photocatalysis-of-basic-black-2-janus-black-dye-using-titanium-dioxide

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Citation: Ayebe B Yelling M Amana BS et al. Photocatalysis of Basic Black 2 Janus Black Dye Using Titanium Dioxide Doped with Zinc Zn-TiO 2 . Org Chem Ind J. 2017133:115. © 2017 Trade Science Inc. 1 Photocatalysis of Basic Black 2 Janus Black Dye Using Titanium Dioxide Doped with Zinc Zn-TiO 2 Ayebe B 1 Yelling M 2 Amana BS 1 Obadahun J 1 and Pascaline PL 1 Nigerian Institute of Leather and Science Technology NILEST Zaria Nigeria 2 Department of Chemistry Kaduna State University Nigeria Corresponding author: Ayebe B Nigerian Institute of Leather and Science Technology NILEST Zaria Nigeria Tel: 08063078756 E-mail: bulusayebe1gmail.com Received: May 18 2017 Accepted: June 27 2017 Published: June 28 2017 Introduction Dyes are coloured organic compound that is used to impart colour to a substrate like leather paper cloth plastics etc. and the imparted colour is reasonably wash-fast and lightfast. Azo dyes are the largest group of synthetic dyes used in leather and textile industries which constitutes up to 70 of exclusively the known marketable dyes produced. The processing industries such as leather and textile industries are putting a severe burden on the environment through the release of heavily polluted wastewater and the exposures of these dyes to the environment generate coloration of natural water toxicity carcinogenicity and causes contamination and perturbation in aquatic life in eco-system. The treatment of colored waste water containing hazardous dyes is one of the rising needs of the present time and there is consequently great demand of technology to decolorize these extremely colored dyes waste water more efficiently 1-23. Abstract Photocatalysis of basic black 2 janus black dye was carried out to evaluate the effect of time metal load concentration and light source on the photodegradation of basic black 2 dye. The catalyst was synthesized by wet-impregnation of zinc onto titanium dioxide followed by calcinations at 500°C. The catalyst characterization results indicated that the synthesized TiO 2 powder had a pure two phases of anatase and rutile structures. The level of mineralization of basic black 2 dyes was monitored by taking the absorbance of the dye solution before and after irradiation with the light source at an interval of 20 min. The results obtained indicated that the efficiency of photodegradation of basic black 2 dye was 99.92 95.94 and 74.46 using 1 3 and 5 Zn-TiO 2 under visible light and 98.22 97.46 and 73.61 using 1 3 and 5 Zn-TiO 2 under UV light after irradiation for 80 min respectively. Keywords: Photocatalysis Catalyst Mineralization Titanium dioxide Dye

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www.tsijournals.com | March-2017 2 Traditional chemical physical and biological processes for treating textile dye wastewaters have difficulties such as high cost energy waste and generating secondary pollution during the treatment process and the treatment plant is ineffective in elimination of these dyes from the waste water hence photocatalysis seems as the most emerging destructive technology this is because Titanium dioxide TiO 2 has the greatest efficiency productivity the highest solubility and lowest cost. The key advantage is its inherent destructive nature: it does not involve bulk transfer it can be carried out under ambient conditions atmospheric oxygen is used as oxidant and may lead to whole mineralization of organic carbon into CO 2 and H 2 O. The modification of these photocatalysts facilitates to give better photo activity .Advance oxidation process AOPs have been established to degrade a wide variety of organic compound including dyes. Titanium dioxide particularly in the anatase form is a photocatalyst under ultraviolet UV light. It has been reported that Titanium dioxide when doped with metal is also a photocatalyst under either visible or UV light improved degradation rates due to their improved band gap energy for using visible and solar radiation reduces crystallize size reduces band gap and control the surface property through increase in surface area. Materials and Methods Basic black 2 Janus Black dyes oven X-RD machine centrifuge FT-IR spectrometer UV/Vis- spectrophotometer magnetic stirrer model 79-1 analytical balance model ES-B UV-fluorescence analysis cabinet muffle furnace volumetric flasks magnetic stirrer beakers measuring cylinder spatula syringe titanium dioxide TiO 2 zinc oxide ZnO and distilled Water. Catalyst preparation The Zn doped TiO 2 catalyst was synthesized based on the method of catalyst preparation described by Chakraborty and Roychowdhury. Commercially available titanium dioxide 14.81 g support was weighed and dissolved in 100 ml distilled water as per wet-impregnation method and 0.19 g of zinc oxide was added to synthesize 1 zinc in TiO 2 in total mass of 15 g. The mixture was stirred at ambient temperature using mechanical stirrer for 1h and the powder was separated by decantation. The powder was then dried in an oven at 150°C for 4 h and calcined at 500°C. Similarly 3 and 5 Zn-TiO 2 were synthesized by changing the amount of ZnO to 0.56 g 0.93 g and TiO 2 to 14.44 g and 14.07 g to obtain samples of 3 and 5 Zn-TiO 2 in total mass of 15 g respectively. The synthesized photocatalyst was then characterized using XRD machine to determine the phases and the various minerals present. Photodegradation The photocatalysis was achieved by using UV/Visible analysis cabinet photo-reactor. 0.20 g of Zn-TiO 2 catalyst was weighed into 100 ml of 2 × 10-5 mol. L -1 of the dye in 200 cm 3 beaker. The absorbance of the dye was measured at 620 nm before irradiation and after every 20 min interval. In all the experiment 0.20 g of the catalyst was suspended in 100 ml aqueous solution of 2 × 10-5 mol. L -1 of the dye concentration with constant stirring using a magnetic stirrer. The rate of photodegradation of the dye was assessed through decolourization level of the dye.

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www.tsijournals.com | March-2017 3 After irradiation for every 20 min 10 ml of the solution was taking out of the reactor and centrifuged at a rate of 4000 rpm to remove the photocatalyst and the absorbance was measured. The absorbance of the supernatant was estimated to determine the dye concentration after every 20 min and the used catalyst was use for FT-IR analysis after 80 min of irradiation. FIG. 1. Photo-reactor. SCHEME 1. Basic black 2 dye greenwood and earnshaw 1997.

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www.tsijournals.com | March-2017 4 Results and Discussion XRD patterns of Zn-TiO 2 FIG. 2. XRD pattern for 1 Zn-TiO 2. FIG.3. XRD pattern for 3 Zn-TiO 2. FIG. 4. XRD Pattern for 5 Zn-TiO2. The major minerals contained in 1 Zn-TiO 2 as confirm by the various peaks against corresponding 2 Theta Bragg’s angle were Zn rutile and anatase and the major minerals contained in 3 Zn-TiO 2 as confirm by the various peaks against corresponding 2 Theta Bragg’s angle were: Anatase zinc baite and cadmoselite while the major minerals contained in 5 Zn-TiO 2 as confirmed by the various peaks against corresponding 2 Theta Bragg’s angle was anatase as indicated in FIG. 1to 4 respectively. Photodegradation FIG. 5. Rate of photodegradation of basic black 2 dye using 1 Zn-TiO 2 3 Zn-TiO 2 and 5 Zn-TiO 2 under visible light irradiation. 0 0.5 1 1.5 2 2.5 0 20 40 60 80 100 Concentration ×10 -5 Mol.L -1 Time Min. 1 Zn-TiO2 3 Zn- TiO2 5 Zn-TiO2

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www.tsijournals.com | March-2017 5 FIG. 6. Percentage photodegradation of basic black 2 using visible radiation. FIG. 7. Rate of photodegradation of basic black 2 dye using 1 Zn-TiO 2 3 Zn-TiO 2 and 5 Zn-TiO 2 under UV light irradiation. FIG. 8. Percentage photodegradation of basic black 2 using UV radiation. Effects of time on the photodegradation of basic black 2 dyes For the purpose of this research 100 ml of 2.0 × 10 -5 mol.L -1 of basic black 2 Janus Black dye was used to assess the degree of photodegradation of the dye. 0.20 g of the catalyst was used in all experiment. From the results shown in FIG. 5 to 7 the 0 20 40 60 80 100 120 0 10 20 30 40 50 60 70 80 90 Photodegradation Time Min. 1 Zn-TiO2 3 Zn-TiO2 5 Zn-TiO2 0 20 40 60 80 100 120 0 20 40 60 80 100 Photodegradation Time Min. 1 Zn-TiO2 3 Zn-TiO2 5 Zn-TiO2 0 0.5 1 1.5 2 2.5 0 20 40 60 80 100 Concentration ×10 -5 Mol.L -1 Time Min. 1 Zn-TiO2 3 Zn-TiO2 5 Zn-TiO2

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www.tsijournals.com | March-2017 6 percentage photodegradation was 99.92 95.94 and 74.46 with 1 3 and 5 Zn-TiO 2 under visible light and 98.22 97.46 and 73.61 via 1 3 and 5 Zn-TiO 2 under UV light after irradiation for 80 min respectively and the degree of mineralization of the dye equally increases exponentially with respect to time which is attributed to the fact that as the time increases more light energy falls on the catalyst surface which increases the establishment of photo excited species which in turn improves the photo catalytic activity. The rate of photodegradation of the dye was in the following order for both visible and UV irradiation: 1 Zn-TiO 2 3 Zn-TiO 2 5 Zn-TiO 2 . Effect of light source on the photocatalysis of basic black 2 100 ml of 2.0 10 -5 mol.L -1 of basic black 2 Janus Black dye was used to evaluate the effect of light source on the photodegradation of basic black 2 dye. From the results shown in FIG. 5 and 7 the percentage photodegradation was 99.92 95.94 and 74.46 using 1 3 and 5 Zn-TiO 2 under visible light and 98.22 97.46 and 73.61 using 1 3 and 5 Zn-TiO 2 under UV light after irradiation for 80 Min respectively. The percentage photodegradation under visible light gives better activity compared to UV light irradiation. The higher activity of the modified catalyst might be attributed to the Zn which was used as the doping element which assists in narrowing the band gap of titanium. However the higher activity might also be ascribed to higher surface area and small particle size of the modified catalyst. The percentage of photodegradation of the dye was in the following order for both visible and UV irradiation: 1 Zn-TiO 2 3 Zn-TiO 2 5 Zn-TiO 2 . Effect of metal loading on the photocatalysis of basic black 2 dyes 100 ml of 2.0 10 -5 mol.L -1 of basic black 2 Janus Black dye was used to measure the effect of metal concentration on the photodegradation of basic black 2 dye. From the results shown in FIG. 5 and 7 the percentage photodegradation was 99.92 95.94 and 74.46 using 1 3 and 5 Zn-TiO 2 under visible light and 98.22 97.46 and 73.61 using 1 3 and 5 Zn-TiO 2 under UV light after irradiation for 80 Min respectively. However reduction in the rate of degradation was in the following order: 1 Zn-TiO 2 3 Zn-TiO 2 5 Zn-TiO 2 in both visible and UV light. Conversely the reduction in the photodegradation of basic black 2 using 3 and 5 Zn-TiO 2 could be owing to higher metal concentration which leads to the deactivation of active molecules by collision with ground state molecules thus dominating the reaction. Results for the FT-IR analysis of the used Zn-TiO 2 FIG. 9. FT-IR spectrum of used 1 Zn-TiO 2 after the photodegradation. From the result of the FT-IR spectra of used 1 Zn-TiO 2 shown in FIG. 8-10 a vibration was observed at 1435.09 cm -1 which is assign to O-H due to hydroxyl or alcohol group broken from basic black 2 dye. Also 1633.76 cm -1 is observed due to

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www.tsijournals.com | March-2017 7 CH 2 broken down during the photocatalytic reaction. The 2285.72 cm -1 is for –NCO -N-CN or –N 3 which is the azide group and at 3435.34 cm -1 –N-H is a primary amine formed as intermediate during irradiation. FIG. 10. FT-IR spectrum of used 3 Zn-TiO2 after the photodegradation From the FT-IR spectra shown in FIG. 9 the used 3 Zn-TiO 2 the following can be deduced from the spectrum at various frequencies. The vibration at 1424.48 cm -1 and 3459.45 cm -1 is due to the hydroxyl group present in the dye molecule. The vibration at 1801.57 cm -1 and 2535.51 cm -1 is due to the carboxylic CO group broken down from the dye molecule in the photocatalytic process using visible and UV light. FIG. 11. FT-IR analysis results for used 5 Zn-TiO 2 From the result of the FT-IR spectra of used 5 Zn-TiO 2 shown in FIG. 10 and 11 a vibration is observed at 1437.98 cm -1 which is assign to O-H due to hydroxyl or alcohol group broken from basic black 2 dye. The vibration at 1807.36 cm -1 and 2896.21 cm -1 is observed due to the carboxylic CO and C-H group broken down from the dye molecule. The 3002.30 cm -1 is for CH 3 CH 2 or CH which is the alkane group and at 3448.84 cm -1 is the hydroxyl group broken down during the phocatalytic process. Conclusions Photocatalytic degradation of basic black 2 dyes was carried out using TiO 2 modified with 1 3 and 5 Zn-TiO 2 respectively as Photocatalyst. From the results shown in FIG. 5 and 7 the percentage photodegradation was 99.92 95.94 and 74.46 using 1 3 and 5 Zn-TiO 2 under visible light and 98.22 97.46 and 73.61 using 1 3 and 5 Zn- TiO 2 under UV light after irradiation for 80 Min respectively and the FT-IR analysis results indicated that the basic black 2 dye was mineralized by the Photocatalyst. The degradation efficiency in the visible light seems to be more efficient compare to that of the UV light which could possibly be as a result of Zinc doped in Titanium dioxide which reduces the band gap of

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www.tsijournals.com | March-2017 8 the Titanium and enhances its efficiency in the visible light. The results of this study clearly indicate that organic dyes in the tannery and textile waste can be efficiently degraded in the presence of photocatalyst. Recommendations From the results obtain as shown in FIG. 4 5 6 and 7 1 Zn-TiO 2 was more effective in the photodegradation of the effluent when compared to 3 Zn-TiO 2 and 5 Zn-TiO 2 respectively. Therefore 1 Zn-TiO 2 can be effectively used in the decolourization of basic black 2 dye effluent. Hence more research should be conducted to Optimize PH Temperature Catalyst concentration and mechanism of photo activity of the catalyst on dyes. Acknowledgements The authors wish to express their heartfelt gratitude to Almighty God for the success of the research and also to staff of the Department of Petrochemical National Institute for Chemical Technology NARICT Zaria where the research was conducted. REFERENCES 1. Ahmed HA. Study on the photocatalytic degradation of indigo carmine dye by TiO 2 photocatalyst. Journal of Kerbala University. 2013112. 2. Wu C Chang HW Chern J et al. Basic dye decomposition kinetics in a photocatalytic slurry reactor. J Hazard Mater. 2005137B. 3. Sima J Hasel P. Photocatalytic degradation of textile dyes in TiO 2 /UV system. The Italian Chemical Engineering Transaction. 201332:79-84. 4. Kumar J Bansal A. Dual Effect of photocatalysis and adsorption in degradation of azorubine dye using nanosized TiO 2 and activated carbon immobilized with different techniques. Int J ChemTech Res. CODEN USA. 201023:1537-543. 5. Kazuhito HHI Fujishima A. TiO 2 Photocatalysis: A historical overview and future prospects. Jpn J Appl Phys. 20054412:8269-285. 6. Mondal K Sharma A. Photocatalytic oxidation of pollutant dyes in waste water by TiO 2 and ZnO nano materials : A mini-review. Department of Chemical Engineering Indian Institute of Technology Khanpur India.2010. 7. Kurtoglu ME Longenbach T Gogotsi Y. Preventing Sodium Poisoning of Photocatalytic TiO 2 Films on Glass by Metal Doping. Int J Appl Glass. 20112:108-116. 8. Kvavadze E Bar-Yosef O Belfer-Cohen A et al. 30000 year old wild flax fibers. 9. Devi LG Kottam N Murthy BN et al. Enhanced Photocatalytic activity of metal Mn 2+ Ni 2+ and Zn 2+ doped polycrystalline titania of analine blue under UV/solar light. J Mol Catal. 2010328:44-10. 10. Lachheb H Puzenat E Photocatalytic degradation of various types of dyes Alizarin S Crocein Orange G Methyl Red Congo Red Methylene Blue in water by UV irradiated titania. Appl Catal B. 2002391:75-90. 11. Li Yan-chang Zou Lin-da Eric Hu. Photocatalytic degradation of dye effluent by titanium dioxide pillar pellets in aqueous solution. J Environ Sci. 2004163:375-79.

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www.tsijournals.com | March-2017 9 12. Shanthi M Kuzhalosai V. Photocatalytic degradation of an azo dye acid red 27 in aqueous solution using nano ZnO. Indian J Chem. 20115:428-34. 13. Kulkarni M Thakar P. Photocatalytic degradation and mineralization of reactive azo dye using semi-conductor metal oxide nanoparticles. 2014:245-49. 14. Laid N Bouanimba N Zouaghi R et al. Study of the Photocatalytic Degradation of cationic Dye in aqueous solution by different types of catalyst.2014. 15. Greenwood NN Earnshaw A. Chemistry of Elements 2 nd ed. Butterworth- Hainemann Oxford UK.1997. 16. Potti PR Srivastava VC. Effect of dopants on ZnO mediated photocatalysis of dye bearing waste water: A review Mater Sci Forum. 2013757:165-74. 17. Peternel IT Koprivanac N Locaric Bozic AM et al. Comparative study of a UV/TiO2 UV/ZnO and photo-fenton processes for organic reactive dye degradation in aqueous solution. J Hazard Mater. 2007148:477-84. 18. Preeti Mehta Rajeev Mehta Menka Suranaa et al. Influence of operational parameters on degradation of commercial textile azo dye acid blue 113 Cyanine 5R by avanced oxidation technology J Curr Chem Pharm Sc. 2011. 19. Chakraborty R Roy chowdhury D. Fish bone derived natural hydroxyapatite-supported copper acid catalyst: Taguchi optimization of semibatch oleic esterification. Chem Eng J. 2013215:491-99. 20. Morrison RT Boyd RN. Organic Chemistry. 2011 Seventh Edition1095-1096. 21. Abo-Fara SA. Photocatalytic degradation of monoazo and diazo dyes in wastewater on Nanometer-Sized TiO 2 . Chemistry Department Faculty of Science Al-Azhar University Girls Naser city Cairo Egypt Vol.27. 22. Tehurisa Ohno Koji Sarukawa KojiroTokieda et al. Morphology of TiO 2 Photocatalyst Degussa p-25 consisting of anatase and rutile crystalline phase. J Catal.2001203:82-86. 23. Kim W Tachikawa T Majima T et al. Photocatalysis of dye-sensitized TiO 2 nanoparticles with thin overcoat of Al 2 O 3 : Enhance activity for H2 production and dechlorination of CCL4. 2009.