose content on Their surface, using
vibrational spectroscopy (FTIR), electronic microscopy (SEM) and
thermal degradation behavior (TGA and DSC).
The interest for the treatment and conditioning of fibers dates
back 80 Such years from now, When the
 Moon; Melo; Murcia; Charry. Surface modification of cellulose microfibers Obtained
first composite materials with polymer matrix that used high rigidity and
longitudinal resistance such as boron, carbon, aramide and fiberglass,
which can be used as a reinforcement agent to improve the
mechanical properties of polymers, due to the load transfer that occurs
from the polymer matrix to the fiber (Masuelli, 2013). These materials
have been found in hundreds of structural applications such as
helicopter fuselage parts, boats, space shuttles, sports elements, cars
and even bridges (Mohanty and Drzal, 2002).
There is a great interest exists to Develop and upgrade cost
Characteristics Such as, density, biodegradability and environmental
impact of fiber-reinforced polymers (FRP) (Luz et al., 2007, Vilay et al.,
2008, Ashori, 2008). In parallel, there is a great expectation Also These
upgrades can be since Achieved With the usage of the natural fibers and
the replacement of the commonly used synthetic fibers in FRP's
(Stupenengo, 2011). The Natural fibers offer clear benefits: such as low
density, elasticity modules to like synthetics, low production costs,
renewable ITS generous availability and Their biodegradability. Their use
is strongly supported by National Regional and order Initiatives like the
European Union, Which Demands That All automobiles and the materials
present in them, must be 95% recyclable by 2015.
Keeping this in perspective, innumerable studies have been
conducted on many various natural fibers such as linen, hemp, yute,
coconut fiber, banana, fique, straw, amongst others (Joseph et al., 1996).
Using in the same way, a variety of polymeric matrices in which
polyethylene (Chen, Porter,
1994, Coutinho et al., 1997), polypropylene (La Mantia and Morreale 2007,
Khalil et al., 2000), polystyrene (Khalil et al.,
2000), Polyester resins (Lovely, 2004) and natural rubber (La Mantia
and Morreale, 2011). In spite of its advantages, the use of natural fibers
as reinforcement material contains its own challenges fundamentally by
the presence of water and its high affinity with cellulose. One of them is
the low adhesion to hydrophobic polymers (PE and PP), the other being
the high absorbency of the composite material, making it dimensionally
unstable (Gao et al., 2012). As solution to these limitations, diverse
options are suggested. Mainly, the adhesion of the fibers to the plastic
matrix can be improved using coupling agents which are chemical
precursors that establish a bridge between the polymer matrix and the
cellulosic material, forming covalent chemical bonds or electrostatic
interactions (Kazayawoko et al., 1999).
These bonding agents, Such as maleic acid, can be bonded to
the polymer Directly (polyethylene, MAPE and
from sugarcane bagasse, by silanization
polypropylene, MAPP), which reacts with the -OH groups on the surface
of the fiber, forming stable bonds between the fiber and the polymer
(Mohanty et al., 2002, Gassan y Bledzki, 1997, Karmarkar et al., 2007).
Another approach consists of the bonding of the compatibility agent
directly to the fiber, through a superficial modification that transforms the
hydrophilic nature of cellulose (Xiea et al., 2006). The silanes, that react
the same way with the -OH groups, forming siloxane-type bonds and
freeing the chemical groups that can bond through Van der Waals’
forces or free radicals, created through the high temperatures used in
the compositing process of the material through extrusion (Leu et al.,
2012). The improve in adherence using coupling agents usually results
in higher tensile module values, elasticity modules (MOE) and rupture
(MOR) of the fiberreinforced material in comparison to the polymer
alone (Sobczak et al, 2012, Brugnago et al. 2011).
The sugar cane bagasse is one of the planet's Most
abundant agro-industrial residues, with an annual production of
101 to 340 million tons, worldwide (Huang et al, 2012.); esta
Converts it into a good candidate as a source for natural fibers for
reinforcement of FRP's. Some studies Have Been Reported using
sugar cane bagasse as reinforcement for polypropylene, polyester,
recycled PET, PVC, HIPS and HDPE, using compatibility agents:
such as Aluminates, mercerization (NaOH treatment), Ethylen and
methylacrylate usage as co-polymers and benzyl chloride ( Vilay et
al., 2008, Huang et al. 2012, Corrandini et al. 2009, Benini et al,
2011, Mulinari et al. 2009). However, in our best knowledge, there
is no report of the usage of silanes as compatibility agent on sugar
cane bagasse microfibers,
In this article, the process of sugar cane bagasse microfiber
obtention, sourced from the Valle del Cauca region in Colombia, was
exhibited, using different pretreatments for delignification and the
effective modification of their surfaces using hexadecyltrimethosiloxane
as compatibility agent, with the object of producing a lignocellulosic
material that is potentially useful for the reinforcement of thermal
polymers.
Materials and methods
Reactants
Sodium Hydroxide (NaOH)in pellets, 50% Hydrogen Peroxide
(H 2 O 2), Glacial Acetic Acid(C 2 H 4 O 2 ), Sodium Chlorite (NaClO 2 ), Absolute
Ethanol (C 2 H 6 O). All
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Informador Técnico (Colombia) 78(2): 106-114 July - December 2014

of them were reactant-grade (Merck- Germany). The agitated for an hour, after which it was filtered, taken to neutral pH and
hexadecyltrimethosiloxane, 98% pure, was acquired from Aldrich dried at 50°C until constant weight.
(Aldrich, USA). Sodium Hypochlorite, 5.25% solution, commercially
available as Patojito, Which was Purchased at a local convenience
store. In all cases, the water used came from a Aquelix 5 equipment.
Sugar cane bagasse, fresh from a local Obtained Sugar Cane
Reduction of bagasse fiber size and
processing plant.
granulometry.

The bagasse fibers Obtained from all the pretreatments Were

ground in a bladed grinder grinding in 10 minute batches. The particulate
materials generated from milling was sorted by size for 45 minutes, using

Delignification and pretreatment of the ASTM-grade sift kit, made of stainless steel With No. 400, 325, 270, 200,

bagasse-chlorite With acetic acid solution. 100 and 80 particle caliber.

The sugar cane bagasse was cleaned With distilled water to free
it from impurities. Then it was dried at 60 ° C for 6 hours Until constant
weight was Obtained. Approximately, 13 grams of dry bagasse Were
Surface modification through the process of
submerged in 500 mL of an aqueous solution, composed by 250 mL of
2% Sodium Chlorite and 250 mL of 3M acetic acid. The solution, Along
silanization.
With the bagasse Were kept in agitation at 47 ° C for 2 hours. After
The hydrolysis and condensation of
This, it was filtered with filter paper and washed thoroughly With neutral
hexadecyltrimethosiloxane (HDS) was Conducted in 8: 1.8, water:
pH deionized water was Obtained Until. Then it was dried at 50 ° C Until
ethanol, NaOH 2.5 x 10 -5 M and 2% V / V solution of HDS. This
constant weight.
solution was agitated for 2 hours and then a loaded pistol into a spray.
The solution was misted on the pretreated bagasse fibers in a Manner
That Such all its surface is moist. The fibers Were left to dry at room
temperature and then a 90 ° C to submitted drying for 8 hours.

Delignification and pretreatment of the bagasse with

3% Sodium hypochlorite.
FTIR-based Spectroscopy bagasse
Approximately 100 gm of clean, dry bagasse were treated with
100 mL of 3% W/V Sodium hypochlorite aqueous solution while being
characterization
agitated constantly for 20 minutes. In continuance, the blanched
Infrared spectrums Were Obtained with a Perkin Elmer 1600
bagasse was filtered with a cloth filter and was thoroughly washed
apparatus, Which have to work range spans from 4000 cm That ¹ to 500
with deionized water until neutral pH. Finally, the bagasse was dried
cmˉ¹. The spectrums Were captured in the transmission mode, while
at 50°C until constant weight.
using dry KBr to preparing the sample for the transparent pill format.

Delignification and pretreatment of the bagasse with

bagasse characterization Electronic
OX-B solution.
Scanning Microscopy (SEM)
Approximately 50.0 gm of clean, dry bagasse were submerged in
Micrography was Obtained with a JEOL JCM 50000 Desktop
2000 mL of an oxidizing solution constituted by 1000 mL of 0.5% Sodium
microscope. The high vacuum mode was used and a voltage range
Hypochlorite W/V and 1000 mL of 0.34% V/V Hydrogen Peroxide. The
Between 5 and 15 kV. The samples Were submitted to a gold PVD
bagasse was kept agitated at room temperature for 2 hours, after which it
coating previous to the ESM analysis.
was filtered and thoroughly washed with deionized water until neutral pH.
Next, the bagasse treated with the oxidizing solution was submerged in a
0.6% NaOH solution and kept

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 Moon; Melo; Murcia; Charry. Surface modification of cellulose microfibers Obtained
from sugarcane bagasse, by silanization

Characterization by thermogravimetrical (TGA) and
differential thermal analysis (DTA).
Thermograms from the samples Were Obtained with a TGA /
DSC thermogravimetrical 2 STAR system from Mettler-Toledo. 70 uL
Crucibles Aluminum oxide Were used to Contain the sample Which
1115, 1030 and 895 cmˉ¹ Which corresponden asymmetrical
deformations of CH, CH symmetrical deformations of, asymmetrical
vibrations of COC asymmetric stretching of the glucose ring,
stretching of CO and COC of the
β- glycosidic bond Between glucose molecules (Zhao et al.
2010).

Weighed in at 13 mg. For all the experiments, a non-oxidizing

In contrast, the absorptions around 1510 cmˉ¹ and 1465 cmˉ¹
atmosphere with nitrogen was used with a flow rate of 40 mL / min¹ and
associated to vibrations of the lignine aromatic scaffolding are clearly
20 mL / min¹ of argon gas as purge fluid. The temperature range for the
present in the untreated bagasse sample but disappears after applying
study was from 30 ° C to 600 ° C with a heating rate of 10 ° C / min¹.
all treatments (Zhao et al, 2008). This proves the utility of the methods
used to remove certain amount of lignine. It is interesting to note that
the band associated to absorptions of hemicellulose C=O (xilanes) at
1732 cmˉ¹, is present in all the samples except for the Ox-B treatment.
Results and Analysis This is strong evidence that even though the HP and the CAc
treatments are capable of removing a lignine percentage, they are not
Delignification and production of cellulose microfibers.
as effective in the hemicellulose removal as the Ox-B. Even further, and
directly related with the oxidative power of the treatment, the spectrum
of the Ox-B shows a clear increase in absorption at 1645 cmˉ¹, showing
The objective of reducing the hydrophilic character of the
the increase of the C=O group, probably byproducts of the cellullose’s
microfibers is to minimize its affinity for water, therefore turning them
-OH group.
compatible with the polymer matrix, which is usually hydrophobic.
The fact that both fiber and polymer have a hydrophobic behavior will
allow the matrix to soak the fiber through the extrusion process and
completely fusing the 2 elements, augmenting the possibilities of Additionally, the thermal stability behavior of the samples was
obtaining a true FRM. studied after the diverse treatments. The figures 3A and 3B, reveal the
results of the TGA and DTA analysis, respectively. In the figure 3A, it
can be observed that for all samples, there is a mass loss that starts
With the objective of applying a superficial modification with
approximately at 50°C and occurs with a rate surge (%/ min) at 87°C
silanes to reduce the affinity of the fibers for water, the silanol groups
(first peak in Figure 3B), which is attributed to water loss. After 200°C,
present in the silanes are required to react with the hydroxyl (-OH)
the samples exhibit different behavior. For the untreated bagasse case,
groups present in the sugars that compose the fibers (Figure 1.).
HP and CAc present a second loss of mass between 220°C and 280°C,
However, the natural fibers are coated with a lignine and
with maximum loss rates (%/min) in 280, 240 and 260 °C, for untreated,
hemicellulose film that encapsulates the cellulose inside. In this
HP and CAc respectively. This surge is associated to the rapid
research, 3 different methods were studied in first instance, to
degradation to hemicellulose which occurs at temperatures that are
remove lignine and hemicellulose: Acetic Acid
inferior to those of cellulose (220-315°C), due to its amorphous material
characteristics (Yang et al, 2007).
– Chlorite (Cac), 3% hypochlorite (HP) and an oxidizing mixture,
followed by a basic treatment (Ox-B).

The figure 2 shows the results of the FTIR-based analysis

performed on the sugarcane bagasse fibers after the treatment With
As it was expected, commercially available cellulose does not
ACC, HP and Ox-B, as well as untreated fiber. The findings show the
exhibit this surge but neither does the Ox-B sample, fact that is
marks That around 3400 and 2910 cmˉ¹ cmˉ¹, Which corresponden to
corroborated found with FTIR in which the Ox-B was able to remove
OH and CH stretching, are more visible and intense With all the
virtually all the hemicellulose. A third region between 280°C and 360°C
treatments than the untreated bagasse fibers. This can be Attributed to
shows a large and rapid loss of mass, being these the temperatures of
the Increase in cellulose at the surface exposed after the treatment. It is
maximum loss rate (%/min) and being much more homogeneous
Necessary to observe That the method With the largest increment in
between the samples, with marks at 328°C for HP, 338°C for
mark visibility was Ox-B. The same behavior was found for the typical
commercially available cellulose, Ox-B and CAc and 350°C for the
absorption bands associated With around 1430 Cellulose, 1375,
untreated bagasse. This surge between 315°C and 400°C in DTA is
associated to the cellulose pyrolysis

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Informador Técnico (Colombia) 78(2): 106-114 July - December 2014

(Yang et al, 2007). After 370 ° C, it is Observed That all samples suffer
slow and constant degradation Until the working limits of the apparatus,
550 ° C. It is interesting to observe That the overall mass loss at the end
of the heating cycle Ox-B Have the order (75%)> HP (68%)> untreated
bagasse, CAC (64%). This sequence can be associated to the amount of
lignine still remaining in the different materials Studied, since lignine That
is the Gradients With Material
the highest difficulty; in fact, it does, decomposing slowly between 30 ° C
to 900 ° C, without presence of thermal transitions in DTA (Yang et al,
2007). In This manner, the content of materials lignine With higher would
be the ones With lower mass loss, at the end of the heating cycle, 500 °
C for esta case. This result shows the remaining lignine That are higher
in the samples Treated With CAc than with HP and OX-B.

Figure 1. Silanes With the cellulose fibers interacting surface

after delignification

Figure 2. FTIR Spectrums of the sugar cane fiber and without treatment Figure 3. Thermal analysis of sugarcane bagasse samples Submitted to
With delignify and to remove hemicellulose. The region on Most diverse treatments for hemicellulose and lignine removal. A: Thermo
Significant bands for pretreatment is gravimetrical analysis (TGA) B.
Highlighted in gray. Differential Thermal Analysis (DTA)

110
 Moon; Melo; Murcia; Charry. Surface modification of cellulose microfibers Obtained
The ability of the different treatments studied to degrade
hemicellulose and lignine has a direct relationship with the type of fibers
that can be produced. As the there is higher removal of the substances
that keep the fibers bundled, which are lignine and cellulose, the
liberation of individual fibers is more probable and proper reinforcement
grade characteristics are developed in the fiber, such as a high aspect
ratio. In the figure 4, SEM micrographies corresponding to HP and Ox-B
treatments are shown and were captured from the granulometric
fractions corresponding to fibers that passed through the No. 325 (45
µm pore) and those that did not split with a No. 80 (150 µm pore). The
results show a larger amount of fibers with diameters inferior to 45 µm
with the OX-B treatment than with HP (Figures 5A,B,D,E). The OX-B
fibers are free of amorphous particles similar to barks, which are evident
for the HP case. An observation of the length and diameter of the
produced fibers shows in general that the OX-B method fibers are
longer than the HP method, being 567 ± 115 µm for the first and 296 ±
32 µm for the latter. Regarding diameters, it is possible to calculate
values of 18± 10 µm and 19± 2 µm for OX-B and HP respectively. With
these values, it is possible to estimate the aspect ratio for each group of
fibers which result as 31.5 for OX-B and 15.6 for HP. The literature
reports that the critical aspect ratio is between 10 and 50 (Bigg, 1985).
In fact, this is a good perspective for the obtained fibers, especially for
those obtained with the OX-B method, since it supposes that with such
aspect ratio, there is an ample probability that they are effective as
reinforcement for polymeric matrices.
Salinization of Fibers
The results show that the most efficient method to remove
lignine and hemicellulose was OX-B and consequently is the
treatment with higher cellulose fiber exposure rate. Then the bagasse
treated with OX-B was submitted to superficial modification with HDS,
in the pursue of obtaining hydrophobic vegetal fibers. The
effectiveness of the superficial reaction between cellulose and HDS
was evidenced through FTIR and TGA. The FTIR results (spectrum
not shown in the text), evidence a clear marking at 2850 cm-¹,
corresponding to the C-H stretching of CH2, which is expected due to
that each HDS molecule adds 16 aliphatic carbons to the surface.
Additionally, a notable reduction of the -OH marking at 3408 cm -¹,
fact that is always expected when the HDS reacts with the hydroxyl
groups on the surface. However, there was not a total absence of the
marking, which indicates that
from sugarcane bagasse, by silanization
the modification was not carried out completely on the hydroxyls
available and there were probably cellulose domains that were not
covered by silane. Additionally, the thermal analysis results evidence the
occurrence of the silanization reaction. In first instance, in DTA as well
as TGA, the loss of mass and its water loss related rate surge is clearly
reduced when the fibers are silane treated. (Figure 3A and 3B),
observing a 2% water loss, compared to a 6% of the untreated bagasse.
Additionally, when comparing the thermal degradation profiles, it is
evidenced that the HDS treated bagasse influences positively its
behavior, making the material even more stable. For example, at 400°C,
the material treated only with OX-B presents a a 70% mass loss while
the HDS treated material only lost 58% of its mass. The DTA profiles
(figure 3B) show 3 clear signals of maximum mass loss rates. One
occurs at 280°C that can be associated to the loss of physically
absorbed silanes, that do not react on the surface. At 340°C, a small
surge that occurs at the same temperature than the cellulose
degradation, as well as the other samples but at a much slower rate,
being this completely congruent with the cellulose domains that were not
completely coated with HDS. Finally, at 500°C, one that can correspond
to the degradation of glucose and silanes simultaneously. These results
altogether show that in effect, a superficial reaction on the bagasse has
occurred with the OX-B method. However, an efficiently modified
lignocellulosic material by apolar groups must change its affinity for
water and now should exhibit a clear repellence to it. Figure 5 shows a
photograph in which the HDS modified material (Figure 5A) does not
absorb water. On the contrary, the bagasse treated only with OX-B
absorbs the added water totally. This result is a conclusive evidence
regarding the effectiveness of the method for producing hydrophobic
fibers from sugar cane bagasse and their superficial reaction with
silanes.
conclusions
Three Methodologies Were EVALUATED to perform the
pretreatment, conditioning and production of sugarcane bagasse
microfibers. Through FTIR, TGA and DTA techniques, it was
corroborated That the HP, CAC, and OX-B methods permit the removal
of large Amounts of lignine. It was shown That the only method capable
of completely removing the hemicellulose was the Basic Oxidant, OX-B.
It was shown the type of pretreatment That influences the Characteristics
of the Fibers Obtained. The fibers That Were submitted to OX-B
treatment Were longer, 567 ± 115 microns, than With the HP method,
296 ± 32 microns. In cases Both, the fibers than higher aspect ratios
presented 20. The method OX-B shows a larger capacity to loosen fibers
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Informer Technical (Colombia) 78 (2): 106-114 July - December 2014

individually. Additionally, the surface modification of bagasse fibers
using HDS to replace hydroxyl groups on the surface With 16 Carbon
chains. Product of esta modification, a hydrophobic materials was
Obtained, with a high water repellence. These have all of the
características show That Obtained as a potential reinforcement
materials in polymer based matrix composites, since it contains
lignocellulosic fibers With an adequate aspect ratio and low water
affinity.
This research will be extended in future papers are to determine
the That effectiveness of the materials as reinforcement agent for
polypropylene and polyethylene through the formation of the composite
materials using extrusion and mechanical tests on samples test essay.
Also it is pretended to study further the influence of diverse silanes as
coupling agents and the mass ratio of the composite materials
relationship and Its Effects on end the FRM mechanical properties.

Figure 4. SEM Micrographies of sugarcance bagase, Treated With different methods. A and B
metohod, OX-B, 325 sift. C: OX-B method, 80 sift. D and E, HP method. 80 Sift.

Figure 5. Water absorption essay in sugarcance bagasse fibers Treated With OX-BA
With HDS treatment, B treatment without HDS.

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 Moon; Melo; Murcia; Charry. Surface modification of cellulose microfibers Obtained
Acknowledgements
We thank the generosity of the SENNOVA,
Technological Development, Research and Innovation System for
the development of this research. We also thank the technical
support of the Polymer Analysis Laboratory of the ASTIN center and
the spaces as well as the instrumentation equipment available at the
Red Tecnoparque – Cali node.
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