silica–kaolinite network on cellulose fiber to improve the functionality

Composites: Part B 48 (2013) 158–166

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UV radiation inducing succinic acid/silica–kaolinite network on cellulose fiber to improve the functionality Mazeyar Parvinzadeh Gashti a,⇑, Alireza Elahi b, Mahyar Parvinzadeh Gashti c a

Department of Textile, Islamic Azad University, Shahre Rey Branch, Tehran, Iran Department of Textile, Islamic Azad University, South Tehran Branch, Tehran, Iran c Faculty of Mechanical Engineering, Islamic Azad University, Parand Branch, Parand, Iran b

a r t i c l e

i n f o

Article history: Received 28 August 2012 Received in revised form 25 October 2012 Accepted 7 December 2012 Available online 20 December 2012 Keywords: A. Fabrics/textiles B. Thermal properties D. Chemical analysis

a b s t r a c t The aim of this research was to embed silica–kaolinite on a cotton surface using succinic acid (SA) as a cross-linking agent and sodium hypophosphite (SHP) as a catalyst. The influence of inorganic particles on the performance of the cellulose fiber was investigated using Attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermo-gravimetric analyzer (TGA), scanning electron microscope (SEM), electron dispersive X-ray spectrometer (EDX), water contact angle (WCA) and reflectance spectroscopy (RS). ATR showed the possible interactions between silica, kaolinite, the cross-linking agent and cellulose functional groups on the surface. The results obtained from the thermal measurements demonstrated that the stabilized silica–kaolinite particles can significantly improve the thermal stability of the cotton fiber. This research suggests a successful method for stabilization and compatibility of various inorganic particles on cotton. Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction In recent years, clay layers have attracted a great deal of interest as they are often claimed to improve different properties of polymers such as modulus, strength, stiffness, flame retardancy, dimensional stability, electrical conductivity, barrier performance, solvent and heat resistance, wettability and dyeability depending on the type and contents of clay used [1–5]. The layered clays used for these purposes are bentonite, montmorillonite, attapulgite, mica, sercite, hydrotalcite, fluoromica, hectorite and saponite, but kaolin is one of the most commercially available clay minerals with the chemical composition of Al2Si2O5(OH)4. It is composed of one tetrahedral silicon–oxygen [Si2nO5n]2n and one octahedral alumo-oxygen-hydroxylic [Al2n(OH)4n]2n+ sheet with the net negative charges in water [6–9]. Coating of inorganic nano-particles on textiles is a new concept that has been introduced in recent years to open up multifunctional properties [10,11]. For this purpose, a great number of coating processes have been carried out on textiles to produce specific properties including protection from UV irradiation [12]; softening [13–17]; flame-retardancy [18]; antibacterial finishing [19–21]; superior stain, water and oil repellency [22,23] and electrically conductivity [24–26]. The major problem associated with coating of textiles with inorganic nano-particles is lack of compat⇑ Corresponding author. Tel.: +98 (0)91 23137115; fax: +98 (0)21 22593135. E-mail address: [email protected] (M. Parvinzadeh Gashti). 1359-8368/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved. http://dx.doi.org/10.1016/j.compositesb.2012.12.002

ibility between them which has limited their application in the textile industry [10,11]. Cellulose fibers are low thermal resistant and highly combustible. Thus, their behavior against heat and flame has been investigated by researchers in the field of safety and protective aspects of textile products used in public spaces such as schools, theatres or special event venues [27–29]. Nano-particles such as clay, silica and carbon nanotubes have been extensively considered for modification of low thermal resistant polymers. The drastic enhancement in thermal stability of such polymer nanocomposites could be due to different effects of nano-particles including high thermal stability and high insulation properties [30,31]. However, to the best of our knowledge, there is no study on the effect of silica– kaolinite on thermal stability of cotton. Here, we introduced a novel method for embedding silica–kaolinite on cotton fiber due to the fact that there is no attraction between them. Attempts were made in the present study to investigate different properties of SA/silica–kaolinite nanocomposite coated cotton fiber. 2. Experimental 2.1. Materials and methods A desized, scoured and bleached plain weave 100% cotton fabric with 36 wrap/cm and 26 weft/cm was supplied by Yazdbaf Fabrics Company (Yazd, Iran). SiO2–kaolinite particle was Sillitin V88 supplied by the German company, Hoffman Mineral. It is a natural

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combination of corpuscular, cryptocrystalline and amorphous silica and lamellar kaolinite with chemical composition of SiO2–Al2 [(OH)4Si2O5]. As stated by manufacture, its density is estimated to be 2.6 g/cm3 from the chemical composition. Succinic acid (SA), sodium hypophosphite (SHP) and cetyltrimethyl ammonium bromide (CTAB) were supplied by Merck Chemical Co., Germany. Nonionic detergent from Shirley Development Limited was used for washing. SA/silica–kaolinite network was produced on cotton by a multiple-step method. First, different colloidal dispersions were prepared by mixing 1%, 5% and 10% (o.w.f) silica–kaolinite, CTAB and deionized water (The ratio of silica–kaolinite: CTAB was kept as 2:1). The colloidal dispersions were then treated with an ultrasonic machine at 50 °C for 2 h to reduce the particle sizes. Second, a 10% (o.w.f) SA with SHP (6% o.w.f) were added to the different dispersions of silica–kaolinite under ultrasound vibration at 40 °C for 20 min. Third, the fabrics were padded (85% wet pick up) in prepared solutions. The treated fibers were dried at 60 °C for 10 min and cross-linking of the fabrics was conducted by UV irradiation (Germicidal UV lamp from Keosan Enterprise Co., Ltd.: 15W/0.3A, UV-C, kmax = 250 nm and light intensity of 0.4 lW cm2) at the ambient temperature for 30 min. The irradiated fibers were then washed separately at 40 °C for 15 min using 2 g/L sodium carbonate and 1 g/L nonionic detergent, which was found useful for removing residual silica, kaolinite, SA and SHP. Finally, the fabrics were dried completely at 40 °C in a vacuum.

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2.2. Characterization Surface characterization of the resultant samples was carried out using a ThermoNicolet NEXUS 870 FTIR spectrophotometer (Nicolet Instrument Corp., USA) integrated with an IBM personal computer. The spectrophotometer was equipped with a single reflection ATR accessory for reflection mode. All the ATR spectra of SA/silica–kaolinite network coated fibers were normalized. The morphology of the fibers was characterized with the wide angle X-ray diffractometry using a computerized SEIFERT/PTS 3003 X-ray diffractometer. Ni-filtered Cu Ka radiation generated at 40 kV (k = 0.1542 nm) and 30 mA was used. The measured angle ranged from 5° to 84° for SiO2–kaolinite particle, and 5–80° for SA/silica–kaolinite coated fibers with the scan speed of 1°/min. A differential scanning calorimetry of the samples was carried out using a Perkin Elmer pyris 6 DSC model integrated with an IBM personal computer. The samples were heated from 20 °C up to 440 °C at a rate of 5 °C/min in a nitrogen atmosphere. The thermal degradation properties of the samples were performed on a TGA-PL thermoanalyzer from UK. In each case a 5 mg sample was examined under an N2 at a heating rate of 5 °C/min from room temperature to 650 °C. Surface morphology analyses of the coating were carried out by means of a scanning electron microscope (SEM, Philips, XL30, The Netherlands). The samples were covered with an Au layer under vacuum conditions prior to the measurement. The presence of elements on each coated surface was also determined by energy dispersive X-ray microanalysis (EDX) attached to the

Fig. 1. ATR curves for (a) untreated cotton, (b) cotton sample coated with SA/10% silica–kaolinite network.

Fig. 2. The possible cross-linking reactions catalyzed with SA under UV irradiation [53,56,57].

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SEM. Contact angle measurements of the samples were carried out at room temperature on a Kruss G10 instrument of German origin. Water was used as the probe liquid at 23 ± 2 °C and 65% relative humidity. The average contact angle from six different locations on each sample was determined and the experimental uncertainty was within ±2°. The reflectance of each sample was recorded using a Cary 500 UV–Vis–NIR spectrophotometer from Varian (USA) integrated with an IBM personal computer. 3. Results and discussion 3.1. Structural information by ATR spectra The infrared spectra of the untreated cotton and the sample coated with SA/10% silica–kaolinite network are shown in Fig. 1.

The intermolecular O–H stretching vibrations relating with O–H in cellulose chains appears at 3433 cm 1. Another band appearing at 1033 cm 1 represents the C–O symmetric vibration of ether bonds for cotton [32,33]. After coating of the cotton with SA/silica–kaolinite network (Fig. 1b), new bending and stretching peaks appeared at about 1081 and 780 cm 1 related to Si–O–Si (siloxane groups) and Si–O–Al of SiO2–kaolinite particles [5,6]. These changes showed that inorganic materials are successfully incorporated onto the cellulose. New bands appearing at 1634 and 2884 cm 1 can be explained as ester links and CH2 asymmetric stretching of SA in the cross-linked cotton [19,22,23]. A band at 3424 cm 1 was shifted to 3309 cm 1 and a new band appeared at 1334 cm 1. These results confirm the changes in inter- and intra-chain hydrogen bonds of cotton after coating with SA/silica–kaolinite network [22].

Fig. 3. XRD patterns for SiO2–kaolinite particle.

Fig. 4. XRD patterns for (a) untreated cotton, (b) SA cross-linked cotton, (c) cotton sample coated with SA/10% silica–kaolinite network.

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Fig. 2 shows the mechanism for cross-linking of cotton with SA in the presence of silica–kaolinite. In water, cellulose carries negative charges, which together with the negative charges of the silica–kaolinite causes an electrostatic repulsion. CTAB used in this study significantly increased the dispersability of the silica–kaolinite in water. In other words, by addition of CTAB to the bath for dispersion of particles, this electrostatic repulsion is postponed, which causes a better interplay of electrostatic and van der Waals forces leading to a greater affinity of silica–kaolinite to cotton [34]. To improve the performance of inorganic particles on cotton, SA was used in the presence of SHP as a catalyst. UV irradiation produces the free radicals on SA which directly bind to cotton free radicals producing esteric cross-linkages. In a further reaction, silica–kaolinite particles can react with carboxylate anions and radicals of SA through formation of electrostatic interactions and ester linkages [22,34]. This leads to a greater affinity of silica–kaolinite particles to cotton [23]. This result is also supported by other authors for the photo-reduced SA in the presence of different nano-particles under UV irradiation [35]. 3.2. Evaluation of morphology by XRD Figs. 3 and 4 present X-ray diffractograms recorded for the SiO2–kaolinite as well as for cotton samples coated with different contents of inorganic particles in SA/silica–kaolinite network. Three intensive peaks at 2h = 12.4°, 26.6° and 36.5° can be seen for SiO2–kaolinite powder representing d(0 0 1), d(0 0 2) and d(0 0 3) Bragg’s reflections of the characteristic layer structure in kaolinite. Another intense peak at 2h = 20.9° is assigned to silica phase for SiO2–kaolinite [4–6]. Diffraction peaks in Fig. 4a are characteristic of cellulose I, with three reflections at 2h = 18.8°, 21.1°, 25.9° and 28.9° representing d(1 0 1), d(1 0 1), d(0 2 1) and d(0 0 2) Bragg’s reflections [36]. The crystallite form of cotton was not changed by SA and silica–kaolinite network. On this basis, it can be concluded that neither SA nor silica–kaolinite changes the crystalline structure of cellulose. Subsequently, the effects of these treatments must be confined to the cotton surface. Other authors have confirmed this phenomenon after crystallinity measurement of cotton in cases where different cross-linking agents were used for cotton modification [37]. They showed that only amorphous regions of cellulose were accessible for esterfication by cross-linkers [38]. 3.3. Determination of thermal properties Fig. 5 illustrates measured DSC curves of the untreated and SA cross-linked fibers together with samples coated with SA/silica– kaolinite network. A peak at about 63 °C was generated in the curve for the untreated cotton fiber due to a glass transition occurring in the amorphous regions of the cellulose chains. After crosslinking of cotton with SA, the glass transition temperature (Tg) showed an increase to 68 °C. Coating of cotton with SA/1% silica– kaolinite increased Tg to 75 °C followed by a greater increase to 84 and 120 °C as the silica–kaolinite concentrations were increased to 5% and 10%, respectively. This result shows that silica and kaolinite may act as a heat and thermal barrier that influences on the heat transition toward cellulose molecular chains and the absorbed heat for chain movements [18]. On the other hand, SA improved the interaction between cotton surface, silica particles and the layered kaolinite which effectively restricted the motions of the molecular segment in cellulose. A peak at 318 °C was generated in the curve for the cotton fiber usually associated with the melting and decomposition occurring in the crystalline regions of the cellulose chains and subsequent formation of volatile products [4]. After coating of the cotton with different SA/silica–kaolinite networks, the melting temperatures (Tm) were increased to 320, 329 and

Fig. 5. DSC curves for (a) untreated cotton, (b) SA cross-linked cotton, (c) cotton coated with SA/1% silica–kaolinite network, (d) cotton coated with SA/5% silica– kaolinite network, (e) cotton coated with SA/10% silica–kaolinite network.

331 °C respectively, depending on the content of silica–kaolinite used. This finding is also further supported by other authors [39]. Our previous studies showed that thermal behavior of fibers is influenced by its molecular structure, density, crystallization level, crystal orientation angle and mobility of molecular chains in amorphous and crystalline regions [40,41]. Our ATR results indicated some changes in chemical properties of the fibers after coating of network and changes in thermal characteristics could also be expected. Fig. 6 summarizes the thermal degradation of the untreated cotton together with those samples coated with different SA/silica–

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Fig. 6. TGA curves for (a) untreated cotton, (b) SA cross-linked cotton, (c) cotton coated with SA/1% silica–kaolinite network, (d) cotton coated with SA/10% silica–kaolinite network.

kaolinite networks. The TGA curves of cotton generally consists of three regions of 1, 2 and 3 as the initial, main, and char decomposition regions. In the first part, the changes of the thermal properties and weight loss of fibers are due to some physical damages occurring mostly in the amorphous region of the cellulose. The main thermal stage occurs in the second region, where the weight loss is significant. Researchers showed that glucose together with all kinds of combustible gases are generated in this region [42]. Moreover, thermal degradation in this region takes place in the crystalline region of the cellulose fibers. Production of char occurs at the third region at temperatures higher than 360 °C. This process continues by dewatering and charring reactions, releasing water and carbon dioxide and increasing the carbon and charred residues. Generally, the carbon content in the decomposed products becomes higher and the pyrolysis will develop from amorphous regions to crystalline regions in cellulose [43]. Cross-linking of cotton with SA increased the thermal stability of cotton at different regions and it was intensified after incorporation of silica–kaolinite in network. This may suggest that the physical structure of the substrate has a significant effect on the thermal properties of SA/silica–kaolinite coated fibers [44]. As it was stated by XRD and ATR results, SA can cross-link preferentially the amorphous regions rather than the crystalline structures. Generation of ester linkages on cotton resulted in capability of migration and bonding of more silica–kaolinite particles on the cotton surface. This resulted in an enhancement in thermal stability and increasing char content after TGA analysis of coated samples. A increased amount of char is ascribed to the high heat resistance, the heat insulation effect and the mass transport barrier exerted by the silica–kaolinite particles themselves, which is a measure of flame retardancy [45]. Other researchers suggested that the flame-retardant effect found in polymer–clay nanocomposites arises from the formation of char layers, which comes from the dispersion of the clay structures within the nanocomposites [46]. In other word, inorganic particles slow the escape of volatile decomposition products during the cotton thermal analysis resulting in improvement of char formation [30]. Thermal stability is an area studied by different researchers in the field of safety and protective aspects of textile products. Here we confirm that silica–kaolinite decreases the thermal degradation of cotton, which is an advantage for human safety.

3.4. Microscopic characterization The SEM images of the untreated and SA cross-linked cotton samples together with those coated with SA/silica–kaolinite network are shown in Fig. 7. It can be seen that the untreated and SA cross-linked cotton fibers have a relatively smooth surface. The SEM images of the cotton fibers coated with SA/1% silica– kaolinite show a formation of some aggregated silica–kaolinite particles on the surface of cotton. Any increase in silica–kaolinite content to 5% and 10% resulted in an increase in aggregation and stabilization of particles on cotton surface. Generally, nano-particles are able to aggregate on the surface of textiles, which depends on several factors such as size, mobility, end-group functionalities, relative composition, and molecular architecture [47]. In addition, nano-particles with appropriate functionalities can provide a significant control over hydrophobicity or hydrophilicity of the modified polymer surfaces [48]. As mentioned previously, the ATR spectra of the samples illustrate that hydroxyl groups of cotton can make a cross-link with SA resulting in generation of new bonds with silica–kaolinite particles. These interactions are strong enough to enable aggregation of inorganic materials on the cellulose surface as a result of their high surface area. Other authors have confirmed this phenomenon in cases where nano-particles were incorporated into multilayer organic coatings [49–52]. Table 1 depicts the presence of chemical elements on the surface of the untreated cotton as well as on the surface of the various SA/silica–kaolinite coated samples as examined by EDX analysis. It can be seen from Au peaks that gold thinly covered the surfaces of the samples; and there is no Si and Al present on the untreated and SA cross-linked cotton fibers. EDX analysis of coated textiles indicated the interactions between SA, silica, kaolinite and cellulose leading to stabilization of the particles containing Si and Al. We observed a strong tendency of silica–kaolinite particles to cross-link on the cotton surface using SA, which is also further supported by other authors [35]. 3.5. Water contact angle analysis A probe fluid of water was used in this study. Fig. 8 illustrates variation in contact angles of the samples versus water drop age.

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Fig. 7. SEM images of cotton fibers at 2500 and 7500: (a and b) untreated cotton, (c and d) SA cross-linked cotton, (e and f) cotton coated with SA/1% silica–kaolinite network, (g and h) cotton coated with SA/5% silica–kaolinite network, (i and j) cotton coated with SA/10% silica–kaolinite network.

The amount of contact angle decreased after cross-linking of cotton with SA. Through incorporation of silica–kaolinite in coating, the amounts of contact angle continued to decrease. The extent of the decrease may be due to two different factors. SA is able to pro-

vide cross-links with cellulose functional groups, hence causing a dense macromolecular network with less capillary spaces for water molecules in the amorphous regions. On the other hand, a decreased number of the functional groups available for bonding

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Table 1 EDX analysis results of element compositions for untreated and SA cross-linked cotton samples together with those coated with SA/silica–kaolinite network. Sample

Untreated cotton Cotton cross-linked with SA Cotton coated with SA/ silica–kaolinite network

Silica–kaolinite content (%) – – 1 5 10

advantage of SA/silica–kaolinite coating to produce hydrophobic textiles [53,54].

Content of element (%)

3.6. Optical properties Al

Si

Na

Au

– – 0.51 1.90 2.64

– – 1.97 3.68 5.12

– – 0.42 1.05 3.13

100 100 96.28 89.52 80.11

with water as a result of the generation of the numerous crosslinks in the SA treated fibers is another reason for an increment of the contact angle. Furthermore, SiO2–kaolinite is hydrophilic in nature due to its surface hydroxyl groups and high surface area, it is capable of forming a denser inorganic–organic macromolecular network with SA, thereby cellulose coated with SA/silica– kaolinite is less accessible for water molecules. This could be an

Fig. 9 illustrates measured reflectance spectra of the untreated cotton and the samples coated with different SA/silica–kaolinite network. There was not any difference between the untreated and SA cross-linked cotton fabrics. The reflectance values for the cotton coated with SA/1% silica–kaolinite network increased in the considered spectral region followed by more increase as the silica–kaolinite content increased in coating. This can be due to two factors: first, surface property of the coated fibers may influence the reflectance properties. Preparation of silica–kaolinite network on cotton surface may increase the surface roughness due to its larger particle size resulting in an increase of scattering throughout the visible range [55]. The ionization of silica–kaolinite is the second factor influencing the reflectance of fibers. In this phenomenon, a core electron of silica atom filling in an inner-shell

Fig. 8. Variation in contact angles of different samples measured in this study.

Fig. 9. Reflectance of the cotton fabrics coated with different SA/silica–kaolinite networks.

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vacancy is removed, leaving a vacancy. An electron from a higher energy level is then emitted, resulting in a release of energy. This energy can contribute to more reflection of the resultant SA/silica–kaolinite coated samples. The energy can also be transferred to another electron, which is ejected from the atom as an Auger electron [2,5]. We have shown similar results in our previous studies on various polymer nanocomposites containing silica, kaolinite, clay, zirconia or silver nanoparticles [2,3,5,6,56,57]. Additionally, some researchers have demonstrated the increment in scattering as a result of the presence of OH groups on the surface of silica or SiO2-based materials and various organic/inorganic hybrid SiO2 coatings [58]. This result is incidentally consistent with our other results obtained from FTIR and EDX analyses.

4. Conclusion Silica–kaolinite and SA were used for fabricating a thermal resist and hydrophobic surface on cotton through a UV radiation technique. Embedding of silica–kaolinite particles in the coating was performed by a reaction of SA and cellulose chains. This reaction resulted in the attachment of inorganic particles to the surfaces of the cotton fibers. The ATR technique showed the crosslinking reaction among the carboxylic acid group of SA, hydroxyl groups of silica–kaolinite and cellulose to form esteric links under the UV curing process. The results obtained from DSC and TGA tests demonstrated an enhancement of thermal properties of the coated samples. This can be as a result of the high heat resistance, heat insulation effect and the mass transport barrier of silica–kaolinite embedded in coating. Cross-linking of cotton with SA increased the average contact angles for the water used. Furthermore, silica–kaolinite increased water contact angle, which can be attributed to a denser inorganic–organic macromolecular network on cellulose. In conclusion, optical measurement stated that the cotton coated with SA/silica–kaolinite network reflects a higher portion of photons compared to the untreated sample. The reflectance curves of composites increased toward the visible region, which could be attributed to the surface roughness, larger agglomerates of particles and excitation state of silica atoms. References [1] Miyamoto N, Kawai R, Kuroda K, Ogawa M. Adsorption and aggregation of a cationic cyanine dye on layered clay minerals. Appl Clay Sci 2000;16:161–70. [2] Parvinzadeh M, Eslami S. Optical and electromagnetic characteristics of clayiron oxide nanocomposites. Res Chem Intermed 2011;37:771–84. [3] Parvinzadeh M, Moradian S, Rashidi A, Yazdanshenas ME. Effect of addition of modified nanoclays on surface properties of the resultant polyethylene terephthalate/clay nanocomposites. Polym-Plast Technol Eng 2010;49:1–11. [4] Parvinzadeh Gashti M, Moradian S. Effect of nanoclay type on dyeability of polyethylene terephthalate/clay nanocomposites. J Appl Polym Sci 2011;125:4109–20. [5] Parvinzadeh Gashti M, Eslami S. Structural, optical and electromagnetic properties of aluminum–clay nanocomposites. Superlattice Microstruct 2012;51:135–48. [6] Parvinzadeh Gashti M, Almasian A. Synthesizing tertiary silver/silica/kaolinite nanocomposite using photo-reduction method: characterization of morphology and electromagnetic properties. Compos Part B – Eng 2012; 43:3374–83. [7] Sinha Ray S, Okamoto M. Polymer layered silicate nanocomposites: a review from preparation to processing. Prog Polym Sci 2003;28:1539–641. [8] Herney-Ramirez J, Vicente MA, Madeira LM. Heterogeneous photo-Fenton oxidation with pillared clay-based catalysts for wastewater treatment: a review. Appl Catal B: Environ 2010;98:10–26. [9] Isabel Carretero M. Clay minerals and their beneficial effects upon human health. A review. Appl Clay Sci 2002;21:155–63. [10] Parvinzadeh M. Surface modification of synthetic fibers to improve performance: recent approaches. Global J Phys Chem 2012;3:2. [11] Parvinzadeh Gashti M, Willoughby J, Agrawal. Surface and bulk modification of synthetic textiles to improve dyeability, textile dyeing, In: Peter J, Hause (editors), ISBN: 978-953-307-565-5, InTech; 2011. .

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