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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

3

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

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


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 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).


17

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

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 45 oC, 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:


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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) hydrogen peroxide (P)

[24]

and

[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 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

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 (m f) 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 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 (ATCC), according International Standardization Organization (ISO 10 993-5) methodology by Rogero et al.(2003)

[34].

[33]

and the previously described

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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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 (%)

Cellulose (%) Polyoses (%) Insoluble lignin (%) Soluble lignin (%) Total lignin (%) Ash (%)

52.3 ± 0.7 17.2 ± 0.3 21.4 ± 1.1 1.5 ± 0.1 22.9 ± 1.2 2.5 ± 0.1 Ex 94.9 ± 2.3

Total

Unclassified Pulps (%)

Classified Pulps (%)

88.4 ± 0.5 88.9 ± 0.3 2.7 ± 0.1 1.8 ± 0.3 1.8 ± 0.2 1.5 ± 0.2 3.0 ± 0.2 3.5 ± 0.4 4.8 ± 0.4 4.8 ± 0.6 1.1 ± 0.1 Non- determined Non- determined Non- determined 97.0 ± 1.1 95.7 ± 1.2

Bleached Pulps with H2O2 (%) 93.7± 0.3 1.0± 0.2 0.3± 0.1 0,.5± 0.1 0.8± 0.2 Non- determined Non- determined 95.5± 0.7

Bleached Pulps with NaClO2 (%) 94.6± 0.3 0,8 ± 0.2 0.3± 0.1 0,5± 0.1 0.8± 0.2 Non- determined Non- determined 96.2±0.7

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

Bagasse (%)

Cellulose (%) Polyoses (%) Insoluble lignin (%) Soluble lignin (%) Total lignin (%) Ash (%)

52.3 ± 0.7 17.2 ± 0.3 21.4 ± 1.1 1.5 ± 0.1 22.9 ± 1.2 2.5 ± 0.1 Ex 94.9 ± 2.3

Total

Unclassified Pulps (%) 88.4 ± 0.5 2.7 ± 0.1 1.8 ± 0.2 3.0 ± 0.2 4.8 ± 0.4 1.1 ± 0.1 Non- determined 97.0 ± 1.1

Classified Pulps(%) 88.9 ± 0.3 1.8 ± 0.3 1.5 ± 0.2 3.5 ± 0.4 4.8 ± 0.6 Non- determined Non- determined 95.7 ± 1.2

Bleached Pulps with H2O2 (%) 94,1± 0.3 1± 0.2 0,3± 0.1 0,6± 0.1 0,9± 0.2 Non- determined Non- determined 96± 0.7

Bleached Pulps with NaClO2 (%) 95,2± 0.3 0,7 ± 0.2 0,3± 0.1 0,5± 0.1 0,8± 0.2 Non- determined Non- determined 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


21

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

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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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.


23

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

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 between mass and length

[37]

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

[14].

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

Commercial Bag SH/ H2O2 b Bag CH/ H2O2 c Bag SH/ NaClO2c,d (60% a+ 40% b) (50% a + 50% b) (60% b + 40% a) a cellulose sigma

Diameter (µm) 104.6 ± 18.4 165.6 ± 23.1 119.7 ± 19.3 131.1 ± 16.1 170.8 ± 12.2 143.5 ± 15.9 108.5 ± 9.4

Rupture Load (N)e 1.06 ± 0.45 1.69 ± 0.68 1.37 ± 0.20 1.13 ± 0.15 0.28 ± 0.14 1.12 ± 0.14 0.93 ± 0.22

Elongation (%) 4.23 ± 2.17 2.21 ± 1.14 2.66 ± 0.53 2.40 ± 1.08 6.79 ± 2.30 4.23 ± 1.21 2.2 1 ± 1.65

Titer

Tenacity

(Tex)f 25.7 39.7 25.9 33.9 60.3 33.6 24.4

(cN/tex) 4.3 4.3 5.3 3.3 0.5 3.3 3.8

b

bagasse without hydrolysis and bleaching with H2O2

c

bagasse with hydrolysis and bleaching with H 2O2

d e

bagasse with hydrolysis and bleaching with sodium chlorite

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 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 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.

(a)

(b)


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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)

(c)

(b)

(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


25

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

(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


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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2.Textile fiber.FULL