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Transcript of Maretva Baricot Mendoza Supervisor Dr. Josep Font Capafons Chemical Reaction Engineering and Process...
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Maretva Baricot Mendoza
Supervisor Dr. Josep Font Capafons
Chemical Reaction Engineering and Process Intensification Group, Department of Chemical Engineering, Universitat Rovira i Virgili
Tarragona, February 3rd 2005
Experimental design for the functionalization of activated carbon as catalyst in Catalytic wet air oxidation of
phenol
CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Content
1. Introduction
2. State of the art
3. Objectives
4. Methodology
5. Expected Results
6. Future work
2/13
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Introduction
Environmental problem
AdsorptionMembranes
Filtration UltrafiltrationReverse osmosis
ChemicalOxidation
Biological
Treatments
3/13
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Introduction
Activated Carbon
Adsorption, catalyst support but lately…..
As catalyst itself!!!
What is it ?
Growing interest!!!
4/13
Carbonaceous materials, highly crystalline formExtensively developed internal pore structure
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
State of the Art
Characterization of carbon surfaceChemical titrations Temperature programmed desorptionsInfrared and X-ray photoelectron spectroscopy
Most common functional groups
PhenolicsCarbonylsCarboxylsQuinonesLactonesAnhydrides
5/13
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
State of the Art
Carboxylic acid
Lactone
Phenol
Carbonyl
Anhydride
Ether
Quinone
OOH
H
O
CO
OH
O
C O
OH
O
O
O
C
C
O
O
O
6/13
Functional groups
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
State of the Art
Baçaoui et alEnviron. Sci. & Technol, 2002.
36(17): p. 3844-3849
Herbicides
Pereira et alAppl. Catal., A, 1999.
184(1): p. 153-160 Activated carbon as catalyst in the oxidative dehydrogenation of ethylbenzene
Modified AC
7/13
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
State of the Art
CREPI
Phenol oxidation in a Trickle bed reactor (TBR)@ 160ºC and Oxygen partial pressure 0,82 MPa(1)
Conversion up to 99 %
Commercial activated carbon
as Catalyst
8/13
(1) J. Chem. Technol. Biotechnol., 2001. 76(7): p. 743-751
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Objectives
Design an experimental procedure to functionalize activated carbon in order to
obtain a good surface chemistry that improves the catalytic activity of carbon in
the TBR.
Main
Secondary
Superficial functional groupsCarbon textureDefunctionalization-Refunctionalization process
9/13
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Methodology
DefunctionalizationHeat treatment under Inert atmosphere
Elimination of surface functional groups
Temperatures ranges
RefunctionalizationHeat treatment under Oxygen and Nitrogen
atmosphere
Formation of specific surface functional groupsVarying T, PO2 and time
Carbon treatment
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Methodology
From Refunctionalization Stage
MAC tests
Adsorption tests
Catalytic activity tests
Batch configuration
TBR, Milder conditions
Set of Modified Activated Carbon MAC
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Methodology
From the set of MAC those that shows better performance as catalyst and adsorptive material…
MAC characterization
Chemical titrationsTGA + TPDInfrared Spectroscopy
Thermogravimetric analysis + Thermal programmed desorptions
12/13
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Expected Results
1. Clarification of the influence of the surface chemistry on the AC catalytic performance
2. Determination of better surface chemistry on activated carbon for it to show catalytic activity
3. Obtaining a better catalyst for phenol oxidation than commercial AC
4. Procedure to design tailor made AC active for CWAO, from any source
13/13
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Future work
1. Develop an experimental procedure combining oxidizing treatments and characterization techniques to obtain catalyst useful in oxidation of several compounds as halogenated phenols
2. Improve adsorptive performance of AC with chemical surface modification
3. Establish experimental procedures to specifically functionalize AC surface in order to improve its behavior as catalyst, support or adsorptive material
14/13
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CCCHHHEEEMMMIIICCCAAALLL RRREEEAAACCCTTTIIIOOONNN EEENNNGGGIIINNNEEEEEERRRIIINNNGGG &&&PPPRRROOOCCCEEESSSSSS IIINNNTTTEEENNNSSSIIIFFFIIICCCAAATTTIIIOOONNN GGGRRROOOUUUPPP
Questions
Thanks for your attention!!!
Questions ????