Journal of Natural Fibers, 00:1–11, 2015Copyright © Taylor & Francis Group, LLCISSN: 1544-0478 print/1544-046X onlineDOI: 10.1080/15440478.2014.964445

Eco-Friendly Dyeing of Gamma Ray Induced Cotton UsingNatural Quercetin Extracted from Acacia Bark (A. nilotica)

T. Gulzar,1 S. Adeel,2 I. Hanif,1 F. Rehman,1 R. Hanif,1 M. Zuber,1 and N. Akhtar3

1Department of Applied Chemistry and Biochemistry, Govt. CollegeUniversity Faisalabad, Pakistan 5

2Department of Chemistry, Govt. College University Faisalabad, Pakistan3Nuclear Institute of Agriculture and Biology, NIAB, Jhang Road, Pakistan

For the present study Quercetin has been extracted and applied onto the gamma irradiated cotton. Fabricsand powder have been exposed to different absorbed doses and dyeing has been performed at variousparameters. It is observed that 20 kGy is the optimum absorbed dose for surface modification of cotton. 10It has been also found that good colour strength has been obtained at 60◦C by dyeing optimal fabric for40 min using dye bath of pH6 keeping liquor concentration of 1:30 and electrolyte concentration of 1 g.7% of tannic acid as pre-mordant and 5% of Copper sulphate as post mordant was optimum conditionsto get good fastness properties according to ISO standard methods. Quercetin from acacia bark underionizing radiation can safely be used as possible substitute to reddish-brown synthetic dyes. 15

Keywords: absorbed dose, dyeing, acacia bark, mordanting, querecetin, spectraflash

INTRODUCTION

Textile researchers since last decade are trying to improve color strength and fastness properties ofdifferent natural and synthetic fabrics dyed with natural dyes through various techniques (Saakshyet al. 2013; Tutak and Korkmaz 2012). These techniques include plasma treatment (Haji et al. 202013), bio polishing, cationization (Ghorannevirs et al. 2010), ultasonic, microwave and UV radia-tion (Iqbal et al. 2008; Bhatti et al. 2014). But of such techniques gamma ray treatment has a markedeffect in textile processing by surface modification of fabrics.

It has been already reported in the literature that gamma ray treatment is useful in crosslinking andgrafting of fabrics (Wojnarovits et al. 2010), dye degradation to treat waste water, alkali treatment of 25cotton (Takacs et al. 2001) and extraction of colourant without any adverse effect (Kim et al. 2006).Only few studies have been reported in the improvement of dyeing behavior of cotton using gammaray treatment. The frequent use of gamma ray treatment is becoming popular in textiles due to itshigh treatment speed, easy to use and cost effectiveness (Ferrero and Periolatto et al. 2012; Bokariet al. 2013). 30

Dyeing from natural sources is the oldest way of colouring textiles. The naturally dyed fabricsrecently have attracted both consumers and manufacturers in fashion markets (Chattopadhyay et al.

Address correspondence to S. Adeel, Department of Chemistry, Govt. College University Faisalabad 38000, Pakistan.E-mail: shahidadeelchemist@gmail.com

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2 T. GULZAR ET AL.

2009; Haji 2012; Tayade et al. 2013). The use of dyes and pigments of vegetable and mineral originswas found frequently until 19th century due to availability of natural resources such as fungi, plants,insects and molluscs (Manhita et al. 2011; Narayanaswamy et al. 2013; Yusuf et al. 2013). Ever 35since, man has discovered ways of exploiting the colouring matters of nature to his own advan-tage, with applications ranging from the painting of culturally relevant events on walls of buildings(environmental embellishment) to their use as cosmetics in facial treatments and lipsticks (per-sonal adornment) (Kamel et al. 2011; Kasiri and Safapour 2013). Other more important areas ofuse include the dyeing of various household articles ranging from clothing to leather articles and 40carpet (Avinc et al. 2013; Tutak and Benli 2012). But with the Perkin’s discovery of mauvine, theindustry started using synthetic dyes. It has been found with the time that synthetic colours not onlyoften are harmful to health but also result in the cause of pollution for eco system (Acquaviva et al.2010; Zheng et al. 2011). These drawbacks about using synthetic dyes due to involvement of highlytoxic and carcinogenic effluents in waste water during processing has expelled them for dye-housed 45(Haji 2010). Many plant which extracted dyes have antioxidant, antimicrobial properties are used invarious walks of life, well known for their health curing characterization. Studies on their character-ization are also going on the way (Farizadeh et al. 2009; Adeel et al. 2014; Adeel et al. 2013).

Keeping in view the advantages of gamma ray treatment in textile dyeing, we have selectedAcacia bark (nilotica) as a source of natural dye (quercetin) and its application onto gamma ray 50treated cotton. Acacia bark is rich in phenolic constituents such as tannins, quercetin and catechin,acacetin and is frequently used for dyeing of different fabrics such as cotton, polyester, wool and silk(Dube et. al. 2001; Saleh et al. 2013). The main colourant present in bark of A. nilotica is quercetinand its structural formula has been given below.

OOH

OH

OH

O

OH

OH

Quercertin

The bark has an inspiring range of medicinal uses with potential antioxidant and anticancer, 55antipyretic, antiasthamatic, antidiabetic, antiplatelet agregatory and antifungal activities along withinhibition potential against human immunodeficiency (Ali et al. 2011).

The main objective of the study is to improve the dyeing behavior of cotton by enhancing its dyeuptake ability through gamma ray treatment and color strenght of dye onto surface modified fabricby pre and post mordanting using quercetin dye extracted from Acacia bark. 60

MATERIALS AND METHODS

Pretreatment Process

Acacia bark was collected from Local area of Faisalabad, Pakistan, washed with distilled waterand dried under shade. The dried bark was ground and passed through a sieve of 20 meshes to get

DYEING OF GAMMA RAY INDUCED COTTON USING NATURAL QUERCETIN 3

powder of equal size. Raw grey cotton fabric was procured from Raheem Textile Centre Faisalabad 65and subjected to desize, scour, bleach, and mercerized by reported methods (Bhatti et al. 2013). Allthe chemicals used in fabric preparation, extraction, dyeing and mordanting were of commercialscale.

Irradiation and Extraction Process

Pretreated cotton and dye powder were exposed to absorbed doses of 10, 15, 20, 25, and 30 kGy 70using Cs-137 gamma irradiator at Nuclear Institute for Agriculture and Biology (NIAB), Faisalabad,Pakistan (Khan et al. 2014). Aqueous and alkaline extract were obtained by boiling irradiated (RP)and un-irradiated accacia powder (NRP). For this purpose, 5 g of both irradiated and un-irradiatedpowder was mixed with 150 mL of water and 0.1 N NaOH solution allowed to boil in a beakerkept over hotplate for rapid extraction for 1 hr. After boiling the crude mixture was filtered through 75cotton cloth and residue was discarded. The aqueous and alkaline extracts obtained were used to dyeirradiated (RC) and un-irradiated fabrics (NRC) (Batool et al. 2013; Rehman et al. 2013).

Optimization of Dyeing and Mordanting Conditions

Different dyeing parameters such as time, temperature, pH, material to liquid ratio and salt con-centration were optimized. In order to observe the effect of radiation on color strength, dyeing was 80carried out for 25, 30, 40, 55, 70 and 85 min using material to liquid ratios of 1:10, 1:20, 1:30, 1:40,1:50 and 1:60. Dyeing was performed using dye solutions of 1 g/L, 3 g/L, 5 g/L, 7 g/L and 9 g/Lof salt concentration (Na2SO4 and K2SO4) at pH 4, 5, 6, 7, 8, and 9 (Rekaby et al. 2009; Zhang andCai 2011). To improve colour characteristics, fabric dyed at optimal conditions were post mordantedusing variable concentration of metal salts and tannic acid (Bechtold et al. 2007). 85

Evaluation of Color Strength and Fastness Properties

Spectraflash spectrophotometer SF 650 with an illuminant of D 65 10◦ observer was used to inves-tigate colour strength (%) of all dyed fabrics (irradiated and un-irraidated). Light, wash and rubfastness were investigated using ISO standard methods. Wash fastness was employed according toISO 105 CO3 in Rota wash machine. Both dry and wet colourfastness was tested using ISO 105 × 12 90protocal using crockmeter. Light fastness was carried out according to ISO 105 BO2 in fado meterusing xenon arc lamp.

RESULTS AND DISCUSSION

Gamma ray treatment is very useful in extraction of colorant as well as surface modification ofcotton. Two media has been applied onto fabrics for extraction of colorant. At natural pH (aqueous) 95the colorant has extracted along with tannins which might sorbed onto fabric. Upon investigationin spectra flash the low tinctorial strength was observed. In alkaline media, tannins are hydrolyzedinto ellagic and gallic acid which interact with alkali to form salt. Due to the reason only quercetingets significant chance to sorb which showed good tinctorial strength (%). This is also attributedwith extraction of quercetin due to presence of acidic hydroxyl group in it (Saleh et al. 2013). After 100interaction of acidic groups with alkali on to fabrics show darker shades with more colour strength.Data displayed in Figure 1(a) and (b) reveal the fact. The other factor which has got more importanceis the red curing of silk fabric.

At low absorbed dose, the cellulosic fabric is not activated while at higher absorbed dose, break-age of glycosidic bond might occur. This degradation results in weight loss as well as sorption of 105

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FIGURE 1 (a) Effect of absorbed dose on the extraction and dyeing of cotton using aqueous extract of acacia barkpowder. (b) Effect of absorbed dose on the extraction and dyeing of cotton using alkaline extract of acacia barkpowder.

less colorant. At 20 kGy, the cellulosic fabric may face even oxidation at surface which improves thedye uptake ability and interaction with dye molecules. It was also observed that abundant hydroxylgroup one C-6 and two C-2, C-3 of cellulosic group allow extensive H-bonding to enhance cellu-losic dye ability. These groups are also responsible for chemical reactivity in dyeing and finishing(Brodbent 2001; Hseih 2007). Upon investigation in spectra flash, high colour strength is observed. 110Here 20 kGy, using alkaline medium gives not only good colourant extraction but also high tinctorialstrength (Figure 1b).

DYEING OF GAMMA RAY INDUCED COTTON USING NATURAL QUERCETIN 5

In optimization of dyeing temperature, dyeing is started at low temperature and is graduallyincreased. At low temperature, less colorant is sorbed and mainly remain at surface of gamma irra-diated fabric while at higher temperature dye molecules rush onto surface and passed to interior of 115fabrics through open voids in cellulosic fabric. At fixed temperature (60◦C), simultaneously dye iseither sorbed or stripped (Chairat et al. 2005). After sometimes equilibrium is established, whileabove that temperature, quercetin may face hydrolytic degradation and other constituents get chanceto sorb onto fabric. Upon investigation in spectra flash less color strength is observed. The data inFigure 2 reveals that 60◦C is the optimal dyeing temperature. 120

Gamma ray treated fabric when dyed for long time, the dye enter into modified fiber-structureand distributes into interior of fiber. While for short time dyeing, the colorant molecules cannot getenough time to enter into spaces between fabric molecules and mainly remain on the surface andafter dyeing upon dyeing, the molecules are washed off. Hence dyeing for 40 min is the optimaltime (Figure 3), not only leveled dyeing is achieved but also good color strength is observed. Hence 125it is found that instead of 60 min, gamma ray treatment has given good color strength at 40 min.Thus it is concluded that gamma ray treatment is time saving technique.

pH of dyeing bath also played role in dyeing. At acidic pH, quercetin is active and impart reddishbrown colour while at basic pH, it gets neutralized. Also under alkaline conditions, fabric may swelland physical characters may disturb. Similarly reduction or hydrolytic degradation under alkaline 130conditions may also occure. Colourant along with other tannins and resin get sorbed onto fabric andcauses unleveled dyeing. The data given in Figure 4. Show that pH 6, is favorable stable conditionof colourant on to fabric.

Extract concentration is also one of the important dyeing parameters. The data displayed inFigure 5, shows that gamma ray treatment has reduced the amount of extract used. At 1:30, good 135colour strength is obtained, while using high liquor concentration the insoluble impurities get morechance to sorb onto fabric instead of colourant itself. Using low liquor concentration, eventually

FIGURE 2 Effect of dyeing temperature on the colour strength of irradiated cotton (20 kGy) using alkaline extractof irradiated acacia bark powder.

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FIGURE 3 Effect of dyeing time on the colour strength of irradiated cotton (20 kGy) using alkaline extract ofirradiated acacia bark powder.

FIGURE 4 Effect of dyeing pH on the colour strength of irradiated cotton (20 kGy) using alkaline extract ofirradiated acacia bark powder.

gives less colour strength so it is found that 1:30 is the optimal material to liquor ratio. Thusgamma ray ray treatmetn has also reduced the amount of liquor (extract) used which shows thatit is cost-effective technique. 140

Salt plays an important role in dyeing because it tends to neutralize the charge created intofiber which repel dye anion. It also modifies the structure of water around hydrophobic group of

DYEING OF GAMMA RAY INDUCED COTTON USING NATURAL QUERCETIN 7

FIGURE 5 Effect of salt concentration on the colour strength of irradiated cotton (20 kGy) using alkaline extract ofirradiated acacia bark powder.

dye and around fabric surface creating a new arrangement in dye solution due to solvation. Thesolvation enables colourant to approach more closely to gamma irradiated surface within range ofshort attractive surface. Hence darker shade is obtained. Greater the amount causes more dye sorp- 145tion that results in unevenness. Gamma ray treatment has reducing the amount of salt used. Using1 g/100 mL of table salt, not only good colour strength is obtained but also dark shades are observed.(Figure 6). More the salt added the greater will be the exhaustion, which results in accumulation ofdye molecules as clusters instead of single molecule sorption. This situation may lead to unevenness

FIGURE 6 Effect of extract concentration on the colour strength of irradiated cotton (20 kGy) using alkaline extractof irradiated acacia bark powder.

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and even desorption (Shore 2002). Hence using 1 g/100 mL is the optimal conditions. Again it is 150found that gamma ray treatment has reduced the amount of electrolyte used for achieving maximumexhaustion, which is the proof that it is cost effective.

It is well known that natural dyes require metal salts for fixation of dye on to modified fabric byforming insoluble precipitates on the surface. This is due to metal ion present in electrolyte whichgives a wide range of shades depending upon their nature. Data given in Figure 7(a) shows that 1555% of copper is the best mordant as compared to iron, aluminium and tannic acid (Osman 2014).The metal ion present in these mordants act as electron donors to form coordination bonds withthe dye molecules making them insoluble in water. So the more interaction with dye causes more

FIGURE 7 (a) Effect of pre-mordants on the colour strength of irradiated cotton (20 kGy) using alkaline extract ofirradiated acacia bark powder. (b) Effect of post mordants on the colour strength of irradiated cotton (20 kGy) usingalkaline extract of irradiated acacia bark powder.

DYEING OF GAMMA RAY INDUCED COTTON USING NATURAL QUERCETIN 9

TABLE 1Effect of gamma ray treatment on colorfastness properties of the irradiated cotton dyed at optimal conditions

Dye Used Optimum Dyeing ConditionWashingfastness Light fastness

Dry rubbingfastness

Wet rubbingfastness

Acacia Bark powder(Alkaline Extract)

Control 2–3 3 3 3

Absorbed Dose (RP/RC,20 kGy)

4 3–4 4 4

Dyeing temperature (60◦C) 3–4 3–4 4 4Dyeing Time (40 min.) 4 4 3–4 4Dyeing p H (6) 4–5 4 3–4 3–4Salt Concentration (1 g/L) 4–5 4 4 4Extract Concentration

(M:L; 1:30)4–5 4 4 4

Pre-mordant 7% TannicAcid

4 4 4–5 4–5

Post-mordant 5% CopperSulphate

4 4 4–5 4–5

aggregation of dye on to fabric. This is due to good chelating ability of Cu than Fe and Al present inalum. Iron due to low reduction power form more darker complex onto fabric result in unevenness, 160while Al dye complex onto fabric may be distributed due to presence of Al in Alum. Similarly datagiven in Figure 7(b) shows that 5% of tannic acid is the best mordant after dyeing. Tannic acid dueto covalent bond formation with dye onto fabric firmly attached and gives darker shades which resisttodetach after washing, rubbing and exposure to heat or light. It is found that gamma ray treatmentalso reduced the amount of mordant used. 165

The rating results given in Table 1 pertaining to light, washing and rubbing show that colourfast-ness properties are improved after pre and post mordanting at optimal condition. The improvementin colourfastness properties of different textiles is due to photochemical interaction of dye-metalcomplex or pronounced tendency of the dye molecules to aggregate inside the fiber. This improve-ment depends upon metal dye interaction with fabric (Tera et al. 2012). This is also due to presence 170of benzene ring, conjugation, OH and Oxo group which causes firm bonding with metal, OH groupof tannic acid onto fabric. After mordanting the darker shades obtained, when exposed to deter-gents in rota wash, rubbing using crock meter and heat/light in fado meter do not detach easily.When compared with ISO standards, greatly improved its rating. Thus the colour after mordantingbecomes deeper and shows less resistance, which might be attributed to the metal complex forma- 175tion between metal, dye and their binding with fibers (Kechi et al. 2013). It can also be observed thatwithout mordanting on light exposure, colourant may take photolytic degradation and results in lowrating (Pathade et al. 2011; Umer et al. 2013). It is observed that gamma ray treatment has enhancedcolourfastness properties but also proved to be cost effective and time effective technique in textileprocessing. 180

CONCLUSIONS

The results of current work indicate that gamma ray treatment is very effective technique for surfacemodification of fabric. This technique has not only reduced the amount of dose when mercerized

10 T. GULZAR ET AL.

fabric is used but also reduced the time, amount of salt and mordant used. It is found that at 20 kGyusing alkaline extract of acacia give good colour strength. Dyeing for 40 min at 60 0C using 1 g/L 185salt has proved that gamma ray treatment is time and cost effective technique. Tannic acid for preand copper sulphate for post mordant has been proved as the best for improving colour strengthand fastness properties. Thus gamma ray treatment can be applied successfully for dyeing of otherfabrics using other dye yielding plants with out harming their physical characteristics.

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