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Article Download wjpls, 2019, Vol. 5, Issue 2, 73-79 Research Article ISSN 2454-2229 Ali et al. World Journal of Pharmaceutical World Journal and Life of Pharmaceutical Sciences and Life Sciences WJPLS www.wjpls.org SJIF Impact Factor: 5.008 MODIFICATION OF WOOL AND SILK FIBERS BY PRETREATMENT WITH QUATERNARY AMMONIUM SALT AND DYEING WITH NEW METAL COMPLEX DYE N.F.Ali*, E.M.EL-Khatib and Saadia A. Abd El-Megied Textile Research Division, National Research Centre, Dokki, Cairo, Egypt. *Corresponding Author: Dr. N. F. Ali Textile Research Division, National Research Centre, Dokki, Cairo, Egypt. Mail ID: [email protected] Article Received on 11/12/2018 Article Revised on 02/01/2019 Article Accepted on 23/01/2019 ABSTRACT Our present study focuses mainly on the synthesis and dyeing of azo metal complex on silk and wool fibers. The present paper describes the synthesis of a new metal complex acid dye obtained from the reaction of acid red 151 2+ 1 with a metallic ion (Co ), and its structure was confirmed by HNMR and IR spectroscopy. The pretreatment of silk and wool fibers by quaternary ammonium salt was carried out by conventional and microwave methods. The absorbance of the original and residual dye in the dye bath calculated from dye exhaustion. The color data of untreated and pretreated silk and wool fibers at different conditions was calculated. The fastness properties of washing, rubbing, perspiration and light to dyed fibers have been measured. KEYWORDS: Synthesis dye, metal complex, wool fiber, silk fiber. INTRODUCTION research (Gaber et al., 2007; Patel et al., 2010; Kaim, 2002), the most common being those containing a hetero Azo dyes and their derivatives have attracted growing nitrogen atom in a position adjacent to the azo group interest over the years because of their versatile (Patel et al.,2011; Karcı, 2013). Utilization and synthesis applications in various fields. There are different of azo dyes is availability of raw materials and simple categories of azo dye such as reactive, direct, vat and synthetic procedures (Otutu, 2011; Kirkan et al., 2008). metal complex dyes. Among the most famous types of Metal complex dyes has high molar extinction these dyes are the metal complex dyes which are coefficient, medium to high fastness, high solubility, considered the predominant dye class for the dyeing of high substantively and diversity in structures (Abdallah, wool, nylon and silk due to but they have to meet very 2012; Chhowala et al., 2015). high requirements as regards their application (Bluss, 1995) and superior fastness properties to washing and In the present work, a new azo-dye with metallic ion light compared with that of non-metallized acid dyes (Co2+) complex using the Acid red 151 as ligand was (Yorkshire, 2004; Zarkogianni et al., 2014). synthesized and characterized. At the same time, spectrophotometric analysis was performed for the Metal complex dyes have played important role in the qualitative investigation of the aggregation behavior of textile industry. Chromium Cr (III) and cobalt Co (III) the metal complex dye, at different concentrations in complexes are used most frequently for the dyeing of aqueous solutions. wool and synthetic fabric (Hrdina, 2004). These metal complex derivatives which show considerable biological 2. EXPERIMENTAL activity may represent an interesting approach for designing new antibacterial drugs. 2.1 Materials - Mill-scoured and bleached wool and silk fibers. The utility of the metal complex dyes is due to their - Ethanol was obtained from Fluka Chemite AG. All versatile applications in the field of dyeing in the textile, other chemicals used in study were of laboratory printing systems, optical storage technology, cosmetics, reagent grade and applied without further drugs, foods coloring (Kondil, 1998; Daniel, 1962; purification. Woisetscla¨ger, 1999) and in analytical chemistry. - Quaternary ammonium salt supplied from Fluka Metallizable azo dyes containing one heterocyclic donor Chemite AG. atom suitably located for the formation of the annulated chelate complex have received much attention in www.wjpls.org 73 Ali et al. World Journal of Pharmaceutical and Life Sciences 2.2. Equipments the boil at (20, 40 and 60 min.). At the end of dyeing - FT/IR spectra were recorded using JASCO FT/IR- process, the samples were thoroughly rinsed and air 4700 spectrometers with high resolution 0.4 cm-1 dried. using ATR accessory. - The 1HNMR spectra were recorded at room 2.4.4. Dyeing at the optimum condition temperature on a Bruker Advance II 400 The treated fibers by the conventional method and spectrometer at 400.13 MHz, the samples were microwave method were dyed at the optimum condition; dissolved in hexadeuterio dimethyl sulfoxide. The pH 5 for wool and silk using 2% o.w.f. 1g/l ammonium 1H chemical shifts was referenced to the central sulphate and L: R 1:50. Each dyeing was performed at signal of the solvent (δ= 2.55). 40°C, allowing the temperature of the dye bath to raise to - UV/Visible spectra were measured on a Shimadzu the boil over 30 min. Dyeing was then continued at the UV-2401 PC UV/Vis spectrophotometer using desired temperature 100˚C further 60 min. distilled water. - The visual color strength (K/S) of dyed fibers was 2.5 Dyeing measurements measured on Data color International SF 600 plus. Measurements and testing dye exhaustion uptake of dye by the wool and silk fibers was measured by sampling 2.3. Synthesis of dye the dye bath before and after dyeing. The dye The cobalt complex was prepared by mixing dye 151 and concentration (g⁄l) of the dye bath was measured on a Co(Cl)2 6. H2O in ethanol solution by molar ratio 2:1 was Shimadzu UV-2401PC UV-visible spectrophotometer at refluxed for 4h and kept overnight at room temperature the λmax value using a calibration curve previously and after cooling, the precipitate was separated by obtained using known dye concentrations (g⁄l).The filtration, washed with distilled water and dried in an percentage of dye bath exhaustion (%E) was calculated oven at 50ºC, dried under vacuum. Yield: 89.5 mg using Eqn 1: (88.8%). % E= [1-C2/C1] x100 Where C1 and C2 are the dye concentrations in the dye The wool and silk fibers treated with the quaternary bath before and after dyeing, respectively. ammonium salt by the following methods: - The conventional method was carried out for wool The relative color strength (K/S) and CIELAB and silk fibers at (30, 45, 60 and 75 min). coordinates (L*a*b*c* h and ΔE*) of the dyed fibers - Microwave method was carried out at (2-7 minutes) were also measured using a Hunter lab's Ultra Scan PRO for wool fibers and at (2-5 minutes) for silk fibers. Spectrophotometer (USA) under illuminant D65, 10°standard observer(Judd et al., 1975). 2.4. Dyeing procedure Dyeing of untreated and pretreated wool and silk fibers 2.5.1. Fastness testing was carried out by exhaustion method. The factors Dyed silk and wool samples with 2% shade (o.w.f) after affecting the dyeing process such as pH, dye washing-off using 2 g⁄l nonionic detergent at 80oC for 15 concentration and time of dyeing were studied. min were tested by standard ISO methods (Methods of Tests for Color Fastness of Textiles and Leather, 1990). 2.4.1. Effect of pH Wash fastness [ISO 105-C02 (1989)], and fastness to The dyeing was applied at pH(3-7) for wool and silk perspiration [ISO 105-E04 (1989)] were evaluated using fibers using 2% o.w.f. dye concentration, using 1g/l the visual ISO grey scale for both color change. Light ammonium sulphate and L:R 1:50. Dyeing was fastness (Xenon arc) was evaluated using ISO 105-B02. performed at 40°C, allowing the temperature of the dye bath to raise to the boil over 30 min. The dyeing was 3. RESULT AND DISCUSSION continued at the boil for a further 60 min. At the end of Acid red 151 dye with the structure I shown in Figure 1 the dyeing process, the samples were thoroughly rinsed under went complexation reaction with Co2+ ion ,using and air-dried. metal- ligand (1:2 molar ratio), in which only the atoms of the – OH functional group are involved in the 2.4.2. Effect of dye concentration coordination reaction. The dyeing was applied at various conc. of dye (1-5), at pH 5 for wool and silk fibers using 1g/l ammonium sulphate and L: R 1:50. Dyeing was performed as the OH N SO Na previous conditions. 3 N N 2.4.3. Effect of time N The dyeing was carried out at different time interval (20,40 and 60 min.) at pH 5 for wool and silk fibers using 2% o.w.f. dye concentration ,1g/L ammonium sulphate and L:R 1:50. Each dyeing was performed at 40°C, allowing the temperature of the dye bath to rise to Figure 1: Acid red 151. www.wjpls.org 74 Ali et al. World Journal of Pharmaceutical and Life Sciences N N N NaO3S N O CO O N SO3Na N N N Figure 2: The proposed formula of the new Metal-complex dye. The above structure was confirmed by structural data The Exhausion of dye on untreated silk 1 and the treated silk at different pH . acquired using FT-IR, and HNMR analyses. The FT-IR 120 has proven to be, in this particular case, a suitable technique to give relevant information to elucidate the way of bonding of the ligand. The study of the infrared 80 spectra reveals the migration of vibration frequencies for the functional groups which were directly involved in the metal ligand.
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