ADSORPCIJA JONA BAKRA KORIŠĆENJEM TRINE BUKVE *
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1 Zbornik radova Tehnološkog fakulteta u Leskovcu ISSN UDK 004/ (05) 20 (2011), UDK :546.56: /.8 Originalni naučni rad ADSORPCIJA JONA BAKRA KORIŠĆENJEM TRINE BUKVE * Dragana Božić 1, Milan Gorgievski 1, Velizar Stanković 2, Vlastimir Trujić 2 1 Institut za Rudarstvo i Metalurgiju Bor, Bor, Srbija, 2 Tehnički fakultet u Boru, Univerzitet u Beogradu, Bor, Srbija. U radu su prikazani rezultati adsorpcije jona bakra iz sintetičkih rastvora korišćenjem trine bukve kao adsorbensa. Izvršena je fizička i hemijska karakterizacija trine, to jest određen sadržaj alkalnih i zemnoalkalnih metala u njoj i u vodi nakon ispiranja trine i nakon adsorpcije bakra iz razblaženih vodenih rastvora. Odredjen je sadržaj organskog u ispirnoj vodi standardnom metodom pomoću rastvora KMnO 4, pri čemu je potrošnja kiseonika iznosila 0.8 mg/l. Takođe je određen i ukupni kapacitet izmene katjona alkalnih i zemnoalkalnih metala između trine i vodene faze sa NH 4 Cl. Ukupni kapacitet izmene katjona iznosio je 1.45 mmol Me z+ /g trine (Me z+ ovde predstavlja jone alkalnih i zemnoalkalnih metala). Odredjena je kinetika adsorpcije. Simultano je praćena promena ph vrednosti vodene faze tokom adsorpcije. Maksimalni kapacitet adsorpcije Cu 2+ iznosio je 4.5 mg/g. Kinetika adsorpcije je relativno brz proces, dostižući ravnotežu nakon 20 minuta. Adsorpcione izoterme su pokazale dobro slaganje sa Lengmuirovim modelom. Sam mehanizam adsorpcije se odvija jonskom izmenom, pri čemu joni bakra bivaju izmenjeni atomima kalcijuma i vodonika sadržanim u molekularnoj strukturi trine. Rezultati pokazuju da se trina može koristiti kao jeftin adsorbent za adsorpciju jona bakra iz vodenih rastvora. Ključne reči: adsorpcija, trina bukve, joni bakra UVOD Uklanjanje jona metala iz različitih efluenata je stalan predmet interesovanja istraživača u svetu. Rudničke vode koje nastaju u aktivnim, ili zatvorenim, rudnicima * Rad saopšten na IX Simpozijumu Savremene tehnologije i privredni razvoj, Leskovac, 21. i 22. oktobar godine Adresa autora: Dragana Božić, Institut za Rudarstvo i Metalurgiju Bor, Zeleni bulevar 35,19210 Bor, Srbija dragana.bozic@irmbor.rs 27
2 teških obojenih metala su jedan od takvih efluenata sa značajnim sadržajem odgovarajućih jona teških metala u sebi, te predstavljaju ozbiljan i dugotrajan izvor zagađivanja prirodnih vodotokova iz svog okruženja [1]. Joni teških metala mogu biti uklonjeni iz rudničkih voda više ili manje efikasno postojećim konvencionalnim tehnologijama kao što su : hemijska precipitacija i neutralizacija, cementacija i elektrolitičko izdvajanje metala [2]. Trina bukve je korišćena zato što je to drvo dominantno na Balkanskom prostoru, naročito u onim delovima gde postoje ili su postojali rudnici teških obojenih metala, pa se njegovom eksploatacijom stvara značajna količina trine, koja bi mogla da se iskoristi kao adsorbens za jone teških metala, o čemu su neka prethodna istraživanja dala pozitivne rezultate [3]. Cilj rada bio je da se odredi adsorpcioni potencijal korišćene trine za jone bakra koji su zastupljeni u drenažnim rudničkim vodama, kao i da se ustanovi uticaj pojedinih parametara, koji utiču na adsorpcioni proces i da se odredi mera tog uticaja. Cilj je takođe bio da se razmotri uloga alkalnih i zemnoalkalnih metala pri adsorpciji. EKSPERIMENTALNI DEO Hemikalije. Eksperimenti adsorpcije jona bakra na trini su izvođeni korišćenjem sintetičkog rastvora Cu 2+ konstantne polazne koncentracije 0.2 g dm -3. Za određivanje organskih materija u vodi nakon ispiranja trine, odnosno nakon adsorpcije, korišćeni su rastvori M KMnO 4 i M rastvor oksalne kiseline. Za određivanje ukupnog kapaciteta izmene katjona (KIK) korišćen je rastvor 1 M NH 4 Cl. Rastvori su pripremani sa hemikalijama koje su bile p.a.čistoće. Adsorbens. Trina bukve iz lokalnih pilana je korišćena kao adsorbens u ovim eksperimentima. Trina je prosejavana na laboratorijskim sitima i sitovna frakcija <1 mm korišćena je za eksperimente adsorpcije. Radi karakterizacije adsorbensa urađeno je sledeće: određen je hemijski sastav trine, izvršeno je ispiranje trine vodom u cilju određivanja u vodi rastvornih organskih materija, određen je ukupni kapacitet izmene katjona (KIK) i COD. Tabela 1. Hemijski sastav pepela trine. Element Na 2 O K 2 O MgO CaO Fe 2 O 3 SiO 2 Sadržaj, % Element SO 3 Al 2 O 3 P 2 O 5 TiO 2 MnO Ostalo Sadržaj, % Hemijski sastav trine. Radi određivanja sadržaja alkalnih i zemnoalkalnih metala, ali i ostalog neoganskog u razmatranom adsorbensu, određena masa trine (77 g) je sušena, 28
3 da bi se odredio procentualni udeo vlage u njoj. Procenat vlage je iznosio 8.58 %. Trina je potom žarena 1 h na C, da bi se sav organski ugljenik preveo do CO 2. Nakon žarenja, izmerena je masa pepela. Procenat pepela iznosio je 2.06 % od polazne mase trine koja je spaljena, odnosno % sračunato na suvu masu. Hemijski sastav pepela prikazan je u tabeli 1. Ispiranje trine destilovanom vodom vršeno je radi određivanja stepena izluženja alkalnih i zemnoalkalnih metala iz trine. Određena količina trine (1 g) stavljena je na filter papir koji je postavljen u stakleni levak. Trina je ispirana sa 200 ml destilovane vode, u porcijama od po 20 ml. Nakon svake protekle porcije merena je ph vrednost i uzimani su uzorci radi određivanja Na +, K +, Mg 2+ i Ca 2+ u filtratu. U Tabeli 2 prikazan je sadržaj alkalnih i zemnoalkalnih metala nakon proteklih 200 ml destilovane vode. Tabela 2. Sadržaj alkalnih i zemnoalkalnih metala u rastvoru nakon ispiranja trine destilovanom vodom Jon Na + K + Ca 2+ Mg 2+ Koncentracija (mg g -1 ) % Izluženja Određivanje organskih materija u vodi od pranja (COD). Prilikom ispiranja trine vodom, voda od pranja je imala žućkastu boju koja je posledica izluženja organskih materija iz trine. S toga je voda od ispiranja poslužila za odredjivanje COD. Sadržaj organskih materija u vodi od pranja određen je na osnovu potrošnje KMnO 4 na osnovu čega je određena količina kiseonika potrebna za oksidaciju organskih materija (COD) u vodi od ispiranja trine. Potrošnja kiseonika je iznosila 0.8 mg/l. Ukupni kapacitet izmene katjona (KIK). Ukupni kapacitet izmene katjona (KIK) između trine i vodene faze određen je mešanjem 1 g trine sa 50 ml 1 M rastvora NH 4 Cl [4]. Suspenzija je mešana 24 sata u magnetnoj mešalici konstantnom brzinom mešanja od 300 o min -1. Rezultati su prikazani u tabeli 3. Tabela 3. Sadržaj alkalnih i zemnoalkalnih metala u rastvoru nakon dovođenja u kontakt trine sa 1M NH 4 Cl Jon Na + K + Ca 2+ Mg 2+ Koncentracija (mmol g -1 trine) Na osnovu rezultata datih u Tabeli 3, ukupni kapacitet izmene katjona iznosi 1.45 mmol Me z+ /g. (Me z+ predstavlja jone alkalnih i zemnoalkalnih metala). Iz Tabele 3 može se videti da je dominantni jon u izmenljivom položaju Ca 2+ sa najvećim kapacitetom izmene katjona (>80%), dok je kapacitet Na +, K + i Mg 2+ skoro isti, ali za jedan red veličine manji od kapaciteta Ca 2+. Ovo znači da se joni kalcijuma, prisutni u 29
4 strukturi trine, mehanizmom izmene jona izmenjuju sa jonima bakra tokom adsorpcije, te da kapacitet izmene Ca 2+ određuje kapacitet adsorbensa [3]. Postupak izvođenja eksperimenta adsorpcije. Eksperimenti adsorpcije jona metala na trini su izvođeni u laboratorijskim čašama sa magnetnom mešalicom, za održavanje trine u suspenziji. Eksperimenti su izvođeni pri konstantnoj brzini mešanja (300 o min -1 ). Kao adsorbens je korišćena trina prethodno isprana sa 200 ml destilovane vode. Kao vodena faza korišćen je sintetički rastvor jona Cu 2+ početne koncentracije 0.2 g dm -3 i početne vrednosti ph = 4.9. Trina, mase 1 g, dovođena je u kontakt sa 50 ml sintetičkog rastvora datog jona, za različito vreme kontakta faza i održavana u suspenziji mešanjem. Nakon određenog vremena, suspenzija je filtrirana i filtrat analiziran na preostali sadržaj jona ispitivanog metala, kao i na sadržaj alkalnih i zemnoalkalnih metala. Iz materijalnog bilansa određivana je količina adsorbovanog metala, kapacitet adsorpcije i njegova promena sa vremenom. Tokom adsorpcije praćena je promena ph vrednosti rastvora sa vremenom. Svi eksperimenti su izvođeni na sobnoj temperaturi. REZULTATI I DISKUSIJA Promena početne vrednosti ph sa vremenom pri adsorpciji Praćenjem promene ph vrednosti vodene faze tokom adsorpcije, primećena je nagla promena ph na samom početku procesa adsorpcije, koja se manifestovala padom ph vrednosti u prvih nekoliko minuta adsorpcije, a potom povećanjem u narednih nekoliko minuta, te dostizanje ph vrednosti približno jednake onoj inicijalnoj. Sve ove promene su se odigravale u prvih minuta od početka procesa, kada se dešava i najveća promena brzine adsorpcije. Na Slici 1 prikazana je promena početne vrednosti ph rastvora bakra sa vremenom tokom adsorpcije. Slika 1. Promena ph sa vremenom pri adsorpciji bakra Uočava se sa slike 1. da ph vrednost naglo opadne već u prvom minutu, da bi zatim već u sledećem minutu naglo porasla i do kraja adsorpcije imala tendenciju blagog rasta. 30
5 Kinetika adsorpcije Kinetika adsorpcije je ispitivana sa ciljem da se dobije uvid u to kako se količina adsorbovanog metala menja sa vremenom, kao i o vremenu potrebnom da se postigne ravnoteža između vodene i čvrste faze. U ovoj seriji ekspremenata, početna koncentracija jona metala bila je 0.2 g dm-3, dok je ph vrednost bila oko 5, vreme trajanja eksperimenta bilo je 90 minuta. Promena kapaciteta sa vremenom prikazana je na Slici 2, sa slike se može videti da se proces dešava u dva koraka. U prvih 5-10 minuta adsorpcija se odvija dosta brzo, postižući stabilno stanje nakon 20 minuta, nakon toga beleži se porast do postizanja zasićenja. Kinetika adsorpcije može se prikazati jednačinom pseudo drugog reda. Slika 2. Promena kapaciteta adsorpcije sa vremenom Izoterme adsorpcije Ravnoteža između adsorbata, adsorbovanog na aktivnim mestima u adsorbentu i adsorbata zaostalog u tečnoj fazi najčešće se prikazuje izotermama adsorpcije. Sa ciljem da se opišu adsorpcione karakteristike low-cost sorbenata, ravnoteža između adsorbensa i adsorbata najčešće se opisuje pomoću modela bilo Langmuira i Freundlicha [5-8]. Slika 3. Adsorpcione izoterme (levo) i linearizovane Langmuirove krive (desno). 31
6 Mehanizam adsorpcije U tabeli 4 prikazani su rezultati koji praktično potrvrđuju postojanje mehanizma adsorpcije. Utvrđivanjem sadržaja alkalnih i zemnoalkalnih metala u trini, zatim merenjem količine otpuštenih katjona (Na +, K +, Ca 2+, Mg 2+ ) prilikom ispiranja trine destilovanom vodom i merenjem količine otpuštenih katjona nakon adsorpcije bakra, praktično je zaokružena slika o mehanizmu adsorpcije. Tabela 4. Sadržaj alkalnih i zemnoaklalnih metala u trini i u rastvoru nakon adsorpcije jona bakra Jon Sadržaj u trini (mg/g) Sadržaj u trini nakon ispiranja (mg/g) Sadržaj nakon adsorpcije bakra (mg/g) Na K Ca Mg Iz tabele 4 se može videti da je sadržaj alkalnih i zemnoalkalnih metala u trini značajan pri čemu dominira jon kalcijuma. Takođe se može primetiti da je prilikom ispiranja trine destilovanom vodom došlo do delimičnog izluženja alkalnih i zemnoalkalnih metala. Na osnovu svega može se pretpostaviti das u mehanizmom izmene jona, pre svega joni Ca 2+ i Mg 2+, tokom adsorpcije bili izmenjeni jonima bakra. ZAKLJUČAK Rezultati prikazani u ovom radu pokazuju da se trina bukve može uspešno koristiti za adsorpciju jona bakra iz vodenih rastvora. Maksimalni kapacitet adsorpcije postiže se nakon 90 minuta procesa i iznosi 4.5 mg g -1. Potrošnja kiseonika potrebna za oksidaciju organskih materija u vodi od ispiranja trine iznosila je 0.8 mg L -1. Ukupni kapacitet izmene katjona između trine i vodene faze iznosio je 1.45 mmol Me z+ /g trine. Dominantni joni u izmenjivom položaju su Ca 2+ i Mg 2+ sa najvećim kapacitetom izmene katjona u odnosu na ostale jone. Ovo znači da se joni kalcijuma i magnezijuma koji su prisutni u strukturi trine, najverovatnije mehanizmom izmene jona izmenjuju sa jonima bakra i vodonika tokom adsorpcije. Zahvalnica Ovaj rad je finansijski podržan od strane Ministarstva za prosvetu i nauku Republike Srbije kroz projekat br. TR
7 LITERATURA [1] V. Stanković, D. Božić, M. Gorgievski, G. Bogdanović, Heavy metal ions adsorption from mine waters by sawdust, Chemical Industry & Chemical Engineering Quarterly 15 (4) (2009) [2] F. Habashi, Handbook of Extractive Metallurgy, Vol. 4, WILEY-VCH Germany (1997). [3] D. Božić, V. Stanković, M. Gorgievski, G. Bogdanović and R. Kovačević, Adsorption of heavy metal ions by sawdust of deciduous trees; J. Hazard. Mater. 171(2009) [4] S. Matijašević, A. Daković, Adsorption of uranyl ion on acid modified zeolitic mineral clinoptilolite, Chemical Industry 63 (5) 2009, [5] M. Šćiban, M. Klašnja and B. Škrbić; Modified softwood sawdust as adsorbent of heavy metal ions from water, J.Hazard.Mater. B136 (2006) [6] S. Larous, A. Meniai, M. B. Lehocine; Experimental study of the removal of copper from aqueous solutions by adsorption using sawdust, Desalination 185 (2005) [7] M. Šćiban, B. Radetić, Z. Kevresan, M. Klašnja; Adsorption of heavy metals from electroplating wastewater by wood sawdust, Bioresour. Technol. 98 (2007) [8] A. Shukla, Y. H. Zhang, P. Dubey, J.L. Margrave, S. S. Shukla; The role of sawdust in the removal of unwanted materials from water, J.Hazard.Mater.B95 (2002) SUMMARY THE ADSORPTION OF COPPER IONS ONTO BEECH SAWDUST (Original scientific paper) Dragana Božić 1, Milan Gorgievski 1, Velizar Stanković 2 1 The Institute for Mining and Metallurgy Bor, Bor, Serbia 2 Technical Faculty in Bor, University of Belgrade, Bor, Serbia The paper presents the results of adsorption of copper ions from a synthetic solution onto sawdust as an adsorbent. Physical and chemical characterization of sawdust was performed and the content of alkali and alkaline earth metals in aqueous phase, before and after rinsing of sawdust with water, and after adsorption of sawdust with copper, was determined. Total oxygen demand (TOD) was determined volumetrically by means of KMnO 4 solution and consumption of oxygen was 0.8 mg/l. Besides the TOD, the total cation exchange capacities of alkali and alkaline earth metals that are exchanged in the reaction with NH 4 Cl were also determined. The determined total cation exchange capacity (CEC) of the sawdust was 1.45 mmol Me z+ /g sawdust. (Me z+ here denotes alkali and alkaline earth metal ions). The change of the initial ph value and the adsorption capacity with time was also determined. The maximum adsorption capacity evaluated from these results was 4.5 mg/g. The adsorption kinetics was 33
8 relatively fast, reaching the equilibrium for less than 20 min. From the adsorption isotherms it was found that the adsorption equilibrium follows Langmuir adsorption model. The adsorption of copper ions on the sawdust occurs via an ion exchange mechanism. The results show that beech sawdust can be used as a cheap, natural adsorbent for the adsorption of copper ions from industrial effluents. Key words: adsorption; sawdust; copper ions Primljen / Received: 13. maj godine Prihvaćen / Accepted: 12. jul godine 34
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