PHOTOABATEMENT OF WATER POLLUTANTS IN TURBID SUSPENSIONS BY MEANS OF PHOTOACTIVE FLUORINATED TRANSPARENT COATINGS
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1 PHOTOABATEMENT OF WATER POLLUTANTS IN TURBID SUSPENSIONS BY MEANS OF PHOTOACTIVE FLUORINATED TRANSPARENT COATINGS W. Navarrini, Federico Persico, Maurizio Sansotera Dept. CMIC G.Natta, Politecnico di Milano, via Mancinelli 7, Milano, Italy PLAST 2015, May 6, Milano
2 Aim of the Research Production of a chemically stable and resistent coating, able to promote the photooxidation of hydrosoluble organic pollutants [a,b] Organic Compound hν, TiO 2 H 2 O, O 2 Mineralization Products Flexible water treatment system developed up to industrial scale [a] A. Mills, S. Le Hunte, J. Photochem. Photobiol., A 108 (1997) 1. [b] S. Gatto, M. Sansotera, F. Persico, M. Gola, C. Pirola, W. Panzeri, W. Navarrini, C.L. Bianchi, Catal. Today, in press, doi: /j.cattod
![system developed up to industrial scale [a] A. Mills, S. Le Hunte, J. Photochem. Photobiol., A 108 (1997) 1. [b] S. Gatto, M.](/docs-images/45/4207243/images/page_2.jpg "Sansotera, F. Persico, M. Gola, C. Pirola, W. Panzeri, W. Navarrini, C.L. Bianchi, Catal. Today, in press, doi: 10.1016/j.")
3 Photocatalysis as Advanced Oxidation Process [c,d,e] Organic compounds CO 2, H 2 O, N 2 CB Ti IV OH O 2- {HO 2, HO 2-, H 2 O 2, OH - } CO 2 CO, H 2 O,, H 2 NO, 2 Ti IV OH VB Ti III OH O 2 H 2 O Organic compounds Ti IV OH + Ti IV OH H 2 O OH H 2 O Organic compounds CO 2, H 2 O, N 2 [c] O. Carp, C.L. Huisman, A. Reller, Prog. Solid State Chem. 32 (2004) 33. [d] M. Sansotera, F. Persico, C. Pirola, W. Navarrini, A. Di Michele, C.L. Bianchi, Appl. Catal., B 148 (2014) 29. [e] M. Sansotera, S. Gatto, F. Persico, C. Pirola, W. Navarrini, C.L. Bianchi, Decomposition of perfluorooctanoic acid photocatalyzed by titanium dioxide: chemical modification of the catalyst surface induced by fluoride ions, awarded as Best Poster on Sustainability at the 17 th ESFC, Paris, July 2013.
4 Photocatalysis as Advanced Oxidation Process [c,d,e] Organic compounds CO 2, H 2 O, N 2 CB Ti IV OH O 2- {HO 2, HO 2-, H 2 O 2, OH - } CO 2 CO, H 2 O,, H 2 NO, 2 Ti IV OH VB Ti III OH O 2 H 2 O Organic compounds Ti IV OH + Ti IV OH H 2 O OH H 2 O Organic compounds CO 2, H 2 O, N 2 TiO 2 immobilized into a polymeric matrix Chemical stability UV transparency Gas permeability Hydrophilic IONOMERIC AMORPHOUS FLUOROPOLYMERS [c] O. Carp, C.L. Huisman, A. Reller, Prog. Solid State Chem. 32 (2004) 33. [d] M. Sansotera, F. Persico, C. Pirola, W. Navarrini, A. Di Michele, C.L. Bianchi, Appl. Catal., B 148 (2014) 29. [e] M. Sansotera, S. Gatto, F. Persico, C. Pirola, W. Navarrini, C.L. Bianchi, Decomposition of perfluorooctanoic acid photocatalyzed by titanium dioxide: chemical modification of the catalyst surface induced by fluoride ions, awarded as Best Poster on Sustainability at the 17 th ESFC, Paris, July 2013.
![IONOMERIC AMORPHOUS FLUOROPOLYMERS [c] O. Carp, C.L. Huisman, A. Reller, Prog. Solid State Chem. 32 (2004) 33. [d] M. Sansotera, F. Persico, C. Pirola, W. Navarrini, A. Di Michele, C.L. Bianchi, Appl.](/docs-images/45/4207243/images/page_4.jpg "Catal., B 148 (2014) 29. [e] M. Sansotera, S. Gatto, F. Persico, C. Pirola, W. Navarrini, C.L.")
5 Photocatalysis as Advanced Oxidation Process [c,d,e] Organic compounds CO 2, H 2 O, N 2 CB Ti IV OH O 2- {HO 2, HO 2-, H 2 O 2, OH - } CO 2 CO, H 2 O,, H 2 NO, 2 Ti IV OH VB Ti III OH O 2 H 2 O Organic compounds Ti IV OH + Ti IV OH H 2 O OH H 2 O Organic compounds CO 2, H 2 O, N 2 TiO 2 immobilized into a transparent polymeric matrix Chemical stability UV transparency Gas permeability Hydrophilic IONOMERIC AMORPHOUS FLUOROPOLYMERS Easy separation of the treated solution Appliable to turbid solutions Fouling prove photocatalytic assembly [c] O. Carp, C.L. Huisman, A. Reller, Prog. Solid State Chem. 32 (2004) 33. [d] M. Sansotera, F. Persico, C. Pirola, W. Navarrini, A. Di Michele, C.L. Bianchi, Appl. Catal., B 148 (2014) 29. [e] M. Sansotera, S. Gatto, F. Persico, C. Pirola, W. Navarrini, C.L. Bianchi, Decomposition of perfluorooctanoic acid photocatalyzed by titanium dioxide: chemical modification of the catalyst surface induced by fluoride ions, awarded as Best Poster on Sustainability at the 17 th ESFC, Paris, July 2013.
![Hydrophilic IONOMERIC AMORPHOUS FLUOROPOLYMERS Easy separation of the treated solution Appliable to turbid solutions Fouling prove photocatalytic assembly [c] O. Carp, C.L. Huisman, A. Reller, Prog.](/docs-images/45/4207243/images/page_5.jpg "Solid State Chem. 32 (2004) 33. [d] M. Sansotera, F. Persico, C. Pirola, W. Navarrini, A. Di Michele, C.L. Bianchi, Appl. Catal., B 148 (2014) 29. [e] M. Sansotera, S. Gatto, F. Persico, C. Pirola, W. Navarrini, C.")
6 Fluorinated Ionomers Ionomers: TFE + Vinylethers containing sulphonic or carboxylic functions [f] High chemical stability High UV transparency Strong acid behaviour Hydrophilicity [f] W.G. Grot, Fluorinated Ionomers; W. Andrew, Ed.; PDL Handbook Series; Elsevier: Amsterdam, 2008.
![transparency Strong acid behaviour Hydrophilicity [f] W.G.](/docs-images/45/4207243/images/page_6.jpg "Grot, Fluorinated Ionomers; W. Andrew, Ed.")
7 Fluorinated Ionomers Ionomers: TFE + Vinylethers containing sulphonic or carboxylic functions [f] High chemical stability High UV transparency Strong acid behaviour Hydrophilicity Water collects around the clusters of hydrophilic sulphonic side chains [f] High water absorption in which H + can move freely [f] W.G. Grot, Fluorinated Ionomers; W. Andrew, Ed.; PDL Handbook Series; Elsevier: Amsterdam, 2008.
![around the clusters of hydrophilic sulphonic side chains [f] High water absorption in which H + can](/docs-images/45/4207243/images/page_7.jpg "move freely [f] W.G. Grot, Fluorinated Ionomers; W. Andrew, Ed.")
8 Fluorinated Ionomers Ionomers: TFE + Vinylethers containing sulphonic or carboxylic functions [f] High chemical stability High UV transparency Strong acid behaviour Hydrophilicity MW R F Polymer Name Company 446 CF 2 CF O CF 2 CF 2 SO 2 F Nafion DuPont CF Flemion Asahi Glass 3 Aciplex Asahi Chemicals 306 CF 2 CF 2 CF 2 CO 2 CH 3 Flemion Asahi Glass 380 CF 2 CF 2 CF 2 CF 2 SO 2 F 3M Polymer 3M 280 CF 2 CF 2 SO 2 F Dow Polymer Aquivion Dow Chemicals SolvaySpecialtyPolymers Water collects around the clusters of hydrophilic sulphonate side chains [f] High water absorption in which H + can move freely [f] W.G. Grot, Fluorinated Ionomers; W. Andrew, Ed.; PDL Handbook Series; Elsevier: Amsterdam, 2008.
9 Experimental apparatus Quartz sheath TiO 2 containing photoactive coating [g] Low P UV Lamp λ = 254 nm W av = 5 W Polluted aqueous solution Constant O 2 feed (7 L/h) Quartz surface AD60 10% thermally treated AD60 10% non-thermally treated AQ 6% - TiO 2 10% Magnetic stirrer [g] F. Persico, M. Sansotera, C.L. Bianchi, C. Cavallotti, W. Navarrini, Photocatalytic Activity of TiO 2 -embedded Fluorinated Transparent Coating for Oxidation of Hydrosoluble Pollutants in Turbid Suspensions, Appl. Catal., B, 170 (2015) 83-89
![10% Magnetic stirrer [g] F. Persico, M. Sansotera, C.L. Bianchi, C. Cavallotti, W.](/docs-images/45/4207243/images/page_9.jpg "Navarrini, Photocatalytic Activity of TiO 2 -embedded Fluorinated Transparent Coating for Oxidation of Hydrosoluble Pollutants in")
10 Photoactive Coating Low P UV Lamp Polluted aqueous solution O 2 Feed Quartz surface AD60 10% thermally treated AD60 10% non-thermally treated AQ 6% - TiO 2 10% Primer coating Adhesion primer Magnetic stirrer Hyflon AD60 Solvay Specialty Polymers TFE-MDO copolymer High chemical stability [h] High UV transparency [i] High hydrophobicity [i] [h] W. Navarrini, M.V. Diamanti, M. Sansotera, F. Persico, M. Wu, L. Magagnin, S. Radice, Prog. Org. Coat. 74 (2012) 794. [i] F. Persico, M. Sansotera, M.V. Diamanti, L. Magagnin, F. Venturini, W. Navarrini, Thin Solid Films 545 (2013) 210.
![[h] High UV transparency [i] High hydrophobicity [i] [h] W. Navarrini, M.V. Diamanti, M. Sansotera, F. Persico, M. Wu, L. Magagnin, S.](/docs-images/45/4207243/images/page_10.jpg "Radice, Prog. Org. Coat. 74 (2012) 794. [i] F. Persico, M. Sansotera, M.V. Diamanti, L. Magagnin, F. Venturini, W.")
11 Photoactive Coating Low P UV Lamp Polluted aqueous solution O 2 Feed Quartz surface AD60 10% thermally treated AD60 10% non-thermally treated AQ 6% - TiO 2 10% Photoactive layer Magnetic stirrer Aquivion D83-06A Solvay Specialty Polymers TFE-SFVE copolymer High chemical stability [j] High UV transparency Strong acid behaviour [j] Hydrophilicity [j] W. Navarrini, et al., IT L ,
![stirrer Aquivion D83-06A Solvay Specialty Polymers TFE-SFVE copolymer High chemical stability [j]](/docs-images/45/4207243/images/page_11.jpg "High UV transparency Strong acid behaviour [j] Hydrophilicity [j] W. Navarrini, et al.")
12 Experimental apparatus Catalyst: TiO 2 Degussa P25 Nanometric TiO 2 (D p = nm) Anatase : Rutile = 3 : 1 Low P UV Lamp Polluted aqueous solution O 2 Feed Magnetic stirrer
13 Experimental apparatus Catalyst: TiO 2 Degussa P25 Nanometric TiO 2 (D p = nm) Anatase : Rutile = 3 : 1 Low P UV Lamp Polluted aqueous solution Tested organic pollutants: Rhodamine B-base (RhB) Non biodegradable organic dye C 28 H 30 N 2 O 3 - MW = g/mol λ max = 554 nm O 2 Feed Magnetic stirrer
14 Experimental apparatus Catalyst: TiO 2 Degussa P25 Nanometric TiO 2 (D p = nm) Anatase : Rutile = 3 : 1 Low P UV Lamp Polluted aqueous solution O 2 Feed Magnetic stirrer Tested organic pollutants: Rhodamine B-base (RhB) Non biodegradable organic dye C 28 H 30 N 2 O 3 - MW = g/mol λ max = 554 nm Crystal Violet (CRY) Photodegradation standard C 25 H 31 N 3 O - MW = g/mol λ max = 592 nm
15 Experimental apparatus Catalyst: TiO 2 Degussa P25 Nanometric TiO 2 (D p = nm) Anatase : Rutile = 3 : 1 Low P UV Lamp Polluted aqueous solution Tested organic pollutants: Rhodamine B-base (RhB) Non biodegradable organic dye C 28 H 30 N 2 O 3 - MW = g/mol λ max = 554 nm O 2 Feed Magnetic stirrer Crystal Violet (CRY) Photodegradation standard C 25 H 31 N 3 O - MW = g/mol λ max = 592 nm Analytical technique UV-Visible Spectrophotometry Lambert-Beer law: Abs = ε [pollutant] d
16 Experimental apparatus Low P UV Lamp Polluted aqueous solution O 2 Feed Quartz surface AD60 10% thermally treated AD60 10% non-thermally treated AQ 6% - TiO 2 10% Photoactive layer Magnetic stirrer O 2, hν Photoactive layer operating mode Organic Pollutant (R H ) R F -SO 3 -H/R H abs TiO 2 * R F -SO 3 H CO 2 + H 2 O + organic intermediates
17 Photodegradation - Rhodamine B-baseB Tested organic pollutant: Rhodamine B-base (RhB) - [RhB] 0 = mol/l O ested photocatalysts: Photoactive Coating (PC) - Clear solution Photoactive Coating (PC) - Turbid solution (CaSO 4, 8 g/l) TiO 2 slurry (dispersed TiO 2 = TiO 2 content in the coating) CH 3 N O N O CH 3 CH 3 CH 3
18 Photodegradation - Rhodamine B-baseB Tested organic pollutant: Rhodamine B-base (RhB) - [RhB] 0 = mol/l O ested photocatalysts: Photoactive Coating (PC) - Clear solution Photoactive Coating (PC) - Turbid solution (CaSO 4, 8 g/l) TiO 2 slurry (dispersed TiO 2 = TiO 2 content in the coating) CH 3 N O N O CH 3 CH 3 CH 3 C/C TiO2 slurry PC Turbid solution PC Clear solution Time (min) ln C 0 /C TiO2 slurry PC Turbid solution PC Clear solution Time (min)
19 Photodegradation - Rhodamine B-baseB Tested organic pollutant: Rhodamine B-base (RhB) - [RhB] 0 = mol/l ested photocatalysts: Photoactive Coating (PC) - Clear solution Photoactive Coating (PC) - Turbid solution (CaSO 4, 8 g/l) TiO 2 slurry (dispersed TiO 2 = TiO 2 content in the coating) ln C 0 /C C/C TiO2 slurry PC Turbid solution PC Clear solution Time (min) TiO2 slurry 0.8 PC Turbid solution 0.7 PC Clear solution Time (min) Pseudo-first order degradation kinetics C C 0 CH 3 N O N CH 3 = exp(-k app t) Test k app (min -1 ) a [RhB] 60 (%) b PC - Clear solution PC - Turbid solution TiO 2 slurry a Correlation coefficients R 2 higher than 0.99 for all the tests presented b RhB concentration decrease calculated after 60 min treatment O O CH 3 CH 3
20 Photodegradation - Crystal Violet Tested organic pollutant: Crystal Violet (CRY) - [CRY] 0 = mol/l ested photocatalysts: Photoactive Coating (PC) - Clear solution Photoactive Coating (PC) - Turbid solution (CaSO 4, 8 g/l) TiO 2 slurry (dispersed TiO 2 = TiO 2 content in the coating)
21 Photodegradation - Crystal Violet Tested organic pollutant: Crystal Violet (CRY) - [CRY] 0 = mol/l ested photocatalysts: Photoactive Coating (PC) - Clear solution Photoactive Coating (PC) - Turbid solution (CaSO 4, 8 g/l) TiO 2 slurry (dispersed TiO 2 = TiO 2 content in the coating) ln C 0 /C TiO2 slurry PC Turbid solution PC Clear solution ln C 0 /C TiO2 slurry PC Turbid solution PC Clear solution Time (min) Time (min)
22 Photodegradation - Crystal Violet Tested organic pollutant: Crystal Violet (CRY) - [CRY] 0 = mol/l ested photocatalysts: Photoactive Coating (PC) - Clear solution Photoactive Coating (PC) - Turbid solution (CaSO 4, 8 g/l) TiO 2 slurry (dispersed TiO 2 = TiO 2 content in the coating) TiO2 slurry PC Turbid solution PC Clear solution Pseudo-first order degradation kinetics ln C 0 /C ln C 0 /C Time (min) TiO2 slurry 0.8 PC Turbid solution 0.7 PC Clear solution Time (min) C C 0 = exp(-k app t) Test k app (min -1 ) a [CRY] 60 (%) b PC - Clear solution PC - Turbid solution TiO 2 slurry a Correlation coefficients R 2 higher than 0.99 for all the tests presented b CRY concentration decrease calculated after 60 min treatment
23 Photodegradation - RhB, CRY 1.0 Test Pollutant k app (min -1 ) PC - Clear solution RhB PC - Clear solution CRY PC - Turbid suspention RhB PC - Turbid suspention CRY C/C RhB absorption CRY absorption Time (min) Apparent independence of the k app values from the pollutant Pollutant absorption into the photoactive coating is the Rate Determining Step hν CB Organic compounds CO 2, H 2 O, N 2 CO Ti IV Ti OH IV 2, H 2 O, N 2 OH O {HO 2, HO 2-, H 2 O 2, OH - 2- } Organic compounds Ti IV OH + VB Ti III OH O 2 H 2 O
24 Photoactive coating characterization Profilometry Layer Average Thickness (μm) AQ 6% - TiO 2 10% 3.70 ± 0.44 Double AD60 10% 2.11 ± 0.19 Quartz surface Photoactive Coating 5.81 ± 0.63
25 Photoactive coating characterization Profilometry Layer Average Thickness (μm) AQ 6% - TiO 2 10% 3.70 ± 0.44 Double AD60 10% 2.11 ± 0.19 Quartz surface Photoactive Coating 5.81 ± 0.63 Scanning Electron Microscope - SEM
26 Photoactive coating characterization Profilometry Layer Average Thickness (μm) AQ 6% - TiO 2 10% 3.70 ± 0.44 Double AD60 10% 2.11 ± 0.19 Quartz surface Photoactive Coating 5.81 ± 0.63 Scanning Electron Microscope - SEM Atomic Force Microscopy - AFM Average Roughness, Sa = nm Root Mean Square, Sq = nm
27 Photoactive coating characterization Profilometry Layer Average Thickness (μm) AQ 6% - TiO 2 10% 3.70 ± 0.44 Double AD60 10% 2.11 ± 0.19 Quartz surface Photoactive Coating 5.81 ± 0.63 Scanning Electron Microscope - SEM Atomic Force Microscopy - AFM Average Roughness, Sa = nm Root Mean Square, Sq = nm Homogenous dispersion of TiO 2 in the photoactive layer Presence of TiO 2 clusters - Improvable system efficiency
28 Photoactive coating stability Thermogravimetric analysis - TGA 1 Delta Weight (-) 0,9 0,8 0,7 0,6 0,5 0,4 0,3 0,2 Pure Hyflon 0,1 AD60 Pure Aquivion D83-06A Temperature ( C) 1 0,9 Pure AD60 decomposition starts at 450 C Pure Aquivion decomposition starts at 300 C, together with cross-link phenomena that delay the complete degradation Photoactive Coating TGA curves before and after the use are overlapping Used Photoactive Coating appears to be unhaltered Delta Weight (-) 0,8 0,7 0,6 0,5 0,4 0,3 0,2 Pristine Photoactive Coating 0,1 Used Photoactive Coating Temperature ( C)
29 Achievements and Future Developments Achievements Future developments
30 Achievements and Future Developments Achievements The coating allows higher photoabatement rates than TiO 2 slurry Future developments
31 Achievements and Future Developments Achievements The coating allows higher photoabatement rates than TiO 2 slurry The coating can be employed to treat even turbid solutions Future developments
32 Achievements and Future Developments Achievements The coating allows higher photoabatement rates than TiO 2 slurry The coating can be employed to treat even turbid solutions The coating guarantees the abatement of different kinds of pollutants Future developments
33 Achievements and Future Developments Achievements The coating allows higher photoabatement rates than TiO 2 slurry The coating can be employed to treat even turbid solutions The coating guarantees the abatement of different kinds of pollutants Preliminary results show that the coating appears unhaltered after continuous use Future developments PLAST 2015, Federico Milano PersicoMay 6 th 2015
34 Achievements and Future Developments Achievements The coating allows higher photoabatement rates than TiO 2 slurry The coating can be employed to treat even turbid solutions The coating guarantees the abatement of different kinds of pollutants Preliminary results show that the coating appears unhaltered after continuous use Future developments Evaluation of the system efficiency towards different persistent pollutants (PFOA) PLAST 2015, Federico Milano PersicoMay 6 th 2015
35 Achievements and Future Developments Achievements The coating allows higher photoabatement rates than TiO 2 slurry The coating can be employed to treat even turbid solutions The coating guarantees the abatement of different kinds of pollutants Preliminary results show that the coating appears unhaltered after continuous use Future developments Evaluation of the system efficiency towards different persistent pollutants (PFOA) Evaluation of the system efficiency with different photocatalyst deposition (Sol-Gel) PLAST 2015, Federico Milano PersicoMay 6 th 2015
36 Achievements and Future Developments Achievements The coating allows higher photoabatement rates than TiO 2 slurry The coating can be employed to treat even turbid solutions The coating guarantees the abatement of different kinds of pollutants Preliminary results show that the coating appears unhaltered after continuous use Future developments Evaluation of the system efficiency towards different persistent pollutants (PFOA) Evaluation of the system efficiency with different photocatalyst deposition (Sol-Gel) Evaluation of the system efficiency working with different ph conditions
37 Achievements and Future Developments Achievements The coating allows higher photoabatement rates than TiO 2 slurry The coating can be employed to treat even turbid solutions The coating guarantees the abatement of different kinds of pollutants Preliminary results show that the coating appears unhaltered after continuous use Future developments Evaluation of the system efficiency towards different persistent pollutants (PFOA) Evaluation of the system efficiency with different photocatalyst deposition (Sol-Gel) Evaluation of the system efficiency working with different ph conditions Optimization of the ratio TiO 2 / ionomer into the coating
38 Achievements and Future Developments Achievements The coating allows higher photoabatement rates than TiO 2 slurry The coating can be employed to treat even turbid solutions The coating guarantees the abatement of different kinds of pollutants Preliminary results show that the coating appears unhaltered after continuous use Future developments Evaluation of the system efficiency towards different persistent pollutants (PFOA) Evaluation of the system efficiency with different photocatalyst deposition (Sol-Gel) Evaluation of the system efficiency working with different ph conditions Kinetic modelling of the system (Diffusion phenomena) Evaluation of this metodologie for the preparation useful organic compond
39 Acknowledgments Politecnico di Milano Dr. Ing. Francesco Venturini Dr. Ing. M. H. Wu Prof. L. Nobili (DLC) Prof. G. Dotelli Prof. L. Magagnin (AFM) Prof. A. Famulari (QMC) Prof. P. Gallo Stampino Dr. D. Picenoni (SEM) Mr. M. Ursini Solvay Solexis Dr. V. Tortelli Dr. M. Galimberti Dr. A. Sanguineti Dr. S. Radice (IR) Dr. E. Barchiesi (NMR) Dr. R. Pieri Ing. M. Apostolo Università degli Studi di Milano Prof. C.L.Bianchi Dr. S. Vitali Mr. A. Beretta 39
40 Thanks for your kind attention
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