ࡱ> gifqq` bjbjqPqP .::];%$    GGG8GH 2IpI"JJ2JNLNLNL$?hr"tP(L,L"tPtP"  J2JLJdXdXdXtP JZ8JdXtPdXdX} vJ~I `ǡhGXU $~"݇0 F~BdVDpNLBMdXM|NNLNLNL""XdNLNLNL tPtPtPtPd "0"0        ADVANTAGES AND DISADVANTAGES OF SOME CHEMICAL AND PHYSICO-CHEMICAL DisCOLORING METHODS urica PARAC-OSTERMAN; Vedran URA`EVI & Ana SUTLOVI Abstract: Today s chemical and physical-chemical wastewater discoloration methods do not completely meet demands regarding degree of discoloration. In this paper discoloration was performed using Fenton (FeSO47H2O+H2O2+H2SO4) and Fenton-like (FeCl36H2O+H2O2+HCOOH) chemical methods and physico-chemical method of coagulation / flocculation (using polyelectrolyte (POEL) combining anion active coagulant (modified poly-acrylamides) and cationic flocculant (product of nitrogen compounds) in combination with adsorption on activated carbon. Suitability of afore-said methods was investigated on reactive dyes, regarding their most common use in textile industry. Oxidative effect of Fenton and Fenton-like reagent resulted in decomposition of colored chromogen and high degree of discoloration. However, the problem is inability of adding POEL in stechiometrical ratio (also present in physical-chemical methods), when phenomenon of overdosing coagulants occurs in order of obtaining higher degree of discoloration, creating potential danger of burdening water with POEL. Input and output water quality was controlled through spectrophotometrical measurements and standard biological parameters. Keywords: discoloration, reactive dyes, Fenton, coagulation/flocculation, polyelectrolyte, water quality. Introduction Literature divides wastewater purifying into two main categories. First category refers to a survey of procedures and processes of waste water purifying, dividing them into four main groups. Each of the procedures within the category is to produce a higher degree of water purity, removing undesirable substances and making water suitable for recycling, letting out into waterways or even drinking. Three main purifying procedures are preceded by preliminary procedure called screening, which is to remove rather large particles, which could interfere with subsequent purification steps. Primary purifying procedures consider removing unsettled matter by the processes of settling, emerging and percolation on micro screens. Secondary purifying procedures consider various biological, chemical and physical-chemical processes, which are to remove biodegradable matter. Tertiary purifying procedures, often called advance technology, refer to removal of nitrogen, phosphorus, heavy metals and dissolved inorganic matter. Second main category determines the goals of certain purifying degrees in order of distinguishing more accurately, what is excepted out of each purifying degree (1, 2(. This paper revises problems which may occur if only one of the procedures is used, showing both its advantages and disadvantages. Further elaboration suggests solution of the problem by combining certain methods in order of improving purity degree. The paper is to present the problems which may occur when Fenton and Fenton-like chemical methods are used, referring mainly to inability of calculating accurately their amount which leads to undesirable residual amount of ferric ions. Further more, paper presents purification coagulation/flocculation (by poly-electrolyte POEL), which combines anion active coagulant coagulant and cationic flocculant. The result is high discoloration degree, often achieved by overdosing coagulants and unwanted wastewaters burdening with POEL. Solution of the problem presents itself in additional purification process of adsorption on activated carbon (1-4(. Suitability of these methods was investigated on reactive dyestuffs, considering their most common use in cotton fibres dyeing. In addition, over 60 percent of overall dyestuff used, belongs to a group of reactive dyestuff. Furthermore, it was necessary to carry out investigations considering different chemical constitutions referring to associated chromophore, as follows: anthracinone, xanthene and phtalocyanine. Obtained results are represented through spectrophotometrical measurements with calculated discoloration degrees as well as measurements of standard biological parameters, such as pH, electrical conductivity, COD and TOC. Also, amount of residual ferric ions for Fenton and Fenton-like purifying process was measured. Materials and methods Suitability of selected chemical and physical-chemical methods has been investigated for dyestuff of different chemical constitution, as shown in equations 1, 2 and 3. Elaborated purifying methods were, as follows: Fenton and Fenton-like process as the representatives of chemical discoloration methods and coagulation followed by flocculation discoloration method as the representative of physical-chemical methods. Selection of purifying methods presented in the paper was mainly based on the ongoing trend, which favors these methods due to their economical benefits, achieved results and simple application. All spectrophotometrical values were obtained by measurements carried out on Varians Cary 50 spectrophotometer, while standard biological parameters were measured on Macherey-Nagels Nanocolor 500 D spectrophotometer. Electrical conductivity was measured on Metrels MA 5950 conductivity meter and pH on Metrels MA 5736 pH meter. Dyestuff Investigations were performed on dye-rich colored wastewaters containing 1g/l of different chemical constitution dyestuff. Equation 1 shows vinilsuphone reactive dyestuff with associated anthracinone chromophore, while equation 3 shows reactive dyestuff with associated phtalocynine chromphore. Equation 2 shows acid dyestuff with associated xanthene chromophore. Chemical constitution of selected dyestuffs:  C.I. Reactive Blue 19 (1)  EMBED ISISServer  C.I. Acid Red 52 (2)  C.I.Reactive Blue 116 (3)  Methods used Simulated dye-bath solutions were discolored by preliminary optimized chemical and physical-chemical methods. Considering the heterogeneity of dye-house wastewaters, addition of purifying chemicals in stechiometrical ratio was impossible. Avoiding the preliminary step of optimizing the process of purification could lead to unnecessary pollution of wastewaters, now caused by excessive amounts of ferric ions or poly-electrolytes. All of the problem statements are described to the detail in literature references (5-8(. Chemical discoloration methods Fenton (FeSO47H2O+H2O2+H2SO4) (5-7( Fenton-like (FeCl36H2O+H2O2+HCOOH) (5-8( All of the processes were carried out at 25 and 60 C. Temperature of 25 C is the usual temperature under which purification using ferric salts should be performed. Considering how legislation allows outlet wastewaters of higher temperature, additional purifying was carried out at 60 C, also favored because of the avoided wastewater cooling process. Degree of discoloration, for selected dyestuffs, was calculated based on obtained spectrophotometrical values, results of which are shown in Figure 1. Amount of residual ferric ions vs. the dyestuff concentration (1 and 2 g/l) was determined spectrophotometrically, with results shown in Figure 2. Physico-chemical methods coagulation / flocculation (using polyelectrolyte (POEL) combining anion active coagulant (modified poly-acrylamides), eq. 4, and cationic flocculant (product of nitrogen compounds, eq. 3)) (8, 9( adsorption on activated carbon (8, 9(  Anion active polyelectrolyte (4) Cationic polyelectrolyte (5) Discolration was performed using preliminary optimized method, which was to produce easily removable firm floccule (8, 9(. Method optimization implies neutralization of wastewater and varying mixing speed, from 700 rpm in the first phase (addition of anionic coagulant) to 150 rpm in the second phase (addition of cationic flocculant). In order of completely eliminating turbidity after the removal of firm floccules, additional purifying step of adsorption on activated carbon had to be performed. This made possible to spectrophotometrically determine the degree of discoloration, results of which are shown in Figure 1. Discoloration of simulated dye-bath waste water After the investigations and analyses performed on simulated dye-bath wastewaters obtained after dyeing under real conditions had to be carried out. Cotton material was dyed using 3% C.I. Reactive Blue 19 dye-bath with the addition of 60g/l NaCl, 5g/l Na2CO3 and 2 ml/l NaOH 32%. After treatment processes included material rinsing and neutralization of obtained wastewaters. Discoloration methods were Fenton-like (FeCl36H2O+H2O2+HCOOH) and coagulation /flocculation followed by adsorption on activated carbon. Analyses of wastewaters included measurements of pH, electrical conductivity, TOC and COD. Obtained results are shown in Table 1. Results and discussion Figure 1 shows how modification of classical Fenton process, that is use of ecologically more suitable organic formic acid with FeCl3, is to provide similar discoloring degree. However, both of the investigated chemical methods record negative effect of higher wastewater temperature, which varied depending on dyestuff chemical constitution. Higher temperatures caused increased decomposition of H2O2, which results in lower discoloration degree. The highest discoloration degree was obtained for C.I. Reactive Blue 19 (over 90 %). Applied coagulation/flocculation i.e. physical-chemical methods provided with results showing discoloring degree to be less dependent of dyestuff chemical constitution, but rather more to depend on dyestuff molecule size and solubility. This has been confirmed through discoloring degree data obtained for highly soluble, small molecule sized C.I. Acid Red 52.  Figure 1: Degree of discoloration vs. discoloring methods for C.I. Reactive Blue 19, C.I. Acid Red 52, C.I.ReactiveBlue116 One of the greatest negative effects of the presented chemical discoloration processes is the inability to stechiometrically add Fe salts according to the amount of dye in wastewater, quantity of which varies significantly depending on the very dyeing process being performed. This is best seen in Figure 2, where the amount of residual ferric ions decreases with the dyestuff concentration, suggesting how a great portion of ferric ions took part in decomposing dyestuff. Arising ecological problem represent excessively added ineffective Fe-salts, which end up only additionally burdening wastewaters.  Figure 2: Quantity of residual ferric ions vs. C.I. Reactive Blue 19 dyestuff concenrtation Wastewater obtained after dyeing (according to 2.3.), showed typically high values of ecological parameters, which record a significant decrease after each purifying method performed. In addition, advantages of all presented methods are insignificant influence of dyeing auxiliaries on both discoloration degree and measured ecological parameters. One of the important disadvantages of physical-chemical methods came to light after COD measurements. Intolerably high COD value presented a problem which had to be solved. This was done by adding an additional purification phase of adsorption on activated carbon, after which COD values assimilated acceptable values. Table 1: Ecological parameters of simulated dye-bath wastewaters obtained before and after purifying processes BathpHk (mS/cm)TOCCODSimulated dye-bath10.3087.98002300After rinsing and neutralisation7.8216.02501600( Chemical method Fenton-like (FeCl36H2O+H2O2+HCOOH), 25C7.1216.17060( Physical- chemical methodcoagulation / flocculation7.4215.81501000adsorption on activated carbon7.3013.310080 Conclusion Elaborated methods are easy to use and apply, usable for a wide variety of dyestuffs considering their chemical and dyeing properties. Cost benefit is proved through low investments, energy save and less man-power. However, disadvantages of both chemical and physical-chemical methods are the inabilities to stechiometrically add chemicals used for discoloring, which end up additionally burdening wastewaters. In addition, large quantities of sludge are being produced as a byproduct of purifying process, which has to be taken care of. Results confirmed the necessity of combining several purifying methods in order of achieving acceptable values of standard ecological values. References Tedeschi, S.: Zatita voda, Hrvatsko druatvo graevinskih in~enjera, ISBN 953-96085-8-9, Zagreb, (1997) Parac - Osterman, . & uraaevi, V.:  HYPERLINK "http://bib.irb.hr/prikazi-rad?&rad=204300" \t "_blank" Biological Treatment Of Coloured Waste Water Using Wetland System, Proceedings of 5th International Istambul Textile Conference, Akalin, M. (Ed.), Istanbul, Marmara University, Tehnical Education Faculty, Department of Textile Studies, Istanbul (2005) Bulc, T. & Sajn-Slak, A.: Performance of constructed wetland for highway runoff treatment, Water sci. technol., 48 (2003) 315-322, ISSN 0273-1223 Dewick, P., et al: Technological change, industry structure and the environment, Futures, 36 (2004) 267293, ISSN 0016-3287 Tak-Hyun K., et al: Decolorization of disperse and reactive dye solutions using ferric chloride, Desalination 161 (2004) 49-58, ISSN 0011-9164 Ferrero, F.: Oxidative degradation of dyes and surfactant in the Fenton and photo-Fenton treatment of dyehouse effluents, Journal of the Society of Dyers and Colorists, 116 (2000) 5/6, 148-153, ISSN 0037-9895 Papi, S., et al: Removal of reactive dyes from wastewater using Fe(III) coagulant, Journal of the Society of Dyers and Colorists, 116 (2000) 11, 352-358, ISSN 0037-9895 Sutlovi, A.: Study of cotton reactive dyeing from recycled dyebath, University of Zagreb, Faculty of Textile Technology, master thesis, mentor: Parac-Osterman, ., Zagreb (2002) Parac-Osterman, . & Sutlovi, A.  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(Ed.), pp. 7-10, Gdansk, Faculty of Engineering and Marketing of Textiles, Technical University of Lodz, Lodz (2003) Author(s): Prof. urica PARAC-OSTERMAN, Ph.D.University of Zagreb, Faculty of Textile Technology, Department for Technologies of Textile Chemistry and EcologyPrilaz baruna Filipovia 30, HR-10000 Zagreb, CroatiaPhone: +(385) (1) 4877 359Fax: +(385) (1) 4877 355E-mail:  HYPERLINK "mailto:djparac@ttf.hr" djparac@ttf.hr  Vedran URA`EVI, B.Sc.University of Zagreb, Faculty of Textile Technology, Department for Technologies of Textile Chemistry and EcologyPrilaz baruna Filipovia 30, HR-10000 Zagreb, CroatiaEF,-/C 2NRTǹϱϦ|o|g[gPg>#jhguhYM7UmH sH hBChYM7mH sH jhYM7UmH sH hYM7mH sH hJhYM7^JmH sH hYM7hSchYM7^JaJmH sH hYM7^JaJhYM7ho^JaJmH sH hSchq^JaJhb'{^JaJhScho6]^JaJh?^JaJhScho^JaJjhSchoU^JaJU'hScho0J>*B*\^JaJph<>"$țxK9kd7$$Ifl&~&~&64 la9kd$$Ifl&~&~&64 la $IfgdfE.9kd$$Ifl&~&~&64 laTVrtxz|z|ШԨ֨ب *8 0VZ\^ޮڪޟލxplh2njh2nU)hYM7h B*CJ^JaJmH phsH #j;hguhYM7UmH sH h3hYM7mH sH h #jhguhYM7UmH sH hBChYM7mH sH UhJhYM7^JmH sH hYM7hYM7mH sH hguhYM70JmH sH jhYM7UmH sH *xz|V9kd$$Ifl&~&~&64 la $IfgdfE.gdYM7bkdB$$Ifl4Fh =&   ~&6    4 laf48j 9kdJ$$Ifl&~&~&64 la $IfgdfE.9kd$$Ifl&~&~&64 laPhone: +(385) (1) 4877 365Fax: +(385) (1) 4877 355E-mail:  HYPERLINK "mailto:vedran.duresevic@ttf.hr" vedran.duresevic@ttf.hr  Ana SUTLOVI, M. Sc.University of Zagreb, Faculty of Textile Technology, Department for Technologies of Textile Chemistry and EcologyPrilaz baruna Filipovia 30, HR-10000 Zagreb, CroatiaPhone: +(385) (1) 4877 365Fax: +(385) (1) 4877 355E-mail:  HYPERLINK "mailto:ana.sutlovic@ttf.hr" ana.sutlovic@ttf.hr     3rd INTERNATIONAL TEXTILE, CLOTHING & DESIGN :< V9kd$$Ifl&~&~&64 la $IfgdfE.gdYM7bkdy$$Ifl4Fh =&   ~&6    4 laf4 "ƪ9kd$$Ifl&~&~&64 la $IfgdfE.9kd5$$Ifl&~&~&64 la%ST]y&`#$ &dP ^gdTbkd$$Ifl4Fh =&   ~&6    4 laf4%/1679>TU[\]_`aghijkmnýýӽýòý󮪢ӗz)hYM7h B*CJ^JaJmH phsH jhlgUj? hlgUVjhlgUhSh.h?0JmHnHu hlg0Jjhlg0JUh/Uhlg hlgH* h.H*h.jhlgUmHnHuh2njh2nU+CONFERENCE Magic World of Textiles October 08th to 11th 2006, DUBROVNIK, CROATIA PAGE  PAGE 5 EMBED CorelPhotoPaint.Image.9 ]^_`klmnopqrstuvwxyz{|}~ $$dNa$ $&`#$a$&`#$ ^gdT,1h. 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