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TEXTILE FIBER PRODUCED FROM SUGARCANE BAGASSE CELLULOSE: AN

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Textile fiber produced from sugarcane

bagasse cellulose: an agro-industrial residue

International Journal of Textile and Fashion Technology, Chennai, v. 3, n. 2, p. 15-29, jun. 2013
http://www.producao.usp.br/handle/BDPI/45726

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International Journal of Textile and
Fashion Technology (IJTFT)
ISSN 2250-2378
Vol. 3, Issue 2, Jun 2013, 15-28
© TJPRC Pvt. Ltd.

TEXTILE FIBER PRODUCED FROM SUGARCANE BAGASSE CELLULOSE: AN

AGRO-INDUSTRIAL RESIDUE

SIRLENE, M. COSTA1, SILGIA A. COSTA2, RICHARD PAHL3, PRISCILA G. MAZZOLA4,

JOÃO PAULO P. MARCICANO5 &ADALBERTO PESSOA JR6
1,2,5
School of Arts, Sciences and Humanities, Textile and Fashion Course, University of São Paulo, Av. Arlindo Bétio,
1000, Parque Ecológico do Tietê, Ermelino Matarazzo, CEP: 03828-080, São Paulo – SP, Brazil
3
Center for Technical Textiles and Manufactures, Institute for Technological Research of São Paulo State – IPT. Av. Prof.
Almeida Prado 532 Cidade Universitária, CEP: 05508-901 São Paulo/SP –Brazil
4
Faculty of Medical Sciences, University of Campinas, Av. Tessália Vieira de Camargo, 126, Cidade Universitária, CEP:
13081-970 - Campinas, SP – Brazil
6
Department of Biochemical and Pharmaceutical Technology, University of São Paulo, Av. Prof. Lineu Prestes, 580 –
Bloco 16, Cidade Universitária, 05508-000 - São Paulo, Brazil

ABSTRACT

Sugarcane bagasse with and without acid hydrolysis was used for extraction of cellulose. The bagasse pulps
without or with hydrolysis, and commercial mixtures of these materials in different proportions were used for the
production of textile fibers. All sugarcane bagasse pulps were obtained by the alkaline pulping soda-anthraquinone (AQ)
and subjected to chemical bleaching to remove residual lignin using hydrogen peroxide or sodium chloride. Pulps were
used to obtain fibers with N-methylmorpholine-N-oxide (NMMO). Bagasse and pulps were characterized by their chemical
composition. Fibers were analyzed to evaluate maximum water uptake loading or swelling, weight loss and mechanical
properties. Microstructure was analyzed by scanning electron microscope (SEM). The pulping yield was 34.6% for bagasse
without hydrolysis and 26.6% for bagasse with hydrolysis. The fibers showed water uptake capacity in the range of 60 –
86%. Fibers obtained from commercial cellulose and bagasse without hydrolysis and whitened with hydrogen peroxide
had tenacity values of 4.3 cN/tex, which are compatible with commercial lyocell made from wood pulp cellulose.

KEYWORDS: Sugarcane Bagasse, Cellulose, Lyocell, Textile Fibers

INTRODUCTION

In recent years, increasing trends toward a more efficient use of agro-industrial residues have been reported by
[1-5].
different groups Sugarcane bagasse, an abundant agricultural lignocellulosic byproduct, is a fibrous sugarcane stalk
residue.

The annual global production of 800 million tonnes of sugarcane results in 240 million tonnes of bagasse [6].

Brazil is a major producer of sugar cane during the 2012/2013 harvest are expected to be 595.13 million tonnes
[7]
milled to produce sugar and ethanol . When producing alcohol and sugar, cane processing generates different residues
such as bagasse. Sugarcane bagasse is a complex material that consists of approximately 50% of cellulose and
hemicellulose and lignin (25% each) [8, 2, 9, 10].

Despite the wide consumption of bagasse as a fuel for mill boilers, electricity and steam generation, as well as
animal feed, or as a raw material for paper and board manufacture, the residues still remain as a surplus in which poses a
[6].
disposal problem for mill owners This agricultural residue has received increasing attention, since it represents an
16 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,
Joao Paulo P. Marcicano  Adalberto Pessoa Jr

abundant, inexpensive, and readily available source of renewable lignocellulosic biomass for the production of
environmentally-friendly industrial products [8, 11].

Bagasse can also be used as raw material for various types of building boards, production of ethanol and
[12, 10, 5, 13].
polypropylene composites The cellulose component of lignocellulosic materials can be used for production of
textile fibers such as viscose, modal and lyocell [14].

Lyocell fibers are the result of intensive research in the manufacture of unnatural fibers of cellulose originally
different from the traditional ones. The manufacturing process of lyocell fiber is based on an organic solvent spinning
process, making use of N-methylmorpholine N-oxide (NMMO) [15-17]. The solvent NMMO is almost completely recovered
[15-17].
(99.7%) recycled and sent back to the process The reclaimed water is used during the process for washing the fibers
later.

Physical properties of textile fibers, such as dimensions, traction resistance, elastic recovery, electrical resistance
and rigidity, are affected by water uptake. If the fibers are used as units, forming a fabric or a cloth, their humidity plays an
important role to evaluate whether the materials are adequate to a particular purpose [14]. The water-retaining ability can be
especially interesting for some uses, i.e., in sutures, once fibers might be able to absorb secretion from the wound healing
process [18], promoting the scar tissue formation (cicatrization). Other important characteristics for medical applications are
tenacity, softness, biostability and biodegradability [18].

This study aimed to investigate lyocell, a textile fiber made from sugarcane bagasse cellulose with potential
medical and commercial applications. Another study will be conducted using these fibers as support for drug release and
immobilization of enzymes to obtain a technical textile.

Technical textiles have emerged in recent years as an alternative for textile companies from developed countries
that want to reach levels of sustainable growth, escaping the extreme competitive environment that crosses the traditional
textile market. These textile products are used and consumed much more for their performance and functional
characteristics.

MATERIALS AND METHODS

Commercial Cellulose
Cotton linter cellulose, microcrystalline powder, 20µm, pH 5-7 (11 wt.%), Bulk density

0.5g mL-1, α-cellulose. Cat: 31.069-7 of the Sigma-Aldrich.

Sugarcane Bagasse

Sugarcane bagasse (dimensions: approximately 10-60 mm length and 0.4 cm width) was provided by Usina Ester
of Cosmópolis (SP, Brazil). Bagasse was air dried to a final humidity of 10%, passed through a 10-mesh sieve and stored at
4C. The chemical composition of this bagasse consisted of cellulose (43.1%), polyoses (27.6%), insoluble lignin (22.4%),
H2SO4 soluble lignin (1.0%), and ash (2.8%), as demonstrated in Table 1.

Acid Hydrolysis of Sugarcane Bagasse

Acid hydrolysis of the bagasse followed the methodology established by Pessoa-Jr. [19], under the following
conditions: temperature of 121°C, for 10 minutes, using 100 mg of H2SO4 98% for 1 g of bagasse drought: acid solution
ratio of 1:10 (w/v).
Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 17

Soda/AQ Pulping of Bagasse without and with Acid Hydrolysis

Pulping conditions were 16% of Na2O, 0.15% AQ, and liquor: bagasse ratio 12:1 (v/w). Cooking soda was
performed in a 500 mL stainless steel reactor, at 160ºC. The heating time up to 160ºC was previously determined as 1.5 h,
resulting in a total process of 3.5 h. The pulps were washed up to pH 7.0 and filtered, followed by air-drying [20]. The pulp
yield was calculated by equation 1 (dry mass represents the material without humidity):

(1)

In which:

RT = total yield (%); M = bagasse mass (g) (dried base); m = pulp mass after pulping (g) (dried base)

The assay was held in the Center for Technical Textiles and Manufactures – CETIM, Institute for Technological
Research – IPT.

Classification of Sugarcane Bagasse without and with Hydrolysis Pulps

Pulp samples were disaggregated (consistency of approximately 0.3%) in MA - 1032 equipment; afterwards, pulp
suspension was submitted to the Somerville classification, with rift of 0.15 mm. Classified pulps were filtered in a Büchner
funnel and divided into disk samples, at room temperature, to make drying easier. The classification of sugarcane bagasse
whitout and with acid hydrolysis pulps was conducted at laboratories at the Engineering School of Lorena (EEL-USP).

Determination of Classified Pulp Yield

The yield of classified sugarcane bagasse without and with hydrolysis pulps was determined by the difference
between total yield and total rejects. After determining the total yield (equation 1), it was necessary to classify pulps and to
quantify the percentage of rejects, to finally determine the classified pulp yield, which was calculated by equation 2:

(2)

In which: Rc - classified yield (%); RT - total yield (%); tr - percentage of rejects after classification (%) (dried
base); mr - mass of rejects (g) (dried base); M - initial bagasse mass of sugarcane (g) (dried base).

Chemical Analysis of Sugarcane Bagasse without and with Hydrolysis and Pulp
[21]
The modified method standardized by ASTM D 271-48 was used. Samples of 1 g of sugarcane bagasse
without and with hydrolysis and pulp were treated with 5mL H2SO4, 72%. After 7 min of stirring at 45oC, 25 mL of water
was added to the mixture, which was hydrolyzed under 1.05 bars for 30 min. The product was filtered and the insoluble
portion (insoluble lignin) was quantified by weighing. The hydrolysate was acidified to pH 1-3, filtered with a Sep-Pak
C18 cartridge and analyzed by high performance liquid chromatography in a Shimadzu LC10 chromatograph, with an
Aminex HPX-87H column at 45oC. The mobile phase was H2SO4 0.005 mol.L-1 at 0.6mL.min1. The products were
determined by refractive index and quantified by calibration curves [22]. Soluble lignin was determined using the absorption
of alkaline solutions at 280 nm, obtained from the hydrolysate [22, 23].

The concentration of soluble lignin was determined by the following equation:

( 3)
18 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,
Joao Paulo P. Marcicano  Adalberto Pessoa Jr

In which Clig.=lignin concentration at gL-1; Alig280=lignin solution extinction at 280 nm; Apd280 = A1 + A2 e2
= e1 extinction at 280 nm, sugar decomposition products (furfuraldehyde and hydroxymethylfurfural – HMF), whose A1
and A2 concentrations were determined in advance by HPLC and e1 and e2 and UV spectroscopy.

The ashes were determined with about 1 g samples of sugarcane bagasse without and with hydrolysis or insoluble
lignin. The samples with known moisture content were weighed as close as possible to 0.1 mg in a porcelain crucible that
was previously calcined and weighed. The material was first calcined at 300°C and then for more than 2 h at 800°C.
Cooling the crucible in a dissector, the ash mass was determined in analytical balance (adequate from the standard ASTM
[21].
The ash content was calculated from equation 4.

(4)

In which:

Czy% ... percentage by mass of ash; M1= calcined mass of empty crucible in g; M2= mass of crucible and ash in g

M3=mass of dry bagasse or lignin in g

In natura bagasse and cellulosic pulp were chemically analyzed in the laboratories of the Engineering School of
Lorena (EEL-USP).

Pulp Bleaching

Alkaline pulps were submitted to chemical bleaching for removing residual lignin. The bleaching series included
[24]
three chemicals: sodium hydroxide (E), diethylenetriaminepentaacetic acid (DTPA) (0.4% of base drought) (Q) and
hydrogen peroxide (P) [25, 26].

Dried pulps (5g) were suspended in 100 mL of solution with 0.005 g of MgSO 4.7H2O and 0.5 g of sodium silicate.
The flasks were incubated in a thermoregulated bath (60±3ºC) and, after reaching thermal equilibrium; 5 mL of hydrogen
[27]
peroxide (50%) were added and kept under agitation for 1 h . Bleached pulp was filtered, washed with distilled water,
and dried. The bleaching with sodium chlorite was made in a single step. It was weighed 10 g pulp obtained from the
pulping process soda / AQ with and without acid hydrolysis. The samples were placed in Erlenmyer flasks with 333 mL of
distilled water. The flasks were incubated in a thermoregulated bath (60±3ºC) and, after thermal equilibrium, 3.4 mL of
glacial acetic acid and 8.4 g of sodium chlorite were added and kept under agitation for 1h. After this time, the mixtures
were cooled in an ice bath to 10 ° C. The bleached pulps were filtered, washed with distilled water until the filtrate was
colorless and present near neutral pH (about 5 L of water), dried at room temperature and stored for further analysis.

Preparation of Cellulose Fibers

Fibers were obtained using 10% (w/w) of cellulose, adding 80% (w/w) of N-methylmorpholine-N-oxide (NMMO)
and 10% (w/w) of water. The mixture was made in a bath at 75ºC, for a period of 40 min [17]. The obtained gel was
extruded using water at room temperature. Cellulose fibers were kept in water solution for 24 h, rinsed with water, and
dried at room temperature. The mixed fibers were prepared using 60% of commercial and 40% of bagasse without
cellulose, 50% of commercial and 50% of bagasse cellulose, and 60% of bagasse and 40% of commercial cellulose.
Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 19

Water Uptake or Swelling and Weight Loss Studies

Water uptake or swelling and fiber weight loss were measured in triplicate. Fibers were weighed and immersed in
15 mL of phosphate buffer (PBS), pH 7.4. The flask samples were closed and placed in a thermo regulated bath under
agitation (60 rpm), at 37ºC, for 1, 3, 7, 15, 21 and 30 days. Water uptake was determined by increasing the initial fiber
mass (mi), after removing incubation excess solution with a paper filter and determining the mass (m w) with an analytical
balance. Afterwards, fibers were dried at 40ºC until reaching constant weight; the mass was determined (mf) to obtain fiber
weight loss. Water absorption and weight loss are given by equations 5 and 6.

(5)

(6)

Fiber Diameter and Titer Determination

Fiber samples were stored at 20 ± 2ºC and relative humidity of 65 ± 4% for 24 h; diameter determination was in
[28].
accordance with ISO 5084 After storage, each sample was weighed on an analytical scale. Results represent the rate
[14].
between the weight and length of the fiber thread The assay was held in the Center for Technical Textiles and
Manufactures – CETIM, Institute for Technological Research – IPT, based on ISO 2060 [29], ISO 1139 [30] and ISO 139 [31].

Traction and Elongation

Fiber samples were stored at 20 ± 2ºC and relative humidity of 65 ± 4% for 24 h. Tests were performed according
[32]
to the ASTM D 3822 , using “Instron" Universal-Testing Machine mod. 5869, with 10 N as pull strength, 100mm/min
as velocity and 200 mm as distance. The traction parameter was determined when the fiber thread broke, immediately after
maximum elongation. The assay was held in the Center for Technical Textiles and Manufactures – CETIM, Institute for
Technological Research – IPT.

Scanning Electron Microscopy (SEM)

Microstructural analysis of fibers was performed using scanning electron microscope (SEM) (Phipps XL Serie) in
the Nuclear and Energy Research Institute (IPEN), a State of São Paulo autarchy. Each sample was agglutinated to a thin
film of carbon and coated with gold. The microscope magnifications were 50, 100, 1000 and 4000x and fibers were 12 and
100x.

Cytotoxicity Assay

For analysis of cytotoxicity were used 0.5 g of samples of textile fibers obtained from commercial cellulose and
sugarcane bagasse without hydrolysis and bleaching with H 2O2 and and commercial lyocell. Samples were cut (about 0.5
cm) placed in vials of 12 mL and irradiated at 25 kGy.

The cytotoxicity test was carried out using NCTC clone 929 cell line from American Type Culture Collection
[33]
(ATCC), according International Standardization Organization (ISO 10 993-5) and the previously described
[34].
methodology by Rogero et al.(2003) The extract obtained by sample immersion in cell culture medium MEM (Eagle`s
minimum medium) during 24h was serially diluted and placed on cell cultured in a 96 well microplates. The cytotoxicity
effect was evaluated by measuring the neutral red uptake level by the optical density reading with a Tecan Sunrise
spectrophotometer, at 540 nm. The cell viability percentage was calculated in relation to the control cells in the assay
20 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,
Joao Paulo P. Marcicano  Adalberto Pessoa Jr

(100% viability). High-density polyethylene - HDPE and 0.2% phenol solution in PBS were used as negative and positive
controls respectively, both being treated in the same way as the hydrogel samples in the fibers.

The assay was held in the Chemical and Environmental Centre - CQMA, Nuclear and Energy Research Institute -
IPEN, State of São Paulo

RESULTS AND DISCUSSIONS

Chemical Characterization
Chemical analyses of bagasse without and with hydrolysis and pulp are essential for composition determination
and possible changes in samples after pulping and classification processes. Quantifications are based on sample hydrolysis.
Table 1 shows chemical composition for in natura bagasse, unclassified and classified pulps of bagasse and hydrolyzed
pulp. One can observe that the unclassified pulp presents a lower cellulose percentage (3.9%) when compared with the
classified pulp. The difference in the chemical composition of the classified pulp and the unclassified one occurred due to
the disintegration during the pulping process.

Table 1: Chemical Composition of in Natura or without Hydrolysis Sugarcane Bagasse and NaOH/AQ Pulps

Bleached Pulps Bleached Pulps

Components Bagasse Unclassified Classified
with H2O2 with NaClO2
(%) Pulps (%) Pulps (%)
(%) (%)
Cellulose (%) 52.3 ± 0.7 88.4 ± 0.5 88.9 ± 0.3 93.7± 0.3 94.6± 0.3
Polyoses (%) 17.2 ± 0.3 2.7 ± 0.1 1.8 ± 0.3 1.0± 0.2 0.8 ± 0.2
Insoluble lignin (%) 21.4 ± 1.1 1.8 ± 0.2 1.5 ± 0.2 0.3± 0.1 0.3± 0.1
Soluble lignin (%) 1.5 ± 0.1 3.0 ± 0.2 3.5 ± 0.4 0.5± 0.1 0.5± 0.1
Total lignin (%) 22.9 ± 1.2 4.8 ± 0.4 4.8 ± 0.6 0.8± 0.2 0.8± 0.2
Ash (%) 2.5 ± 0.1 1.1 ± 0.1 Non- determined Non- determined Non- determined
Non-
Extractives (%) Non- determined Non- determined Non- determined Non- determined
determined
Total 94.9 ± 2.3 97.0 ± 1.1 95.7 ± 1.2 95.5± 0.7 96.2±0.7

Table 2: Chemical Composition of Sugarcane Bagasse with Hydrolysis and NaOH/AQ Pulps

Bleached Pulps Bleached Pulps

Components Bagasse Unclassified Classified
with H2O2 with NaClO2
(%) Pulps (%) Pulps(%)
(%) (%)
Cellulose (%) 52.3 ± 0.7 88.4 ± 0.5 88.9 ± 0.3 94.1± 0.3 95.2± 0.3
Polyoses (%) 17.2 ± 0.3 2.7 ± 0.1 1.8 ± 0.3 1± 0.2 0.7 ± 0.2
Insoluble lignin (%) 21.4 ± 1.1 1.8 ± 0.2 1.5 ± 0.2 0.3± 0.1 0.3± 0.1
Soluble lignin (%) 1.5 ± 0.1 3.0 ± 0.2 3.5 ± 0.4 0.6± 0.1 0.5± 0.1
Total lignin (%) 22.9 ± 1.2 4.8 ± 0.4 4.8 ± 0.6 0.9± 0.2 0.8± 0.2
Ash (%) 2.5 ± 0.1 1.1 ± 0.1 Non- determined Non- determined Non- determined
Non-
Extractives (%) Non- determined Non- determined Non- determined Non- determined
determined
Total 94.9 ± 2.3 97.0 ± 1.1 95.7 ± 1.2 96± 0.7 96.7±0.7

A reduction of 63.3% in the polyose content was observed for the hydrolyzed pulp, when compared with the
unclassified pulp; a 55% reduction in the polyose content was observed for the hydrolyzed pulp, when compared with the
classified pulp. Hydrolysis reduces significantly the polyose content of fibers after bleaching, resulting in a pure cellulose.
The conversion process of cellulose to its derivatives, such as viscose (rayon) cellulose acetate and cellophane, is efficient
when the polyose content reaches from 1 to 10% [35].
Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 21

Scanning Electron Microscopy (SEM) of Bagasse Pulp

Figure 1 shows sugarcane bagasse pulp soda/AQ microscopies before classification and bleaching, where fibers of
varied sizes can be observed. During pulping soda/AQ process at high temperatures, lignin removal allows separation of
cellulosic fibers. Due to alkalinity, cellulose can be also degraded, decreasing the yield of the pulping process. Pulping
process may not be enough to defiber the material; ideally after pulping (soda/AQ), the pulp should go through a
mechanical refining step or size classification of fibers. Figure 1 (a, b, c and d) shows fibers before the classification
process, resetting varied sizes.

(a) (b)

(c) (d)
Figure 1: SEM Images of Soda/AQ Pulps of Bagasse without Hydrolysis before Classification and Bleaching
(a) 50 X, (b) 100X, (C) 1000 X and (d) 4000X

Yield Studies of Soda/AQ Pulping Process

Due to the presence of nondefibered material in the pulp soda/AQ (visually observed after pulping process), it was
necessary to classify fibers obtaining the classified yield.

Yield classified for pulping process was 34.6% for bagasse without hydrolysis (table 3); values of yield found by
[36].
other authors for alkaline pulping fit the range of 33.1 – 40.9% to sugarcane bagasse In the case of bagasse with
hydrolysis yield was 30% lower compared to bagasse without hydrolysis.
22 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,
Joao Paulo P. Marcicano  Adalberto Pessoa Jr

Table 3: Results of Soda/AQ Pulping for Sugarcane Bagasse without or with Hydrolysis

Soda/AQ Initial Final Total Yield Non Defibered Classified R

Wash
Pulping pH pH R (%) Material (%) (%)
Bagasse without
Water* 13.8 6.7 46 10.9 34.6
hydrolysis
Bagasse with hydrolysis Water* 13.5 6.6 36.8 9.8 26.6
* Water Was Used for Washing and Neutralizing the PH of the Pulp

Bleaching using hydrogen peroxide and sodium chlorite showed that both reagents were efficient. However,
considering toxicity and handling difficulties, hydrogen peroxide is more recommendable.

Water Uptake or Swelling and Weight Loss Studies

Figure 2a shows water uptake or swelling results of fibers over time. Cellulose fibers from bagasse without
hydrolysis and bleaching (sodium chlorite 80%) showed large water uptake ability, followed by 70% commercial cellulose
fibers and cellulose obtained from bagasse after hydrolysis and bleaching with hydrogen peroxide.

Figure 2b shows that fibers obtained from commercial cellulose lost 25% of weight within 30 days of storage;
while fibers obtained from sugarcane bagasse lost 20%.

Some of the most important properties of a textile fiber are closely related to its behavior in various weather
conditions. Most of the fibers are hygroscopic, they are capable of absorbing water vapor from humid atmosphere, and
conversely desorb or lose water in a dry atmosphere. Many of the physical properties of a fiber are affected by the water
content absorbed: dimensions, tensile strength, elastic recovery, electrical resistance, stiffness. As a tissue, moisture
relations exert an important when it is decided that the fabric is unsuitable for a particular purpose [14].

(a) (b)
Figure 2: Results of (a) Swelling and (b) Weight Loss of Fibers Taking Time into Account. (-□-) Cellulose Obtained
from Bagasse without Hydrolysis and Bleaching with Hydrogen Peroxide, (--) Cellulose Obtained from Bagasse
with Hydrolysis and Bleaching with Hydrogen Peroxide, (-▲-) Cellulose Obtained from Bagasse without Hydrolysis
and Bleaching with Sodium Chlorite and (-◊-) Commercial Cellulose

The developed fibers showed a swelling behavior, which is also very important for textile materials aimed to be
used for instance in medical applications.
Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 23

Diameter, Rupture Load, Titer and Tenacity of Textile Fibers

According to the results of diameter determination in Table 4, fibers presenting larger diameters were obtained
from sugarcane bagasse without hydrolysis cellulose and bleaching with H2O2 (165.6 ± 23.1 µm) and mixed cellulose
(60% a + 40% b) (170.8 ± 12.2 µm). Variations in fiber diameter can be related to different pressure in syringe piston
during the extrusion process, once it was performed manually.

Yarn classification establishes fiber differences and works as a guideline to orientate the commercialization and
the production of certain woven tissues or in the comparison between yarns. For this purpose, it was created a form of
[37]
expression for yarn diameter known as yarn titer . A filament titer is represented by a value that expresses the relation
[14].
between mass and length

Table 4: Diameter Rupture Load, Titer and Tenacity of Textile Fibers (20ºC/65%U.R.)

Rupture
Fiber Samples of Different Diameter Titer Tenacity
Load Elongation (%)
Celluloses
(µm) (N)e (Tex) f
(cN/tex)
Commerciala 104.6 ± 18.4 1.06 ± 0.45 4.23 ± 2.17 25.7 4.3
Bag SH/ H2O2 b 165.6 ± 23.1 1.69 ± 0.68 2.21 ± 1.14 39.7 4.3
Bag CH/ H2O2 c 119.7 ± 19.3 1.37 ± 0.20 2.66 ± 0.53 25.9 5.3
Bag SH/ NaClO2c,d 131.1 ± 16.1 1.13 ± 0.15 2.40 ± 1.08 33.9 3.3
(60% a+ 40% b) 170.8 ± 12.2 0.28 ± 0.14 6.79 ± 2.30 60.3 0.5
(50% a + 50% b) 143.5 ± 15.9 1.12 ± 0.14 4.23 ± 1.21 33.6 3.3
(60% b + 40% a) 108.5 ± 9.4 0.93 ± 0.22 2.2 1 ± 1.65 24.4 3.8
a
cellulose sigma
b
bagasse without hydrolysis and bleaching with H2O2
c
bagasse with hydrolysis and bleaching with H2O2
d
bagasse with hydrolysis and bleaching with sodium chlorite
e
mass in grams of 1.000 m of yarn, filament or fibers
f
unit of force kg.ms-2

Table 4 shows the tenacity values obtained for commercial cellulose fibers and bagasse obtained from different

methods in the range of 0.5 - 5.3 cN/tex. The tenacity values found for Lyocell - TencelTM – HT were in the range of
[14].
4.24 – 4.41 cN/tex Fibers presenting tenacity values closer to those found in the literature were obtained from
commercial cellulose and cane bagasse without hydrolysis bleaching with H 2O2.

Due to its cellulosic origin, properties of lyocell fibers, such as softness and absorbency, are suitable for use in the
medical field, especially for skin treatment [18].

Fibers Obtained from Commercial Cellulose and Sugarcane Bagasse

Figure 3a, b, c and d presents the aspects of textile fibers obtained from commercial cellulose and sugarcane
bagasse with hydrolysis and bleaching with hydrogen peroxide, bagasse without hydrolysis and bleaching with hydrogen
peroxide, and bagasse without hydrolysis and bleaching with sodium chlorite. Based on the figure, it is possible to state
that there is no visual difference between the samples.
24 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,
Joao Paulo P. Marcicano  Adalberto Pessoa Jr

(a) (b)

(c) (d)
Figure 3: Textile Fibers Obtained from Different Celluloses, (a) Commercial Cellulose, (b) Bagasse with
Hydrolysis and Bleaching with Hydrogen Peroxide, (c) Bagasse without Hydrolysis and Bleaching with
Hydrogen Peroxide, and (d) Bagasse without Hydrolysis and Bleaching with Sodium Chlorite

Morphological Analysis of Textile Fibers

Scanning electron microscopy was used to evaluate the quality of fibers, once it allows evaluating the presence or
not of scale, thickness or irregularity forms along the fibers. In addition, it can determine fiber grouping, presence of marks
in its interior, presence or not of marrow, shape of transversal and longitudinal sections, color differences, among others. In
the medical field, the SEM can be used to evaluate the presence of microorganisms as fungi, bacteria and cell adhesion to
material surfaces [27, 38-40].

Figures 4 and 5 show SEM fiber images obtained from commercial cellulose and cane bagasse. It can be observed
that fibers are oriented in a certain direction, presenting some uniformity even after the manual extrusion process. It is also
possible to observe the presence of grooves on the fiber surface (figures 4b, d and 5b, d), probably due the syringe used for
extrusion. The needles were cut manually, but by using the laser cutting method would be ideal to avoid these grooves.

(a) (b)
Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 25

(c) (d)

Figure 4: Scanning Electron Microscopy (SEM) of Textile Fibers Obtained from Different Celluloses,
(a, b) Commercial Cellulose, (c, d) Bagasse with Hydrolysis and Bleaching with Hydrogen Peroxide

(a) (b)

(c) (d)

Figure 5: Scanning Electron Microscopy (SEM) of Textile Fibers Obtained from Different Celluloses, (a, b) Bagasse
without Hydrolysis and Bleaching with Hydrogen Peroxide, and (c, d) Bagasse without Hydrolysis and Bleaching
with Sodium Chlorite

Cytotoxicity Assay

In the cytotoxicity assay, the percentages were plotted against extract concentration, resulting in in cellular
viability curves shown in Figure 6. In this plot the sample with curves above 50% cell viability (cytotoxicity index line =
IC50%) are considered noncytotoxic and those below or crossing the IC50% line are considered cytotoxic.
26 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,
Joao Paulo P. Marcicano  Adalberto Pessoa Jr

Figure 6: Cell Viability Curves in Textile Fibers Obtained from (-□-) Cellulose of Sugarcane Bagasse without
Hydrolysis and Bleaching with H2O2, (-◊-) Commercial Cellulose, (-■-) Negative Control and (-○-) Positive Control
Cytotoxicity Test

The percentage of viability was calculated in relation to control and plotted in a graphic to obtain the index of
cytotoxicity IC50%, that is the concentration of extract that cause damage or death of 50% of cell population. The Figure 6
shows the IC50% for the positive control (IC50% = 53), cellulose fiber of sugar cane bagasse (IC50% = 84). It means that
to cause damage or death of 50% of cells, it is necessary a concentration greater than 7.1% for the fiber obtained from
commercial cellulose.

CONCLUSIONS

In this paper, attention has been focused on the process of extracting cellulose from sugarcane bagasse without
and with hydrolysis, preparation and properties of the fiber for potential use in textile applications. Cellulose fibers can be
produced by a wet spinning technique. Bleaching using hydrogen peroxide and sodium chlorite showed that both reagents
were efficient. However, considering toxicity and handling difficulties, hydrogen peroxide is more recommendable.
Mechanical tests showed that fibers had tensile strength compatible with lyocell fibers found in the textile market. After
fully characterized, cellulosic fibers obtained from sugarcane bagasse will be evaluated and tested as a support for enzyme
immobilization and pharmaceutical impregnation, as well as for controlled release studies, aiming medical applications.

ACKNOWLEDGEMENTS

This work was sponsored by the State of São Paulo Research Foundation (Fapesp). The authors thank Sizue Ota
Rogero of Chemical and Environmental Centre - CQMA, Nuclear and Energy Research Institute - IPEN, State of São
Paulo by cytotoxicity assays.

REFERENCES

1. Sun, J. X., Sun, X. F, Sun R. C., Fowler, P.,  Baird, M.S. (2003). Inhomogeneities in the chemical structure of
sugarcane bagasse lignin. Journal of Agricultural and Food Chemistry. 51, 6919-6725.

2. Soccol, C. R.,  Vandenberghe, L.P.S. (2003) Overview of applied solid-state fermentation in Brazil.
Biochemical Engineering Journal, 13, 205–218.

3. Liu, C.F., Sun, R. C., Qin, M. H, Zang, A. P., Ren, J. L., Ye, J., Luo, W.,  Cao, Z. N. (2008) Succinoylation of
sugarcane bagasse under ultrasound irradiation. Bioresource Technology. 99, 1465-1473.
Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 27

4. Vallejos, M. V., Curvelo, A. A. S., Teixeira, E. M., Mendes, F. M., Carvalho, A. J. F., Felissia, E.,  Area, M.
(2011). A. Composite materials of thermoplastic starch and fibers from the ethanol–water fractionation of
bagasse. Industrial Crops and Products, 33, 739-746.

5. Rocha, G. J. M., Gonçalves, A. R., Oliveira, B. R.,  Rossell, C. E. V. (2012) Steam explosion pretreatment
reproduction and alkaline delignification reactions performed on a pilot scale with sugarcane bagasse for
bioethanol production. Industrial Crops and Products, 35, 274-279.

6. Kalderis, D., Bethanis, S., Paraskeva,  Diamadopoulos, E. (2008). Production of activated carbon from bagasse
and rice husk by a single-stage chemical activation method at low retention times. Bioresource Technology, 99,
6809–6816.

7. CONAB National Supply Company. (2013). Monitoring of the Brazilian harvest of cane sugar. Retrieved from
http://www.conab.gov.br. (accessed February 10, 2013).

8. Pandey, A., Soccol, C. R., Nigan, P.,  Soccol, VT. (2000) Biotechnology potential of agro industrial residues. I:
sugarcane bagasse. Bioresource Technology, 74, 69 80.

9. Cerqueira, D. A., Rodrigues, G. F.,  Meireles, C. S. (2007). Optimization of sugarcane bagasse cellulose
acetylation. Carbohydrate Polymers, 69, 579-582.

10. Liu, C. F., Sun, R. C., Quin, M. H., Zhang, A. P., Ren, J.L., Xu, F., Ye, J., Wu, S. B. (2007). Chemical
modification of ultrasound-pretreated sugarcane bagasse with maleic anhydride. Industrial Crops and Products,
26, 212–219.

11. John, M. J.,  Thomas, S. (2007) Biofibres and biocomposites. Carbohydrate Polymers, 71, 343-364.

12. Dawson, L.,  Boopathy R. (2007). Use of post-harvest sugarcane residue for ethanol production. Bioresource
Technology, 98, 1695–1699.

13. Shaikh, H. M., Pandare, K. V., Nair, G.,  Varma, A. J. (2009). Utilization of sugarcane bagasse cellulose for
producing cellulose acetates: Novel use of residual hemicellulose as plasticizer. Carbohydrate Polymers, 76, 23–
29.

14. Maluf, E.,  Kolbe W. (2003) Textile fibers. Technical textile industry data. 2 Ed. Institute for Technological
Research and Brazilian Textile and Confection Industry Association ABIT.

15. Rosenau, T., Ofinger, A., Potthast, A. ,  Kosma, P. (2003). On the conformation of the cellulose solvent N-
methylmorpholine-N-oxide (NMMO) in solution. Polymer 44, 8177-8182.

16. Rosenau, T., Potthast, A., Sixta, H.,  Kosma P. (2001). The chemistry of side reactions and byproduct formation
in the system NMMO/cellulose (Lyocell process). Progress in Polymer Science, 26, 1763 -1837.

17. Fink, H. P., Weigel, P., Purz, H. J.,  Ganster J. (2001). Structure formation of regenerated cellulose materials
from Nmmo-Solutions. Progress in Polymer Science, 26, 1473-1524.

18. Araújo, M., Fangueiro, R.,  Hong, H. (2000). Technical textiles in the medicine Applications, new processes
and new products. Technical textiles material of the new millenium. Williams, Lda (ed).
28 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,
Joao Paulo P. Marcicano  Adalberto Pessoa Jr

19. Pessoa-Jr, A. (1997). Acid hydrolysis of hemicelulose from sugarcane bagasse. Brazilian Journal of Chemical
Engineering, 14, 291-297.

20. Costa, S. M., Gonçalves, A. R.,  Esposito E. (2005). Ceriporiopsis subvermispora used in delignification of
sugarcane bagasse prior soda/anthraquinone pulping. Applied Biochemistry and Biotechnology, 124, 696- 706.

21. ASTM Methods.1996. Standard Test Method for Lignin in Wood, D110656, pp. 396–398.

22. Rocha, G. M., Silva, F. T, Araújo, G. T.,  Curvelo, A. A. S. (1997). A fast and accurate method for determining
the cellulose and polyoses through HPLC. In: V Brazilian Symposium Proceedings on the Chemistry of Lignin
and Other Wood Components, vol. 5, Curitiba, PR, Brazil, 113–115.

23. Rocha, G. J. M. (2000). Delignification of sugarcane bagasse attended for oxygen. (Unpublished doctoral thesis).
University of São Paulo / São Carlos, Chemical Institute.

24. Robert, S.,  Daneault, C. (1995). Yellowing mechanism and kinetics of thick handsheets of softwood
thermomechanical pulp. Journal of Wood Chemistry and Technology, 15, 113-133.

25. Browing, B.L. (1963). The Chemistry of Wood. New York: Interscience Publisher.

26. Hortal, J.A. G.,  Luciá, T. V. (1894). Bleaching of pulp in the paper industry. Terrassa: Polytechnic University
of Catalonia.

27. Araújo, M.,  Castro, E. M. M. (1984a) Textile Engineering Manual. Calouste Gulbenkian Foundation, Lisbon,
Portugal.

28. ISO International Organization for Standardization. (1996). Determination of Thickness of Textiles and Textile
Products, 5084, pp. 1–5.

29. ISO International Organization for Standardization. (1994). Textiles – Yarn from Packages – Determination of
Linear Density (Mass per Unit Length) by the Skein Method, 2060, pp. 1–13, 19.

30. ISO International Organization for Standardization. (1973). Textiles – Designation of Yarns, 1139, pp. 1–5.

31. ISO International Organization for Standardization (2005). Standard Atmospheres for Conditioning and Testing
(German), 139, pp. 1–8.

32. ASTM Methods. Standard Test Methods for Tensile Properties of Singles Textile Fibers, D3822, pp. 1–10, 2007.

33. ISO International Organization for Standardization. (1992). Biological evaluation of medical devices 10 993-5,
Part 5, Tests for cytotoxicity: in vitro methods.

34. Rogero, S. O.,  Malmonge, S.M., Lugão, A.B, Ikeda, T. I.,  Cruz A. S. (2003). Biocompatibility study of
polymeric biomaterials. Artificial Organs, 27, 424–427.

35. Bierman C.J. (1993) Refining and characterization. In C J Biermann (Ed.). Handbook of Pulping and
Papermaking. (2 ed). San Diego, US: Academic Press.

36. Ruzene, D. S., Gonçalves, A. R, Teixeira, J. A.,  Pessoa de Amorim, M.T. ( 2007). Acid and alkaline catalyzed
ethanol pulping Carboxymethylcellulose Chemical bleaching Infrared spectra Sugarcane bagasse Organosolv
pulping. Applied Biochemistry and Biotechnology, 136, 1-12.
 Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 29

37. Ribeiro, G. L. (1984). Introduction to textile technology. Technological of the chemical industry and textile
center, Rio de Janeiro, CETIQT/SENAI.

38. Dadashian, F., Yaghoobi, Z.,  Wilding, M.A. (2007). Internal damage of crimped lyocell fiber. Textile Research
Journal, 77, 457-461.

39. Reddy, N.,  Yang, Y. (2009). Properties of natural cellulose fibers from hop stems. Carbohydrate Polymers, 77,
898–902.

40. Araújo, M., Castro,  E. M. M. (1984b) Textile Engineering Manual. Calouste Gulbenkian Foundation, Lisbon,
Portugal.

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