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TEXTILE FIBER PRODUCED FROM SUGARCANE BAGASSE CELLULOSE: AN AGRO-INDUSTRIAL RESIDUE SIRLENE, M. COSTA 1 , SILGIA A. COSTA 2 , RICHARD PAHL 3 , PRISCILA G. MAZZOLA 4 , JOÃO PAULO P. MARCICANO 5 &ADALBERTO PESSOA JR 6 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 different groups [1-5]. 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 milled to produce sugar and ethanol [7] . 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 disposal problem for mill owners [6]. This agricultural residue has received increasing attention, since it represents an International Journal of Textile and Fashion Technology (IJTFT) ISSN 2250-2378 Vol. 3, Issue 2, Jun 2013, 15-28 © TJPRC Pvt. Ltd.

description

Sugarcane bagasse with and without acid hydrolysis was used for extraction of cellulose. The bagasse pulpswithout or with hydrolysis, and commercial mixtures of these materials in different proportions were used for theproduction 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 wereused to obtain fibers with N-methylmorpholine-N-oxide (NMMO). Bagasse and pulps were characterized by their chemicalcomposition. Fibers were analyzed to evaluate maximum water uptake loading or swelling, weight loss and mechanicalproperties. Microstructure was analyzed by scanning electron microscope (SEM). The pulping yield was 34.6% for bagassewithout 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 peroxidehad tenacity values of 4.3 cN/tex, which are compatible with commercial lyocell made from wood pulp cellulose.

Transcript of 2.Textile Fiber.full

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TEXTILE FIBER PRODUCED FROM SUGARCANE BAGASSE CELLULOSE: AN

AGRO-INDUSTRIAL RESIDUE

SIRLENE, M. COSTA1, SILGIA A. COSTA

2, RICHARD PAHL

3, PRISCILA G. MAZZOLA

4,

JOÃO PAULO P. MARCICANO5 &ADALBERTO PESSOA JR

6

1,2,5School 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

6Department 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

different groups [1-5].

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

milled to produce sugar and ethanol [7]

. 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

disposal problem for mill owners [6].

This agricultural residue has received increasing attention, since it represents an

International Journal of Textile and

Fashion Technology (IJTFT)

ISSN 2250-2378

Vol. 3, Issue 2, Jun 2013, 15-28

© TJPRC Pvt. Ltd.

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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

polypropylene composites [12, 10, 5, 13].

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

(99.7%) recycled and sent back to the process [15-17].

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

4C. 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).

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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):

RT= m/M x 100 (equation 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:

RC= RT - tr (mr/M) (equation 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

The modified method standardized by ASTM D 271-48 [21]

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.min

1. 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:

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18 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,

Joao Paulo P. Marcicano Adalberto Pessoa Jr

Clig.=4.187×10−2(Alig280−Apd280)−3.279×10−4 L-1

(equation 3)

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.

Czy% = (M1-M2) / M3 x 100 (equation 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

three chemicals: sodium hydroxide (E), diethylenetriaminepentaacetic acid (DTPA) (0.4% of base drought) (Q) [24]

and

hydrogen peroxide (P) [25, 26]

.

Dried pulps (5g) were suspended in 100 mL of solution with 0.005 g of MgSO4.7H2O 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

peroxide (50%) were added and kept under agitation for 1 h [27]

. 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.

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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 (mw) 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.

Water absorption= [(mw – mi) mi] x 100 (equation 5)

Weight loss= [(mf – mi)/ mi] x 100 (equation 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

accordance with ISO 5084 [28].

After storage, each sample was weighed on an analytical scale. Results represent the rate

between the weight and length of the fiber thread [14].

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

to the ASTM D 3822 [32]

, 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 H2O2 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

(ATCC), according International Standardization Organization (ISO 10 993-5) [33]

and the previously described

methodology by Rogero et al.(2003) [34].

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

(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.

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20 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,

Joao Paulo P. Marcicano Adalberto Pessoa Jr

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

Components

Bagasse

(%)

Unclassified

Pulps (%)

Classified

Pulps (%)

Bleached Pulps

with H2O2

(%)

Bleached Pulps

with NaClO2

(%)

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

Ex Non- determined Non- determined Non- determined Non- 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

Components

Bagasse

(%)

Unclassified

Pulps (%)

Classified

Pulps(%)

Bleached Pulps

with H2O2

(%)

Bleached Pulps

with NaClO2

(%)

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 Ex Non- determined Non- determined Non- determined Non- 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].

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

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Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 21

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

other authors for alkaline pulping fit the range of 33.1 – 40.9% to sugarcane bagasse [36].

In the case of bagasse with

hydrolysis yield was 30% lower compared to bagasse without hydrolysis.

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

Soda/AQ

Pulping Wash

Initial

pH

Final

pH

Total Yield

R (%)

Non Defibered

Material (%)

Classified R

(%)

Bagasse without

hydrolysis Water* 13.8 6.7 46 10.9 34.6

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

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22 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,

Joao Paulo P. Marcicano Adalberto Pessoa Jr

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.

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.

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Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 23

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

expression for yarn diameter known as yarn titer [37]

. A filament titer is represented by a value that expresses the relation

between mass and length [14].

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

Fiber Samples of Different

Celluloses

Diameter Rupture

Load Elongation (%) Titer Tenacity

(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

bbagasse without hydrolysis and bleaching with H2O2

cbagasse with hydrolysis and bleaching with H2O2

d bagasse with hydrolysis and bleaching with sodium chlorite

emass in grams of 1.000 m of yarn, filament or fibers

funit 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

4.24 – 4.41 cN/tex [14].

Fibers presenting tenacity values closer to those found in the literature were obtained from

commercial cellulose and cane bagasse without hydrolysis bleaching with H2O2.

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.

(a) (b)

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24 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,

Joao Paulo P. Marcicano Adalberto Pessoa Jr

(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)

(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

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Textile Fiber Produced from Sugarcane Bagasse Cellulose: An Agro-Industrial Residue 25

(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.

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

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26 Sirlene, M. Costa, Silgia A. Costa, Richard Pahl, Priscila G. Mazzola,

Joao Paulo P. Marcicano Adalberto Pessoa Jr

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.

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