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Piseth Som

Applications of Fenton and Fenton-like Reactions with Subsequent Hydroxide Precipitation for Derusting Wastewater Treatment. Piseth Som. Master Program in Chemical and Environmental Engineering 07 January 2014. Outline. Background and Problems Rational and Importance

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Piseth Som

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  1. Applications of Fenton and Fenton-like Reactions with Subsequent Hydroxide Precipitation for Derusting Wastewater Treatment PisethSom Master Program in Chemical and Environmental Engineering 07 January 2014

  2. Outline Background and Problems Rational and Importance Theoretical and Empirical Reviews Materials and Experiment

  3. Background and Problem Rust (Fe2O3) • Cleaning operations of pipes and boilers • To dissolve rust • hydrochloric acid or Alkali Flushing • Hot and cold water flushing • Ammoniated Ethylene DiamineTetraacetic Acid (EDTA) Pickling • Pasivative agent (Sodium Nitrite) • Ammonia rinsing (Bansal, 2012) • www.fourquest.com/chemicalcleaning

  4. Background and Problem Generation of Complex Wastewater • High content of metal and organic chelating agent • 5000-10000 mg/L of iron • <100 mg/L of Copper (Huang et al., 2000) • Organic acid (EDTA and Citric Acid) cause metal-complexation(Fu et al., 2012; Chitra et al., 2011 ) • Kation Power (2010) • www.chemicool.com/defination/ligand

  5. Rational and Importance Ability of Fenton reaction for organic degradation and industrial wastewater treatment (Buatista et al., 2008)

  6. Rational and Importance Fenton and Fenton-like reactions for derusting wastewater is not well documented Feasibility for NiEDTA and CuEDTA treatment, so they may do for FeEDTA (Fu et a., 2009, and Lan et al., 2012) Originated Iron (Fe2+/Fe3+ ) and iron oxide (Fe2O3) in wastewater could be used as catalyst for Fenton-like reaction (Lan et al. 2012)

  7. Objectives

  8. Scope and Limitation • Real derusting wastewater is used in the study • Jar Test apparatus is conducted at laboratory room temperature at DChE, BUU • Objective Parameters: TCOD, SCOD, Total Iron, Soluble Iron, Fe2+, Fe3+, Ammonium, Nitrate, Nitrate, TDS • Kinetic degradation organic chelating agents are monitored in term of COD • Oxidation Products or intermediate are NOT monitored

  9. Theoretical Reviews (Fenton-like) (Fenton-like) pH ~ 3 - 4 pH ~ 3 - 4 pH ~ 3 - 4 pH ~ 3 - 4 pH ~ 3 - 4 Fe3+ + OH•+ OH− Fe3+ + OH•+ OH− (Fenton) H2O2 + Fe2+ H2O2 + Fe3+ H2O2 + Fe2+ Fe3+ + OH•+ OH− H2O2 + Fe2+ Fe2+ + HO2• + OH− Feo(ZVI)+ 2H+ Fe2+ + H2 OH •+ Organic Compound  Oxidized Products Fenton Reactions as Advanced Oxidation Processes (AOP) using hydroxyl radical (OH•) (E0 = 2.8V) (Neyens & Baeyens, 2003)

  10. Theoretical Reviews (Cont’)

  11. Empirical Reviews

  12. Materials and Experiment Derusting Wastewater • Boilers cleaning processes • Kation Power Company located in Rayong Province

  13. Materials and Experiment **Pollution Control Department, PCD at www.pcd.go.th

  14. Materials and Experiment Materials • Jar Test Apparatus • pH meter • Portable TSD meter • Multiple parameters Photometer • Hotplate • UV-Vis spectrophotometer • Drying Oven • Centrifugal Machine • supporting glassware

  15. Materials and Experiment Chemicals for Fenton and Fenton-like reaction Chemicals for parameters analysis • H2O2 – 35% w/w (AR Grade) • FeSO47H2O (AR Grade) • H2SO4 , HCl and HNO3 Conc. • NaOH – 10 N • H2SO4 – 5N • Ferrous Ammonium Sulfate (Fe(NH4 )2(SO4)2·6H2O) • Sodium acetate (NaC2H3O23H2O) • Hydroxylamine(NH2OH-HCl) • 1,10-pehnanthroline (C12H8N23H2O ) • Potassium Permanganate (KMnO4)

  16. Materials and Experiment Add Fe2+ under mixing 150 rpm for 10 min Fill 500 mL of sample adjust pH= 3 Analysis of Objective Parameters adjust pH =8 Add H2O2 under mixing 50 rpm for 60 min Settling for 30 min

  17. Materials and Experiment Input Processes Output • initial pH: 2-7 • [Fe2+] : 0.005-0.15 M • [H2O2]: 1-3.5 M • Reaction Time • 20-120 min • Precipitation pH: 6-11 Fenton-like Reaction (Add H2O2 only) Fenton Reaction (Fe2+ + H2O2) • TCOD, SCOD • Total Iron, Soluble Iron, Fe2+, Fe3+ • Ammonium, Nitrate, Nitrate • TDS room temperature (28 0C ), mixing at 150 rpm and 80 rpm Control variables

  18. Materials and Experiment Varying initial pH pH=2 pH=4 pH=6 pH=8 pH=10 pH=12 Repeat with pH: 2, 3, 4, 5, 6 7  Best pH

  19. Materials and Experiment Varying [H2O2] Varying RT (min) Precipitation pH 1M 1.5M 2M 2.5M 3M 3.5M 6 7 8 9 10 11 20 40 60 80 100 120 Best [H2O2] Best RT (min)

  20. Materials and Experiment Repeat experiment with initial pH around the suitable pH to obtain the best initial pH for Fenton reaction

  21. Materials and Experiment Varying [Fe2+] Varying [H2O2] Varying RT (min) Precipitation pH 0.005M 0.01M 0.05M 0.08M 0.1M 0.12M 1M 1.5M 2M 2.5M 3M 3.5M 6 7 8 9 10 11 20 40 60 80 100 120 Optimum Condition, Impacts of each parameters, Kinetics

  22. Materials and Experiment TCOD and SCOD are determined by close reflux titrimetric method (Method, 5520) Total iron , ferric and ferrous concentration are measure by Phenanthroline method (Method, 3500) pH is measured by pH meter (EUTECH) TSS is measured according to standard method (Method, 2540) TDS is measured by portable TDS meter (OHAUS Starter 300C) Ammonium nitrogen, Nitrate and Nitrite are measured by Multiple parameters Photometer (Hana HI 83205-2008)

  23. Outlook

  24. Outlook

  25. Activity Plan

  26. Thank You for Your Attention ! Q & A?

  27. Materials and Experiment Mixing at 50 rpm for 15 min Settling down for 30 min pH=6 pH=7 pH=8 pH=9 pH=10 pH=11 Does Iron precipitate?  Hypothesis 1 Hydroxide Precipitation of Iron Before Fenton and Fenton-like Reaction

  28. Materials and Experiment Oxidized product (P) + CO2 + H20 Organic Matter (COD )+ OH• Second Order Reaction Integrated Equation Pseudo-first order Reaction Skoog and West , 2004 ; Lucas and Peres , 2007 and Samet et al., 2011 Kinetic Study of COD degradation Rate Equation (r)

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