E journal mar apr '18 by TheTextile Association (India)

SPINNING

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Effect of Machine Variables on Rotor Yarn Properties Harish. R. Jambur1, Prof. P. P. Kolte2, Dr. V. G. Nadiger2* & Prof. A. M. Daberao2 1 Bapuji Institute of Engineering & Technology 2 SVKMs, NMIMS, MPSTME, Centre for Textile Functions Abstract As Open end technique is becoming very popular, an effort is made to see that how machine variables will affect the properties of the open end yarn. In this paper, we have studied the effect of various parameters of the rotor spinning machine i.e. opening roller speed, rotor diameter, rotor speed and twist of yarn on the yarn properties. The results indicate that these variables significantly affects unevenness [U%],coefficient of variation (CV%), imperfection index [IPI] and lea strength of the yarn. These parameters have to be optimized in order to get better quality of open end yarn depending up on their end uses. The opening roller speed influences the unevenness [U%], imperfection and yarn strength of yarn to great extent; however the speed has to optimize. The influence of change in rotor diameter is studied, it considerably influence the lea strength of the yarn. This may be due to wrapper fibers.Whereas rotor speed are influences on coefficient of variation (CV%),twist factor has an influence strength of yarn. However, all these parameters have to be optimized in order to get better quality of open end yarn depending up on their end uses. Keywords Opening roller speed, Rotor diameter, Rotor speed, Twist, Rotor yarn properties.

Rotor spinning is considered as most suitable and successful spinning process among many open-end spinning methods [6]. For high production rate of yarn, open-end spinning principle is significantly acceptable not only by using low to medium grade cotton but also from wastage at relatively lower cost than any other existing spinning technology [7]. Cotton yarn produce by rotor spinning is more uniform, fuller, aerated and regular in strength [8]. The quantity of production on rotor spinning has increased in recent years [9]. Now a days, rotor spinning system is rising *All correspondences should be addressed to, Dr. V. G. Nadiger, SVKMs, NMIMS, MPSTME, Centre for Textile Functions, Shirpur, Maharashtra- 425405 Email : nadigervinay.7@gmail.com March - April 2018

due to the considerable reduction in space and personnel [10-11]. The positive impact of spinning parameters on yarn properties were accessed by imperfection index[12]. The yarn characteristics of rotor spun yarn are affected by various factors related to raw material, machine parameters and processing parameters. Many researchers have already investigated the effect of these parameters on yarn quality from different outlooks[7-15]. Rotor yarns are less spun yarn because of bling of fibres in the spun yarns are not as as ring yarns [7].

irregular compared to the ring multiple doubling or back dourotor groove. In addition, rotor affected by roller drafting wave

2. Materials and Methods 2.1 Materials The cotton fiber properties of the material selected for this study is shown by Table 2.1. The cotton fiber properties are assessed by Uster-HVI spectrum instrument. The processing mixture of fiber composed of 30% Brahma cotton, 15% Comber cotton and 55% Flat strip (dropping). The fibers are mixed together homogeneouslyby sandwich mixing method.

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1. Introduction New spinning technologies introduced in late sixties and early seventies, only rotor spinning sustained its promise and in the years to follow, it established itself as a worthy alternative to ring spinning in the course and medium count range [1-3]. The reasons for its phenomenal growth were very high productivity, around 5-8 times that of ring system, and amenability to automation and elimination of roving and winding process [3-5].

SPINNING Table 2.1. Properties of the cotton fiber

Quality Parameters

Details

Particulars

Parameters

Fiber length (mm)

28-30

Front roller delivery speed

300 m/min

Fiber micronairevalue (Âľg/inch)

3.7

Number Of Doubling

Uniformity Index (%)

80.0

Feed Hank

0.100 Ne

Short Fiber Index (%)

8.3

Delivery Hank

0.100 Ne

Moisture (%)

7.5

Front zone roller setting

38 mm

Maturity Index (%)

0.85

Back zone roller setting

32 mm

Draft

2.2 Methods For producing 21s Ne count, the homogeneous mixture of cotton processed through spinning process. The parameters of the process are mentioned in Table 2.2, Table 2.3, Table 2.4 & Table 2.5 respectively. Table 2.2. Blow Room Machine Particulars

Particulars

Speed (rpm)

Roto Flock

400

Blendo clean

350

Ulti clean

450

Maxi clean

450

Shell roller speed

Table 2.3. Carding Machine Particulars

Particulars

Parameters

Feed hank

0.10 Ne

Delivered hank

0.10 Ne

Delivery speed

180 m/min.

Production 8Hr at 95% efficiency

400 Kg/Card/

Table 2.4. Draw Frame Machine Particulars

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Table 2.5. Rotor Machine particulars

Particulars

Parameters

Rotor Speed

80000 rpm

Opening Roller Speed

9000 rpm

Delivery Speed

95 rpm

Doffing tube

50x55x170mm

Draft

80-250

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In this study, to produce rotor yarn of 21s Ne count BD 030, Elitex type rotor spinning machine was used. The yarn were produced depends on various variables. Firstly, Opening roller speed changed from 7000 rpm, 8000 rpm and 9000 rpm with rotor speed 50000 rpm,rotor diameter34 mmand TPI 25 constant. Secondly, Rotor diameter changed from 34 mm, 43 mm, and 54 mm, with Rotor speed 50,000rpm, opening roller speed 8,000 rpm andTPI 25. Thirdly, rotor speed changed 50000 rpm and 60000 rpm with opening roller speed 8,000 rpm,rotor diameter34 mm andTPI 28. Fourthly, TPI changed from 22, 25 and 28 with rotor speed 50000 rpm, opening roller speed 8,000 rpm and rotor diameter34 mm. Firstly, drawn slivers were feed through a sliver guide via a feed roller and feed plate to rapidly rotating opening roller. The rotating teeth of the opening roller comb out the separate fibers from the sliver clamped between feed plate and feed roller. Then the fibers were feed to inside wall of the rotor after completing action in transport channel. The fibers moved forward to the rotor groove from the conical rotor wall by centrifugal forces in the rapidly rotating rotor. Finally, the yarn formed in the rotor is continuously taken off by the delivery shaft and the pressure roller through the nozzle and the draw off tube and wound onto a cross wound package. [7] Figure 2.1 represents the basic working principle of rotor spinning system and flow diagram of yarn preparation respectively.

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SPINNING

Figure 2.1 Basic working principle of rotor spinning system[7].

Figure 3.1 Variables of opening roller speed 7000, 8000, 9000 rpm with rotor speed 50,000 and twist per inch 25 constant

3. Results and Discussion Table 3.1, Fig 3.1 to Fig 3.4 shows that when the opening rollers speed is increased, the U% of the yarn, imperfection and strength of the yarn has improved.Increase in the opening roller speed; fiber individualization, U% as well as strength of the yarn improves. The fiber extent as improved the draft is also increased there by the U% is has improved the imperfection has decreased and strength of the yarn has improved. However we can clearly say that opening roller speed of 8,000 rpm can be optimized since the imperfections and U% the CV% has improved to the great extent. However after 8,000rpm of opening roller when it is increased due to centrifugal force of opening roller fiber extent decreases considerably thereby detoriating the yarn quality . Hence opening roller speed has great bearing on the property of the yarn.

Figure 3.2 Opening roller 7000 rpm

Table 3.1. Variables of opening roller speed 7000, 8000, 9000 rpm with rotor speed 50,000 and twist per inch 25 constant

CV%

Thin/km (-50%)

Thick /km (+50%)

Neps/km (+280)

Rel. cnt (%)

Avg. lea strength in lbs

7000

14.11

17.77

117

108

100

65.1

8000

10.96

13.88

100

53.8

9000

11.61

14.64

100

71.9

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Roller Speed (rpm)

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Figure 3.3Opening roller speed 8000 rpm

Figure 3.5 Variables of Rotor diameter 34, 43, 54 mm, TPI 25. Rotor speed 50,000 rpm, opening roller speed 8,000 rpm.

Figure 3.4 Opening roller speed 9,000 rpm

Table 3.1, Fig 3.1 to Fig 3.4 shown thatrotor diameter has little influence on U%, CV% and yarn imperfection but it has great bearing on strength of yarn this can be seen in the results that is keeping twist per inch rotor speed opening roller speed constant. Tensile strength of the yarn decreases.

Figure 3.5. 1(a) Rotor diameter 34mm

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When rotor diameter is increased to 34mm to 54mm this may be due to fact that as the rotor diameters increases the wrapper fibers are increased which in turn decreases the tensile strength of the yarn.Hence rotor diameter has to be optimized.

Figure 3.5. 1(b) Rotor diameter 43mm

Table 3.2. Variables of Rotor diameter 34, 43, 54 mm, TPI 25. Rotor speed 50,000 rpm , opening roller speed 8,000 rpm.

Rotor Diameter

CV%

Thin/km (-50%)

Thick /km (+50%)

Neps/km (+280)

Rel. cnt (%)

Avg. lea strength in lbs

34 mm

14.11

17.77

108

212

100

61.9

43 mm

10.96

13.88

100

57.3

54 mm

11.61

14.64

145

242

100

51.9

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SPINNING

Figure 3.5.2 - Rotor diameter 54mm Figure 3.6.2. Rotorspeed 65,000 rpm

From the table 3.2 and figure3.5 to figure3.5.2 results even though increase in rotor speed deteriorate the yarn evenness. It was observed, when the speed is increased from 50,000 to 65, 000, there is no difference in the CV%.

From the table 3.3 and figure3.6 to fig 3.6.2, the twist when increased from 22TPI to 28TPI,the lea strength of the yarn gradually increases and reaches optimum

Table 3.3 Variables of Rotor speed 50,000 and 65,000 with constant TPI 28

Rotor Speed (rpm)

CV%

Thin/km (-50%)

Thick /km (+50%)

Neps/km (+280)

Rel. cnt (%)

Avg. lea strength in lbs

50000

11.77

15.01

182

100

65000

12.89

16.15

102

100

Figure 3.6. Variables of Rotor speed 50,000 and 65,000 with constant TPI 28

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Figure 3.6.1 - Rotor speed 50,000 rpm March - April 2018

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level A higher twist produces yarn with a higher co efficient of friction ,hence increase in the strength , even though it has very little or no effect on uniformity of the yarn.

SPINNING Table 3.4. Variables of TPI 22, 25, 28 with constant rotor speed 50,000 and opening 8,000

TPI

CV%

Thin/km (-50%)

Thick /km (+50%)

Neps/km (+280)

Rel. cnt (%)

Avg. lea strength in lbs

13.13

16.52

100

48.9

25 28

14.27 13.36

18.13 16.98

47 18

147 138

210 224

100 100

54.9 59

Fig 3.7. Variables of TPI 22, 25, 28 with constant rotor speed 50,000 and opening 8,000

Figure 3.7.3. Twist per inch 28

Figure 3.7.1 Twist per inch 22

Conclusions Result and discussion clearly show that ◆ Machine variable has definite effect on yarn properties. ◆ Rotor diameter and rotor speed influences strength of yarn considerably. ◆ Opening roller speed has influences uniformity, imperfection and strength of the yarn. ◆ Twist influences strength of the yarn considerably. Hence it is always advisable to optimize these parameters for the open end yarn depending on their end uses.

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Acknowledgment: The Author's want to acknowledge to the Dr. J S Muralidhara, Principal, White Pencil College, Bangalore. Kind support of project and industrial support by Production Manager Girish S.Joshi of SohamCottspinn, Haveri, Karnataka and AnjaneyaCotton Mill, Davangere, Karnataka. Tests carried in lab especiallyUster Evenness Tester.Mr.Ravindra K.B.B.I.E.T. Collage,Davangere for photographs of samples. Figure 3.7.2. Twist per inch 25

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References 1. Barella A., Manich MA., Marinob NP., & Garofalob .J. (1983). Factorial studies in rotor March - April 2018

SPINNING

2. 3.

4. 5.

7. 8.

spinning of part -I: Cotton Yarns. The Journal of the Textile Institute74, 329-339. Istiaque, Sharma N (1990). Fiber disorder in open end spinning. Grosberge P., Mansoor S.A. High speed open end rotor spinning (1975). The Journal of the Textile Institute 66, 389-396. Lord, P.R.(1976). The Structure of Open-End Spun Yarn.The Textile Research Journal, 41, 778-784. Barellaa, A., Turaa J.M., Vigoa,J.P., Esperona, H. O. (1976). An application of mini-computers to the optimization of the open-end-spinning process. Part ii: Consideration of the case of three variables. The Journal of The Textile Institute, 67, 325-333. Khan, M.K.R., Rahman, H. (2015). Study of Effect of Rotor Speed, Combing-Roll Speed and Type of Recycled Waste on Rotor Yarn Quality Using Response Surface Methodology. IOSR. Journal of Polymer and Textile Engineering, 2,47 55. Klein, W, Manual of Textile Technology, The Textile Institute, (1995), 20-25. Nawaz, S.M., Jamil, N.A., Iftikhar, M. and Farooqi, B.(2003). How Does Open-End Processing Variables Effect Imperfections for Different Yarn Count.Pakistan Textile Journal, 22-26. Ishtiaque, S.M., Spinning of Synthetic Fibres and Blends on Rotor-Spinning Machine. Indian Journal of Fibre and Textile Research,17, 224230,(1992).

10. Ahmed, S., Syduzzaman, M., Mahmud, M.S., Ashique, S.M. and Rahman, M.M. (2015). Comparative Study on Ring, Rotor and Air-Jet Spun Yarn. European Scientific Journal,11, 411-424. 11. Rameshkumar, C., Anandkumar, P., Senthilnathan, P., Jeevitha, R.,& Anbumani, N. (2008) Comparative Studies on Ring Rotor and Vortex Yarn Knitted Fabrics. Autex Research Journal, 8,100-105. 12. Md. ReazuddinRepon., Rajib Al Mamun., Selim Reza., MithunKumer Das., Tarikul Islam.(2016). Effect of Spinning Parameters on Thick, Thin Places and Neps of Rotor Spun Yarn, Journal of Textile Science and Technology, 2, 47-55. 13. Gnanasekar K., Chellamani P., Karthikeyan S.(1990). Influence of rotor speed in open end spinning on yarn quality, India Journal of Fiber and Textile Research, 15, 164-168. 14. Ishtiaque S.M., Kumar P.(1994). Impact of rotor and opening roller speed on configuration of fibers in yarn, India Journal of Fiber and Textile Research, 19,71-75. 15. Bagwan A.S., Patil A.(2016).Optimization of Opening Roller Speed on Properties of Open End Yarn, Journal of Textile Science & Engineering, 6, 2-5. 16. Kolte P.P., Patil K.R., Kulabhaskar Sing, Daberao A.M., (2017).Effect of Twist on Yarn Properties. International Journal on Textile Engineering and Process, 3, 19-23. ❑❑❑

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Comparative Study of Wool Descaling Using Various Techniques Ravindra Kale*, Prerana Kane, Jidnyasa Patil & Arjunsing Girase Department of Fibers and Textile Processing Technology, Institute of Chemical Technology, Abstract Wool fabric was descaled using different reagents & processes and their combinations. A comparison between various techniques like chlorination using dichlorodicyanuric acid (DCCA), polyurethane based commercial product, enzyme, plasma treatment and their combinations was made to choose the best process for scale removal. It was found that a combination of plasma and enzymatic treatment gave best results in terms of hydrophilicity, whiteness and brightness index. Also the loss in tensile and tear strength were found to be less in comparison to other techniques. Change in surface morphological of the fibre was studied using scanning electron microscope. Keywords contact angle; descaling; surface energy; wettability; wool

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Graphical Abstract:

1. Introduction Wool is a natural protein fiber made of keratin protein. The outer surfaces of wool fibers have flattened overlapping cuticle cells which provide a protective sheath around cortical cells. The cuticle has many layers. The upper layer, epicuticle is composed of lipoproteins where lipoid part of lipoproteins is bound by the sulfoester bond with proteinous part. The lipoproteins are connected with upper layer of exocuticle which is crosslinked by disulfide links. The surface morphology of *All correspondences should be addressed to, Dr. R. D. Kale, Dept of Fibers & textile Prossing Tech. Institute of Chemical Technology Matunga, Mumbai - 19 Email : rd.kale@ictmumbai.edu.in 384

wool plays an important role in wool processing, since the hydrophobic nature of the cuticle and the high crosslinking density in the outermost fiber surface creates a natural diffusion barrier, making wool hydrophobic and inert to many chemicals [1-4]. The descaling treatment is to get the scales partly removed, or the edges from the overlapping scale smoothed. So wool surface must be modified before processes to improve hydrophilicity and dyeability. In dichlorodicyanuric acid (DCCA), descaling treatment a slow hydrolysis of the DCCA salt reacts to release hypochlorous acid (HClO) which acts as an oxidising agent [5-8]. While in enzymatic treatment, protease enzyme penetrates into amorphous region and causes swelling and it leads to changes in the disulphide region of cystine than amide components during chemical degradation. The important chemical reactions occurred during enzyme treatment are given in Figure 1.1 [9].

Figure 1.1: Chemical reactions between enzyme and wool fiber

In plasma treatment, when woollen materials in top or fabric form pretreated with glow discharge in presence of non-polymerizing gases like air, oxygen and nitrogen, March - April 2018

PRETREATMENT

Polyurethane based commercial product treatment is given to the wool fibres to achieve adequate adhesion of the polymer to the fibre surface to avoid deterioration of the fabric handle caused by the inter fibre bonding [11]. The aim of this work is to choose the best process for scale removal by comparing various descaling techniques like chlorination using DCCA, polyurethane based commercial product, enzyme, plasma treatment and their combinations. 2. MATERIALS AND METHODS 100 % wool fabric with plain weave (22.26 micro) with GSM of 180. DCCA, sodium salt (96%), Cresol Red dye, potassium permanganate (KMnO4) and sodium bicarbonate (NaHCO3) was purchased from Aldrich (Mumbai, India). Protease enzyme was supplied by Novozymes (Mumbai, India). Saragen SO, a dispersing agent was supplied by Sarex Chemicals, Mumbai, India. A polyurethane coating agent was obtained from one renowned company in Mumbai, India. Since the company requested not to disclose its name, this product was termed as commercial product (CP). 2.1. Wool descaling treatment The descaling of the wool was performed by conducting experiments referring the earlier literature as cited in each section and only optimized results are reported. 2.1.1. Treatment with DCCA Treatment with DCCA was given in a bath containing 1gpl DCCA and 1.5 -2 % owf (on weight of fabric) potassium permanganate at 200C and pH 3.5-4.0 for 60 minutes in an Atlas LP2 Launder-o-meter. The treated wool fabric was rinsed with warm water followed by neutralization treatment with 5% owf sodium bicarbonate at 400C and pH 8.5-9 for 20 minutes. This was followed by washing and air drying. The liquid ratio was maintained at 30:1 in all these treatments [8]. 2.1.2. Enzymatic treatment (E) Protease enzyme treatment was carried out by batch March - April 2018

method at a liquor ratio of 25:1 using a Rota Dyer machine (Rossari® Labtech, Mumbai, India) at 550C and pH 8.5 for one hour using 3 % (owf) enzyme. Treated fabric was subsequently deactivated at 900C by immersing it in hot water for 5 minutes followed by rinsing and drying at room temperature [12-13]. 2.1.3. Plasma treatment (P) A dielectric barrier discharge (DBD) atmospheric plasma device was used. The distance between the electrodes was 2 mm. The samples were placed between the electrodes and passed continuously at the speed of 0.45 m/minute. For generating plasma, air and argon were used under a constant power of 5Kv and 0.8 ampere current. The samples were treated for 40 seconds in the plasma [12-13]. 2.1.4. Treatment using Commercial Product (CP) This treatment was carried out by Pad-dry-cure-steam method with 70% expression with pad solution of 25 gram per liter CP, 20 gram per liter Saragen SO, 2 gram per liter Sodium bicarbonate at pH 7-7.5 which also act as cross linking agent. After the treatment the samples were dried at 1000C in an oven, cured at 1600C for 1 minute and finally steamed at 1050C for 3 minutes. Then the samples were washed properly and air dried. 2.1.5. Combine treatment Various combination of decaying treatment was tried like enzyme-DCCA, plasma-CP, plasma-enzyme, CPenzyme and DCCA- enzyme following the procedure as mention earlier [12-14]. 2.2. Assessment methods 2.2.1. Wettability The wettability of the treated and untreated fabrics was evaluated by two different tests: wicking ability and measurement of surface energy. In order to measure the wicking distance, the fabric samples were cut into 3 × 1 inches and held at the top of a measuring cylinder of 100ml capacity by a plastic tape. The cylinder was filled up to 100ml with distilled water. The bottom edge of the fabric was immersed by 2 mm in distilled water for 1 minute. The distance covered by the water was then measured. The test was repeated thrice for each sample [15]. 2.2.2. Measurement of Surface Energy The wettability of wool specimens (1 cm×2 cm) was evaluated by estimating the surface energy by three different methods. It is determined in terms of dy385

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the outer surface of wool fiber (30-50 nm) is modified due to plasma etching and surface oxidation. Plasma attacks the wool fiber surface like gun and partially abrades the fatty acid layer from the cuticle and parts of the exocuticle. Simultaneously, there is surface oxidation by oxygen radical which introduces new anionic groups i.e., sulphonic and carboxylic acid groups. Carboxylate groups are derived from the backbone of the protein chains and sulphonate groups by oxidation of disulphide bonds in the cuticle cells [9-10].

PRETREATMENT namic water adsorption mass using Tensio CAD® 140 (Cad Instruments, France) at room temperature. 2.2.3. Contact Angle measurement Contact angle of the fabric samples was measured by the Sessile drop method, using Rame-hart Model 200 Standard Contact Angle Goniometer where a drop of double distilled water with constant volume (4µL) was placed on a sample surface. Contact angle was measure after 10 seconds. 2.2.4. Drop test Colour drop (10 µL) prepared by dissolving Cresol Red dye 1gm in 100ml distilled water was put on the fabric surface and their images were taken using camera. 2.2.5. Whiteness Index The whiteness of wool fabrics was evaluated by Computer Colour Matching method using CIELAB colour space (Computer Colour Matching System- Spectra Scan 5100+, Data Color International, USA) reflectance spectrophotometer. The parameters taken for all the measurements were sample aperture size of 6.6 mm with standard illuminant D65 and 100 standard observer. 2.2.6. Mechanical Properties Tensile properties of fabrics were measured using H150KU-UTM tensile testing machine Tinius Olsen, United States of America, as per ASTM D 5035. Tearing strength was measured using Elmendorf tear tester as per ASTM D1922 standard method.

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2.2.7. Scanning Electron Microscopy The surface morphologies of the untreated and treated wool samples were evaluated by Scanning Electron Microscopy (SEM) using JEOL JSM-5400 (USA) scanning electron microscope.

Figure 3.1 shows that plasma, enzymatic, chemical or combined treatments can partially destroy or remove the covalently bound fatty layer from the surface of wool fabric, thus improving the hydrophilicity of wool fabric to a certain degree [16]. In general, CP and enzymatic treatment showed lower improvement in wettability than other treatments. From Table 3.1, it was observed that increase in surface energy of wool by various descaling treatments. As per Owens Wendt method the surface energy was highest for P+E treated wool samples which were supported by other two viz. Wu and Fowkes methods. It was also observed that the surface energy decreased marginally by around 10% due to only enzyme treatment while the surface energy increased by 90% due to only plasma treatment with reference to control. Whereas combination treatment with plasma followed by enzyme increased the surface energy by around 250%. This may be due to the surface etching because of plasma treatment and weakening of disulphide linkage which is further specifically degraded easily by enzyme treatment. The proportion of polar components got enhanced by this combined treatment than other treatments resulting in improved hydrophilicity. During subsequent enzyme treatment, protease molecules not only hydrolyze the cuticle of the fibers but also penetrate deep inside the fibers, resulting in the removal of smaller peptide and protein segments with an increase in amorphous region. Thus plasma treatments facilitated the accessibility of protease creating large surface area in fibers and promoting the proteolytic reactions, making more underlying proteins (hydrophilic surface) exposed to the surface [17].

3. RESULTS AND DISCUSSION: 3.1. Wettability

Texttreasure Even the greatest fool can accomplish a task if it were after his or her heart. But the intelligent ones are those who can convert every work into one that suits their taste - Swami Vivekanand. Figure 3.1: Wicking ability of treated wool samples 386

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PRETREATMENT Table 3.1: Effect on change in Surface energy for treated wool fabrics

Samples

OWENS

Wu (mN/m)

FOWKES (mN/m) Polar liquid: water

WENDT (mN/m)

Water Di-iodomethane Glycerol

Glycerol

Dispersive component

Polar interaction solid -liquid

Dispersive component

Polar interaction solid - liquid

Control

21.24

30.38

24.76

18.43

32.71

18.43

13.93

DCCA

28.28

34.18

32.6

17.93

75.94

14.33

41.74

19.63

28.48

24.76

12.8

39.39

14.9

18.98

41.88

27.43

28.32

12.7

48.1

17.26

79.56

19.39

28.04

25.43

13.67

111.07

13.1

22.58

DCCA+ E

24.26

28.48

29.66

12.8

39.39

12.7

37.92

E+DCCA

74.06

73.41

72.82

13.1

40.3

13.67

84.88

CP+E

18.84

27.43

24.41

14.9

36.75

12.8

22.28

P+ CP

51.98

49.42

70.78

14.33

52.79

17.93

78.62

P+ E

74.63

73.72

72.82

12.7

112.32

12.7

86.44

Control

Control (137.20)

CP (122.10)

DCCA+ E

DCCA

E+DCCA CP+E

P+ CP

P+ E

E (112.90)

CP+E (128.70)

Figure 3.2: Contact angles images of different wool samples

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3.2. Contact angle of samples and drop test Figure 3.2 shows the contact angle images of different wool fabrics. It can be seen that the untreated samples showed a contact angle of 137.20 which was reduced by different treatments. For the descaling treatment performed by all other treatments which is not shown in the figure 3.2, the drop sank immediately in the fabric as soon as it was put on the fabric surface. This can be easily corroborated by the drop test in Figure 3.3. We can note that the drop remains on the fabric surface for Enzyme, CP and CP + Enzyme treatment. Both these results are in agreement with what is obtained by measuring the surface energy of these samples.

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Figure 3.3: Drop test images of wool samples

PRETREATMENT 3.3. Physical and mechanical analysis The effect of the treatment on the physical and mechanical properties of wool fabric was studied and the results are mentioned in Table 3.2.

3.4. SEM observations The surface morphology of wool fabric samples was studied by scanning electron microscopy (Figure 3.4). The untreated wool exhibited prominent scale structure

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Table 3.2: Whiteness index, Tenacity and Tear strength of wool fabrics

Samples

Whiteness Index

Tensile strength (KgF)

Elongation %

Tear Strength (KgF)

Control

26.347

26.05

35.21

1860.22

DCCA

-16.378

12.64

29.51

1470.1

29.422

22.31

34.22

1580.02

52.144

23.82

1679.31

35.803

17.56

39.25

2188.5

DCCA+ E

1.773

18.56

29.67

1412.05

E+DCCA

11.619

21.76

32.54

1461.74

CP+E

32.971

14.96

22.68

1766.06

P+ CP

36.403

20.14

31.42

1590.11

P+ E

46.722

22.93

34.58

1634.48

Table 3.2 shows that, plasma-treated wool fabrics present higher whiteness than other samples. Wherever DCCA was used the whiteness index of the samples got reduced as treatment with DCCA can be attributed to the formation of degradative products formed due to the treatment. One of the reason may also be due to the presence of traces of DCCA which is a chlorine based product. Plasma treatment has resulted in maximum whiteness of the treated sample which on further treatment with enzyme has resulted in loss in whiteness to some extent. This may be due to the surface etching because of plasma treatment and weakening of disulphide linkage resulting in removal while the subsequent enzyme treatment degrades the protein linkage thereby imparting some yellowness. Further, the retention of tensile and tearing strength of various treated samples is concerned, only plasma treated sample demonstrates maximum strength retention property due to surface etching phenomena. Subsequent treatment with enzyme results in marginal strength loss in comparison to plasma sample. This may be due to the very specific action of enzyme. Loss in tensile and tear strength of wool sample treated with DCCA followed by plasma treatment can be attributed to the degradation of wool due to the chemical treatment. After polyurethane based CP treatment wool fibres were coated with film which caused improvement in tear strength and % elongation.

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on fabric surface (Figure 3.4-a). The woollen fabrics, after being treated with plasma and CP showed scale damage with film formation due to CP (Figure 3.4-d). However, enzyme-DCCA treatment produced most remarkable destruction to scales (Figure 3.4-c). PlasmaEnzyme treated fabric had a smooth surface with more surface area and the marks of scales almost disappeared, which gave better descaling effect (Figure 3.4 b).

Figure 3.4: SEM images of wool fabric treated with (a) untreated (b) P+E (c) E+DCCA (d) P+CM. March - April 2018

4. CONCLUSION Comparison of various techniques and their combination on wool descaling were studied. Among all the treatments the combined treatment of plasma followed by enzyme gave the best results. The conclusion obtained was based on the maximum increase in surface energy and polar component. The wettability and drop test also supported these results. The mechanical properties of the fabric were also preserved as compared to other methods. The whiteness index of the treated samples was also higher than the control sample. We propose that wool descaling can be effectively done first by treating the wool fabrics to plasma treatment followed by enzyme treatment. 5. ACKNOWLEDGMENT The researchers would like to acknowledge the facilities made available by the DST, Govt of India through FIST and World Bank funded TEQIP-II in successfully completing this research project and University Grants Commission (UGC) for fellowship in successful completion of this research work.

10.

11.

12.

REFERENCE 1.

Chvalinova R. and Wiener, Sorption properties of wool fibers after plasma treatment, II Central European Symposium on Plasma Chemistry, Chem. Listy.; 102, 1473-1477 (2008). Meade, SJ, Dyer, JM, Caldwell, JP. Covalent modification of the wool fiber surface: Removal of the outer lipid layer. Text Res J; 78, 943-957 (2008). M. Huson, D. Evans, J. Church, S. Hutchinson, J. Maxwell, and G. Corino, New insights into the nature of the wool fibre surface, J. Struct. Biol., 163, 127-136 (2008). Evans, D. J., and Lanczki, M., Cleavage of Integral Surface Lipids of Wool by Aminolysis, Textile Res.J. 67, 435-444 (1997). Veldsman D P and Swanepol O A, The influence of the rate of chlorination on the shrinkproofing of wool with DCCA, Appl Polym Symp, 18, 691700, (1971). Levene R and Cohen Y, An oxidative batchwise shrink-resist treatment for wool using

13. 14.

15.

16.

17.

monoperoxyphthalic acid, J Soc Dyers Color, 112, 44-49 (1996). Cardamone, J. M., Yao, J. and Nuñez, A., DCCA shrink-proofing of wool, Part II: improving whiteness and surface properties , Textile Res. J. 74(7), 565-570 (2004). Cardamone JM and Yao J. DCCA shrink-proofing of wool. Part I: the importance of antichlorination. Textil Res J; 74: 555-560 (2004). L. Ammayappan, Eco-friendly surface modifications of wool fiber for its improved functionality: an overview. Asian Journal of Textile, 3, 15-28, (2013). Hesse, A., Thomas, H., Hocker, H., Zero-AOX shrinkproofing treatment for wool top and fabric, part i: glow discharge treatment, Textile Res. J. 65 (6), 355-361 (1995). Cook J. R. and Fleischfresser B. E., Shrink resisting wool with Synthappret BAP: the effect of drying conditions, Textile Res J, 55, 607-614 (1985). Demir, A., Ar?k, B., Ozdogan, E., Seventekin, N., The comparison of the effect of enzyme, peroxide, plasma and chitosan processes on wool fabrics and evaluation for antimicrobial activity, Fibers and Polymers, 11(7), 989-995 (2010). Johnson NAG, Russell IM, Advances in wool technology. CRC Press, North America (2009). Barani, H. and A. Calvimontes, Effects of oxygen plasma treatment on the physical and chemical properties of wool fiber surface. Plasma Chem. Plasma Process., 34, 1291-1302 (2014). Zaman M, Liu H, Xiao H, Chibante F, Ni Y, Hydrophilic modification of polyester fabric by applying CNC containing surface finish. Carbohydrate Polymers 91(2), 560-567 (2013). Negri, A.P., Cornell, H.J., and Rivett, D.E., The nature of covalently bound fatty acids in wool fibers, Aust. J. Agric. Res. 42, 1285-1292, (1991). Fatarella, E., Ciabatti, I. and Cortez, J., Plasma and Electron-Beam Processes as Pretreatments for Enzymatic Processes, Enzyme and Microbial Technology, 46, 100-106 (2010). ❑❑❑

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DYEING

Dyeing of Polyester Fabrics Using Nano TiO2 and Without Using Carrier M. M. El-Molla1,2*, M. Helmy3 & A. Abd-Elghany4 1 Chemistry Department, Faculty of Science & Arts, Jouf University; 2 Textile Research Division, National Research Centre El- Bohouth St., 3 Chemistry Department, Faculty of science, Helwan University, Helwan, Cairo, 4 Technical manager of dyeing in EL-Kkoba dyeing & finishing Co. Abstract The polyester fabrics were firstly treated with nano TiO2 particles using ultrasonic rays (500W/36Hz), and then dyed with either disperse blue 56 150% and / or disperse red 60 200 % at the boil without a carrier used.The dyeing efficiency was compared to the normal dying (without treatment) of the same fabrics dyed with the same shade concentrations. The dyeing adsorption of polyester fabrics was positively affected by nano TiO2 pretreatment and an increase in nano TiO2 content led to higher color strength.The proposed method proved to have no adverse effects on fastness properties and could be considered as the new method for dyeing of different polyester fabrics as an eco-friendly method. This method is also free from some of the disadvantages involved in carrier dyeing such as toxicity. Keywords Carrier, Dyeing, Nano TiO2, Polyester Fabrics.

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1. Introduction Disperse dyes are the most important class of dyes used in dyeing of polyester fibers. The rate of dyeing may be enhanced to the level ofcommercial acceptability,either by using high temperature at 1300C,or by dyeing at 98-1000C by using carrier or by thermo sol method by impregnating the textile with suitable dispersants,drying and then curing at 190-2200C[1]. Solvent-assisted and carrier dyeing has been widely studied as a means of accelerating dyeing rate, improving dye uptake and lowering dyeing temperature by means of changes in the physical properties of polyester, notably such as Glass transition Temperature (Tg). However, both solvents and carriers have serious problems, namely toxicity and unpleasant odor, poor light fastness, an adverse effect on the physical properties of the fiber, high costs of waste water treatment and environmental contamination and destruction. Clearly, it seems sensible that efforts should be devoted toward the development of a new dyeing method to accelerate dyeing rate, improve dye uptake and lower dyeing temperature [1]. *All the Correspondence should be addressed to, Prof. Dr. M. M. El-Molla National Research Centre, Textile Research Division, Dokki, Cairo, Egypt. Email : melmolla@yahoo.com, mohamedelmolla212@gmail.com 390

Carrier dyeing of polyester has been studied [1-3], as a means of accelerating dyeing rate,improving dye uptake and lowering dyeing temperature. The glass transition temperature (Tg) is reducing by the effect of the carrier.However,the effect of carrier on the dyeing rate depends on the dye structure [3].Nanotechnology is a very complex field combining science (biology, chemistry and physics), technology (computer programming), engineering (electronics and design) and math. Nanotechnology can be applied to many areas in textiles. They are used for producing Nano fibers, Nano composites, Nano dyeing and Nano finish. Nano dyeing is the application of reduced size dyes that are smaller than 100nm in textile dyeing6. Nanotechnology is an emerging field that covers a wide range of technologies which are presently under development in Nano scale. It plays a major role in the development of innovative methods to produce new products, to substitute existing oduction equipment and to reformulate new materials and chemicals with improved performance resulting in less consumption of energy and materials and reduced harm to the environment as well as environmental remediation. Although, reduced consumption of energy and materials benefits the environment, nanotechnology will give possibilities to remediate problems associated with the existing processes in a more sustainable way. March - April 2018

DYEING Environmental applications of nanotechnology address the development of solutions to the existing environmental problems, preventive measures for future problems resulting from the interactions of energy and materials with the environment, and any possible risks that may be posed by nanotechnology itself.According to the environmental recommendations we can develop a new methodwithout need for carriers [5, 6]. Several studies reported the potential of TiO2 a nano photocatalyst for imparting multi-functional properties to different textile fabrics [7-17]. Searching for new methods to improve the disperse dyeing of polyester fabric and its fastness properties has attracted a great deal of attention [21, 22]. Application of many auxiliaries in the dyeing of polyester fabrics with disperse dyes have been extensively investigated [23, 24]. The cationic twin surfactant has been proved to be able to control the kinetics and to improve dye uptake in the disperse dyeing of polyester [25]. Plasma and laser treatment have also shown positive effects on dyeing rate and uptake of polyester fabrics [26-29]. The aim of the present study is an attempt to solve some problems with carrier dyeing of polyester fabrics through nano technology.For this purpose,the effect of nanoTiO2 particles on the dyeing behavior of polyester fabrics (Stan, gabardine, poly70) was investigated. 2. Materials and Methods 2.1. Materials 2.1.1. Fabrics Three 100% polyester woven fabrics which are:Stan,Gabardine and Poly70,their square densities are 188,312 and 114 g/m² respectively.Supplied by a private sector company.

2.1.3. Chemicals Nano titanium dioxide was employed as a photo-catalyst with 80% anatase and 20% rutile crystalline structure and average particle size of 21 nm from Degussa, Germany, dispersing agent, andacetic acid. 2.2. Methods 2.2.1. Nano TiO2 pre-treatment The polyester fabrics are firstly treating with nano TiO2particles prior to dyeing. The aqueous dispersions of nano TiO2 by different concentrations (1&3%) wereprepared in an ultrasonic bath (500W/36Hz).The fabrics were immersed in freshly prepared aqueous solutions for 3 min and then padded to 90%wet pickup,dried at 80°C for 3 min. followed by curing at either at 140°C to 220°C,for 2 min. 2.2.2. Dyeing The nanoTiO2 treated fabrics(Stan,Gabardiene,Poly70) which firstly treated with concentrations(1% and / or 3%) nanoTiO2were dyed with either disperse blue 56, 150% and / or disperse red 60, 200% by shade concentrations (0.5%,1%,2%,3%),at boil without carrier in presence of 10% o.m.f.dispersing agent,0.5 g/l acetic acid (pH=4.5-5.5) and liquor to good ratio (L:R)=1:30.The specimens were introduced into the dye-bath at 500C,then the temperature was gradually raised to boil within 20 min,and dyed for 60 min.The fabrics were rinsed in warm water and subjected to reduction clearing for 15 min at 700C using a 30:1 liquor ratio in aqueous solution containing 10% o.m.f. NaOH and 10% o.m.f. Na2S2O4 to remove excess dye and auxiliaries.The untreated fabrics are dyed with the same conditions.

Dyeing Diagram of polyester fabrics

I- Disperse Red 60 (1-Amino-4-hydroxy-2phenoxyanthraquinone) II- Disperse Blue56 (1, 5-Diamino-2-chloro-4, 8dihydroxy-9, 10-anthracenedione) March - April 2018

2.3 Measurements and Analysis 2.3.1. Scanning Electron Microscope (SEM) Untreated & treated samples with nano TiO2 particles of Stan, gabardine, and poly70 polyester fabrics mounted on aluminum stubs, and sputter coated with gold in a 150 Å sputter (Coated Edwards), and examined by 391

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2.1.2. Dyestuffs Disperse red (C.I. Red 60) and Disperse blue dyes (C.I. Blue56), supplied by Clarinet Co.

DYEING Jeol (JXA-840A) Electron Probe Microanalysis (Japan), magnification range 35 - 10,000, accelerating voltage 19 kV [30,31]. Inorder to confirm the presence of TiO2nano particles. 2.3.2. Color strength The relative color strength of the prints expressed as K/S value [32] of the colored samples was determined by reflection measurements using data color international model SF 500, USA. 2.3.3. Fastness properties Fastness to washing, rubbing and perspiration was assessed according to the standard methods of AATCC technical manual, viz Method 8 (1989) 68, 23 (1993); Method 36 (1972) 68 (1993) 23; and Method 15 (1989) 68, (1993) 30 respectively.

Figure 3.1. SEM images of (a) untreatedsatin polyester, (b) treated satin poly ester with1% nano TiO2 (c) treated satin polyester with 3% nano TiO2.

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3. Results and Discussion 3.1. Scanning electron microscope (SEM) Nano TiO2 concentrationpre-treatment, polyester fabrics, the SEM images of Stan, Gabardineand Poly70 polyester fabric untreated and treated with 1& 3%nano TiO2 are shown in Figures 3.1- 3.3 respectively. From the Figures we noticed that, the surface of the treated fibers is uniformly and covered by nano TiO2 particles. Also, the treated fabric at higher concentration of nano TiO2 particles 3% are covered may be equal to that obtained upon usingof nano TiO2 particles 1% concentration as show on the fiber surface in the figures 2, 3 (b & c) respectively.

Figure 3.2. SEM images of (a) untreatedGabardine poly ester, (b) treated Gabardine poly ester with1% nano TiO2 (c) treated Gabardine poly ester with 3% nano TiO2.

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DYEING Figures 3.4-3.7 show the effects of Nano TiO 2 concentrationpre-treatment Poly70, Stan, and Gabardine polyester fabrics and then dyeing upon using disperse dye blue 56at different concentration 0.5,1,2, and 3% respectively on the color strength values (K/S).

Figure 3.3. SEM images of (a) untreatedpoly70 poly ester, (b) treated poly70 poly ester with1% nano TiO2 (c) treated poly70 poly ester with 3% nano TiO2.

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3.2. Effect of nano TiO2 pre-treatment on dye ability using disperse dye blue 56 As we know polyester fiber has a highly compact and crystalline structure, and is markedly hydrophobic. For this reason, its aqueous dyeing is carried out at high temperature and high pressure using disperses dyes. The dyeing of polyester can be divided into several parallel processes such as dissolution and re dissolution of disperse dye, transfer of dissolved dye from bulk solution to the fiber surface, diffusion and adsorption of dye at the fiber surface, and diffusion from the surface into the interior of the fiber. It is well known that the additives in the dye bath affect the dyeing processes.

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DYEING From the Figures, we noticed that using 1 %Nano TiO2 concentration for pre-treatment of Poly70, Stan, and Gabardine polyester fabricsbefore dyeing give K/S comparable or higher than up on using 3 % Nano TiO2 concentration this is true irrespective of either the concentration of dye used or the type of fabric dyed, therefore it is not recommended to use higher than 1 % Nano TiO2 concentration, and this is may be due to increase Nano TiO2 concentration this is lead to make a layer on the surface of polyester fabrics which retard the dyeing process. Also, from the Figures, we noticed that the increasing the dye concentration this is lead to increase the K/S, for example increase the dye conc., from 0.5, 1, 2 and 3%, up on using 1 % Nano TiO2 concentration pretreatment of Poly70 and / or, Stan, and / or Gabardine polyester fabrics before dyeing the K/S increase from 5.2, 11.8, 12 and19 and/or 4.1,7.5, 7.8 and 15.2 and/or 4.2, 8.7, 9.2 and 17.5 respectively.Generally speaking, poly70 fabrics pretreatment using 1 % Nano TiO2 concentration has thehighest K/S compared with Stan, and Gabardine polyester fabrics which have a comparable result.This is may be due to the different in the waving structure of the using fabrics.

Journal of the TEXTILE Association

3.3. Effect of nano TiO2 pre-treatment on dye ability using disperse Red FB 200% Figures 3.8-3.11 show the effects of Nano TiO2 concentration pre-treatment Poly70, Stan, and Gabardine polyester fabrics and then dyeing upon using disperse dye Red FB 200% at different concentration 0.5,1,2, and 3% respectively on the color strength values (K/ S).

From the Figures, we noticed that using 1 % Nano TiO2 concentration for pre-treatment of Poly70, Stan, and Gabardine polyester fabrics before dyeing give K/ S comparable or higher than up on using 3 % Nano TiO2 concentration this is true irrespective of either the concentration of dye used or the type of fabric dyed, therefore it is not recommended to use higher than 1 % Nano TiO2 concentration, and this is may be due to increase Nano TiO2 concentration this is lead to make a layer on the surface of polyester fabrics which retard the dyeing process. Also, from the Figures, we noticed that the increasing the dye concentration this is lead to increase the K/S, for example increase the dye conc., from 0.5, 1, 2 and 3%, up on using 1 % Nano TiO2 concentration pretreatment of Poly70 and / or, Stan, and / or Gabardine polyester fabrics before dyeing the K/S increase from 6.2, 14.5, 20.5 and 24 and/ or 4.8, 9.8, 16.5 and 18 and/or 5.1, 10.3, 18 and 21 respectively. Generally speaking, poly70 fabrics pretreatment using 1 % Nano TiO2 concentration has the highest K/S compared with Stan, and Gabardine polyester fabrics which have a comparable result. this is may be due to the different in the waving structure of the using fabrics. It was determined that nano-sized titanium dioxide[33], zinc oxide whiskers [34], nano antimony-doped tin oxide (ATO) [35] and silanenanosol [36] could impart antistatic properties to syntheticfibers. TiO2, ZnO and ATO provide anti-static effects because they are electrically conductivematerials. Such material helps to effectively dissipate the static charge which is accumulated on thefabric.

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DYEING 3.4. Fastness Properties Tables 3.1 &3.2 show, the overall fastness properties of pre-treatmentPoly70, Stan, and Gabardine fabrics using 1 % Nano TiO2 concentration then dyed with either disperse blue 56 and / or disperse red 60, at (1000C, 1 h, L:R 1:20, at pH 4.5), with 3% dye o.w.f. From Tables 3.1 &3.2 we noticed that, the overall fastness properties to rubbing, washing, and perspiration for the dyed samples of poly70, Stan and gabardine their values ranging from very good to excellent.

4. Conclusions The dyeing of polyester fabrics was positively affected by a nanoTiO2 pre-treatment.WhilenanoTiO2 treated samples absorb the dye almost equally in comparison to the fabric dyed by carrier,they give good and acceptable benefit from multi-properties obtained by nanoTiO2 application including self-cleaning, hydrophilicity and UV protection and they are free from the disadvantages involved in carrier dyeing.Also,the proposed nano dyeing method showed no significant change in fastness properties of the dyed samples.

Table 3.1. Fastness properties of pre-treatment Poly70, Stan, and Gabardine fabrics using 1 % Nano TiO2 concentration then dyed with disperse blue 56, at (1000C, 1 h, L:R 1:20, at pH 4.5), with3% dye o.w.f.

Fabrics dyed

K/S

Fastness to

Wash fastness

Fastness to Perspiration

rubbing Alkaline

Acidic

Dry

Wet

Alt

Poly70

4-5

Stan

15.2

4-5

Gabardine

17.5

4-5

Alt: color change of dyed sample; SC: staining on cotton; SW: staining on wool, Wash-scale (1-5). Table 3.2. Fastness properties of pre-treatmentPoly70, Stan, and Gabardine fabrics using 1 % Nano TiO? concentration then dyed with disperse red 60, at (100Â°C, 1 h, L:R 1:20, at pH 4.5), with 3% dye o.w.f.

Fabrics dyed

K/S

Fastness to

Wash fastness

Fastness to Perspiration

rubbing Alkaline

Acidic

Dry

Wet

Alt

Poly70

4-5

Stan Gabardine

18 21

4-5 4-5

4 4

4-5 4-5

4 4

4-5 4-5

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Alt: color change of dyed sample; SC: staining on cotton; SW: staining on wool, Wash-scale (1-5).

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References 1. Nunn D. M. England, Dyers company publicationstrust; (1979). 2. Arcoria A., CernianiA., DeGiorgiR., Longo M.L., ToscanoaR. M., Dyes & Pigment, 11,269-76, (1989). 3. ArcoriaA., LongoM. L., ParisiG., Dyes & Pigment, 6, 155-61,(1985). 4. Choudhury A. K., USA: Science publishers; (2006). 5. BurkinshawS.M., Jeong D.S., Dyes & Pigment, 92, 1025-30,( 2012). 6. Saligram A. N., Shukla S. R., Mathur M., Journal of the Society of Dyers and Colorists, 109,2636,(1993). 7. Montazer M, Pakdel E. J Photo chem.Photobiol C;12:293e303 (2011). 8. Montazer M, Pakdel E. J Photochem.Photobiol C; 86:255e60 (2010). 9. Montazer M, Pakdel E. J Text Inst; 102:343e52 (2011). 10. Nazari A, Montazer M, Rashidi A, Yazdanshenas ME, Anari M. ApplCatal A;371:10e6 (2009). 11. Nazari A, Montazer M, Moghadam MB, Carbohydrate Polymer; 83:1119-27(2011). 12. Montazer M, Morshedi S. Int J BiolMacromol; 50: 1018-25 (2012). 13. Montazer M, Seifollahzadeh S. Color Technol; 127:1-6(2011). 14. Montazer M, Seifollahzadeh S.J Photochem Photobiol C;87:877-83 (2011). 15. Montazer M, Pakdel E, Behzadnia A. J ApplPolymSci;121:3407-13(2011). 16. Doakhan S, Montazer M, Rashidi A, Moniri R, MoghadamMB.CarbohydratePolymer . http:// dx.doi.org/10.1016/j.carbpol.01.023(2013). 17. Nazari A, Montazer M, Dehghani-Zahedani M. IndEngChem Res;52:1365-71(2013). 18. Mihailovic D, Saponjic Z, Radoicic M, Radetic T, Jovancic P, NedeljkovicJ. Carbohydrate Polymer;79:526-32(2009).

19. Dastjerdi R, Montazer M, Shahsavan S. Colloid Surf A;345:202-10(2009). 20. Dastjerdi R, Montazer M. Colloid Surf B;79:518(2010). 21. Tsatsaroni EG, Kehayoglou AH. Dyes Pigm;28:123-30(1995). 22. Tsatsaroni EG, Eleftheriadis IC. Dyes Pigm;61:1417(2004). 23. Kehayoglou AH, Tsatsaroni EG, Eleftheriadis IC, Loufakis KC, Kiriazis LE. Dyes Pigm;34:20718(1997). 24. Tsatsaroni EG, Kehayoglou AH, Eleftheriadis IC, Kiriazis LE. DyesPigm;38:65-75(1998). 25. Kehayoglou AH, Tsatsaroni EG. Dyes Pigm;23:5363(1993). 26. Choi TS, Shimizu Y, Shirai H, Hamada K. DyesPigm; 50:55-65(2001). 27. Yeung KW, Chan K, Zhang Q, Wang SY. JHKITA: 11-7(1997). 28. Esteves F, Alonso H. RJTA;11:42-7(2007). 29. Montazer M, Taheri SJ, Harifi T. J ApplPolym Sci;124:342-8(2011). 30. ReedW. F. "Automatic Mixing and Dilution Methods for Online Characterization of Equilibrium and Non-Equilib-rium Properties of Solutions Containing Polymers and/or Colloids," US Patent No. 6653150, 2003. 31. AlbA. M., DrenskiM. F. and ReedW. F. Polymer International, 57, No. 3, 390-396(2008). 32. JuddD. B. and WyszenkiG., "Color in Business, Science and Industry," 3rd Edition, John Wiley and Sons, New York, (1975). 33. Dong, W.G. and Huang, G. Journal of Textile Research, 23: 22-23(2002). 34. Zhou, Z.W., Chu, L.S., Tang, W.M., and Gu, L.X., Journal of Electrostatics, 57, 347-354(2003). 35. Wu, Y., Chi, Y.B., Nie, J.X., Yu, A.P., Chen, X.H., and Gu, H.C., Journal of Functional Polymers, 15, 43-47(2002). 36. Xu, P., Wang, W., and Chen, S.L., Melliand International, 11, 56-59(2005). ❑❑❑

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FINISHING

Modification of Banana Fibres by Grafting for Application in Composites M. D. Teli*, Jignesh S. Mahajan & Pintu Pandit Department of Fibres and Textile Processing Technology, Abstract Graft copolymerization of methyl methacrylate (MMA) onto bananafibre was carried out using hydrogen peroxide, ammonium ferrous sulphate combination as initiator in an aqueous medium. The effects oftemperature, material to liquor ratio, monomer and initiator concentration and duration of polymerization reaction on graft yield have investigated. Evidence of grafting was studied from Fourier transform infrared spectroscopy, X-Ray diffraction and microscopic images of raw,NaOH treated and MMA grafted banana fibre. Separate composites were fabricated using raw, delignified and banana fibres modified using best graft polymerization reactions with epoxy resins.The mechanical properties of these composites were evaluated. It was found that composites based on grafted fibres showed better mechanical properties in terms of Young's modulus and tensile strength compared to that of composites based on NaOH treated banana as well as raw banana fibres and plain epoxy composite. It was also seen that as fibre loading increased better mechanical properties of composites were obtained. It was also found that increase in graft add-on percentage on fibre improved mechanical properties of final composites.

The interest in using natural fibres such as different plant fibres as reinforcement in plastics has been increasing. Various natural fibres such as coir, sisal, jute, coir, and banana are used as reinforcement materials.

Investigations carried out in this field have shown that stiffness, hardness and dimensional stability of plastics have also been improved by incorporation of lignocellulosic fillers [4]. Natural fibres have many advantages compared to man-made fibres like low cost, low density, low abrasion, reduced energy consumption, recyclability, biodegradability etc[5]. But at the same time, naturalfibre composites also have some limitations such as enormous variability, poor moisture resistance, lower durability, poor fire resistance, and lack of fibre -matrix adhesion [2]. Renewable natural fibres could be potential substitutes for energy-intensive synthetic fibres in many applications where high strength and modulus are not required. It is therefore important to improve the strength properties and other fibre properties of the existing fibres for better utility [7,5]. In addition, they are renewable raw materials and have therelatively high strength and stiffness and cause no skin irritation[5, 8]. The environment-friendly character is very important for the acceptance of natural fibres in large volume of engineering markets such as automotive, military, aeronautic and building industries[9].

*All correspondences should be addressed to, Prof. (Dr.) M. D. Teli, Institute of Chemical Technology, N. P. Marg, Matunga, Mumbai-400019. Email : mdt9pub@gmail.com

Banana fibre is hydrophilic in nature and this is the most important limitation of this fibre as far as its use as reinforcing material is concerned. It is, therefore, necessary to improve the characteristic properties of

1. Introduction In today's modern world the need for more efficient material is very significant for the development of new products. For this composites play a major role as it has thestrong load carrying material embedded in theweaker material. Reinforcement provides strength and rigidity to help and support the load [1].Variousproblems are associated with synthetic fibrereinforced composites such as waste disposal, recycling landfill disposaletc and thus such composite are being increasingly excluded from the world due to growing environment sensitivity [2]. Employing natural fibres as reinforcing material in polymer composites is studied by a number of researchers. With growing environmental awareness, ecological concerns, and new legislations, bio-fibre reinforced plastic composites are receiving increasing attention during the recent decades [3].

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Keywords Graft copolymerization, methyl methacrylate, banana fibre, composites, tensile strength.

FINISHING these natural polymers chemically, so that they are improved with respect to durability, sustainability, and mechanical strength, but will, at the same time, be degradable and ecofriendly. With this aim in mind, attempts are made to modify its quality and characteristic properties, both genetically and by improving its end products, with a view to diversifying its applications in various fields. Grafting of themonomer onto cellulose fibres is one of the most effective methods to improve mechanical properties and reduce the water uptake tendency [5, 10]. A lot of work has been done on graft copolymerization of monomers onto cellulose and other tensile fibres and yarns. However, very much less work has been reported on grafting of vinyl monomers onto banana fibres. In the present work, graft polymerization of methyl methacrylate on to banana fibres was carried out using ferrous ammonium sulphate and hydrogen peroxide as initiator system. The grafted material is then treated for its contribution in improving composite properties and results of this study are reported and discussed here in this paper.

Journal of the TEXTILE Association

2. Materials and Methods 2.1 Materials Banana fibre used for the research was obtained from Central Institute of Research on Cotton Technology, Mumbai. Ferrous ammoniumsulphate from Thomas Baker, Mumbai was used. Other chemicals like methyl methacrylate (MMA), hydrogen peroxide, N,N'Methylenebisacrylamide (MBA), sodium hydroxide, acetone, methanol, dimethylformamide, hydrochloric acid were used of laboratory grade and were purchased from S.D. Fine chemicals ltd. Mumbai. Epoxy Resin Lapox andepoxy Hardener Lapox from Atul Industry were used. 2.2 Chemical treatment of banana fibres Banana fibres were treated with 2% NaOH solution for 1 hour at 750C temperature. After the treatment, fibres were thoroughly washed with water and further neutralization was done by acetic acid to remove the alkali. The fibres were then dried in anoven at 1050C temperature. 2.3 Grafting procedure Alkali-treated banana fibres were immersed in therequired amount of water along with arequired solution of Ferrous ammonium sulphate (FAS) (8.0x10-3 M) and H2O2 (0.12 M) in a three-necked flask at the 600C temperature. Nitrogen gas was allowed to bubble through the solution and required amount of MMA and MBA were added to the conical flask. The reaction 398

was carried out in the N2 atmosphere with continuous stirring at required temperature and time. After thereaction was allowed to proceed for the desired interval of time, the fibres were taken out, washed with cold and hot water and then dried. The grafted material was then subjected to Soxhlet extraction with acetone for 12 hours and then dried at 1050C.Graftadd on % was calculated as per increase over the original weight of the sample.The graft add on (%) was calculated as:

2.4. Chemical resistance test The Chemical resistance of raw, NaOH treated and grafted banana fibre was studied as a function of percent weight loss of fibre when treated with different chemicals. A known amount 0.1 gmbanana raw, NaOH treated and graftedfibre was treated with thedefinite volume of hydrochloric acid and sodium hydroxide of different strength for atime interval of 24hrs. The fibres were then washed 2 to 3 times with distilled water and finally dried in an oven at 1100C to a constant weight to get final weight. The percent weight loss was determined as per Sangha and Rana's method.

WhereWg is the percent chemical resistance and Wo, Wtare the weights of the samples before and after treatment. 2.5 Swelling behavior test The swelling behavior of the raw, NaOH treated and grafted banana fibre was studied indifferent solvents such as water, methanol anddimethylformamide (DMF). A dry sample of grafted as well as raw fibres (0.1 g) was suspended in 100ml of the solvent kept at room temperature for 24hrs. The solvent that adhered on the surface of the samples was removed by softly pressing between the folds of the filter paper. The samples were then weighted to get the final weight. The percent swelling was calculated as per Sangha and Rana's method.

WhereWg is the percent swelling and Wo, Wtis the weight of the samples before and after treatment. March - April 2018

FINISHING 2.6 Fourier Transform Infrared (FTIR) Spectra FTIR analysis was used to confirm the grafting of MMA on to banana fibre. FTIR spectra of untreated and the treated cotton were recorded using a Shimadzu FTIR-8400S spectrometer at a resolution of 1cm-1 in the wavelengths region of 800-4000 cm-1.

was then placed on compression moulding machine at 120oC for 1hour at 150 psi pressure. The setup was left to cure for 12 hours at room temperature. The prepared composite was cut for testing to conform to the dimensions of the specimen as per ASTM standards.

2.7 X-Ray Diffraction XRD measurement was performed to check the crystallinity.Wide angle X-ray diffraction (WAXD) spectra were obtained using Lab X XRD-6100 of Shimadzu Ltd. with radiation from 100 to 400. The crystallite sizes of the fibres were determined by modified Scherer's formula whereas the degree of crystallinity is computed by comparing the areas under crystalline peak and amorphous curve i.e., the area under the crystalline peak is compared with thesum of the areas of amorphous peaks.

2.10 Tensile strength analysis After the fibres reinforced composite was dried, it was cut using a saw cutter to get the dimension of thespecimen for mechanical testing. The tensile test specimen was prepared according to ASTM D3039. The testing was done using Instron Universal Test Machine (UTM) to measure the force required to break a polymer composite specimen and the extent to which the specimen stretches or elongates to that breaking point. The specimen was mounted in the grips of the UTM with 6 mm gauge length. The stress-strain curve was plotted during the test for the determination of ultimate tensile strength and elastic modulus. All the test results were taken from the average of three tests.

2.8 Morphology of grafted banana Morphological images were taken to see the surface changes of raw, NaOH treated, and grafted banana fibres. The superficial morphologies of fibre samples were observed by LEICA DMEP microscope. 2.9 Preparation of the Composite The composite was fabricated by compression moulding technique. The mould used for fabricating the composite was made up of aluminum. The inner cavity dimension of the mould was 180mm x 180mm x 2mm. The plastic sheet was laied first and wax was applied to it. Some amount of resin was sprayed uniformly over plastic sheet and then fibre mat was laid on it. After that reaming resin was poured on fibres. Then one more wax coated plastic sheet covered from thetop. The upper side was pressed using a roller at room temperature until the matrix was set properly. Mould

3. Results and Discussion 3.1 Optimization of conditions for grafting of MMA onto banana fibres In the present investigation, the physicomechanical properties of banana fibres were improved through graft copolymerization using MMA monomer. The effect of process parameters such as monomer concentration, time, temperature and material to liquor ratio on the extent of grafting, chemical resistance, swelling behavioretc was studied (refer Table 3.1). The changes in surface morphology, composition and crystallinity were investigated by using microscopic images, XRD and FTIR.

Canias ERP Canias ERP Gentex GOTS India GTTES Intex ITAMACH AFRICA ITMA 2019 Lakshmi Machine Works Meera Industries Limited March - April 2018

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Precision Rubber Ind. Pvt. Ltd. Rieter India Ltd. Rieter India Ltd. (Components) Reliance Industries Ltd. TEMTECH-2018 Thymas Electronics Pvt. Ltd. Trutzschler India Unitech Techmech Yarnfab Expo Precision Rubber Ind. Pvt. Ltd.

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FINISHING Table3.1 Optimization of conditions for grafting of MMA on banana fibres Sr. No. Fibre (gm)

F:M Ratio

Temperature (0C)

M:L

Time (Min)

FAS (ml) H2O2 (ml) MBA (gm)

GY (%)

1:4