Preparation and Characterization of Catalysts
Code
11052
Academic unit
Faculdade de Ciências e Tecnologia
Department
Departamento de Química
Credits
6.0
Teacher in charge
Isabel Maria de Figueiredo Ligeiro da Fonseca
Weekly hours
5
Total hours
104
Teaching language
Português
Objectives
The students learn how to select the catalytic species for a specific catalytic process and how to prepare massic or impregnated catalysts. In order to understand the activity , selectivity and catalyst deactivation, they also learn how to characterize them using physical and chemical techiques.
Prerequisites
None
Subject matter
Lectures
1. Importance of Industrial catalysis
1.1. Introduction
1.2 Definitions
1. 3. Concepts and heterogeneous catalysis theories
1. 4. Adsorption
1.5. Catalytic activity of metals
1..6. Catalytic activity of semi conductors
1.7. Catalytic activity of stoichiometric oxides
2. Catalysts properties
2.1. Selectivity
2.2. Activity
2.3. Statabity and regenerability
2.4. Mechanical and thermal properties
3. Selection of active species
3.1. Selection of criterious
3.2. Transformation analysis
3.3. Selection of catalaytic species.
.3.3.1. Empirical classifications
3.3 .2 General laws of catalysis and scientific correlations
3.3.3 Bibliography research
3.3.4 Experimental exploration
4. Catalysts preparation
4.1. Massic catalysts and supports
4.1.1. Fused catalysts
4.1.2. Raney-Ni catalysts
4.1.3. Metallic glasses
4.1.4. Precipitation and co precipitation
4.1.5. Sol gel method
4.2. Supported catalysts
4.2.1. Supports impregnation
4.2.2. Thermal treatments
5. Zeolites
5.1. Synthesis
5.2. Caracterization
5.3. Shape selectivity
6. Physical and chemical characterization of catalysts
6.1. Chemical composition of catalysts
6.2. Nature and structure of chemical compounds
6.3. Textural properties
6.3.1. Adsorption isotherms
6.3.2. Isotherm of Brunauer-Emmett-Teller (BET)
6.3.3. Calculation of surface area
6.3.4. Calculation of pore volume, porosity and solid density
6.3.5. Pore size distribution
6.3.6. Porosimetry of mercury
6.3.7. Metallic phase characterization.
6.3.8. Temperature program reduction.
6.3.9. Temperature program desorption
6.4. Acidity of solid catalysts
6.4.1. Methods of titration
6.4.2. Infrared spectroscopy
6.4.3. Base adsorption followed by infrared spectroscopy.Temperature programmed desorption
6.4.4. Chemical reaction models
7. Catalysts deactivation
7.1. Solid phase change
7.2. Poisoning
7.3. Fouling
8.Zeolites application.Catalytic cracking
9.Catalysts apllication in industrial processes
2. Laboratory classes
2.1Preparation of bulk catalysts by precipitation
2.2. Ionic exchange of a zeolite NaY
2.3. Preparation and optimization of a carbon xerogel
2.4. Textural characterization of a silica -alumina and an activated carbon
2.5. Characterization by X Ray diffraction of bulk catalysts and catalysts supported on activates carbon
2.6 Catalysts caracterization by TEMand SEM (MCM-41,SBA-15;Pt/AC)
Visit to a portuguese Refinary(GALP, Sines)
3. Solving problems sessions
3.1. Catalysts characterization solving problems
3.2. Discussion and treatment of the experimental data obtained in the lab classes(reports elaboration)
Bibliography
3. Catalyse de Contact, J.F. Le Page, J. Cosyns, P. Courty, E. Freund, J.P. Montarnal, A. Sugier, H. van Landeghem, Éditions Technip,1978
5.Characterization of Heterogeneous Catalysts , F. Delannay, Ed. Marcel Dekker,1984, ISBN 0-8247-7100-1
6. Catalyst Characterization, physical techniques for solid materials, Boris Imelik and Jacques C. Vedrine. Plenum Publish Corporation, 1992,ISBN 0-306-43950-6
7. Zeólitos um nanomundo ao serviço da catálise, Michel Guisnet, Fernando Ramoa Ribeiro, ed. Fundação Calouste Gulbenkian, 2004. ISBN 972-31-1071-7
Teaching method
The lectures are given using tranparencies or data show. Most of the problems solving sessions require computer ( EXCEL).The experiments are carried out in group ( 2-3students) in the laboratory . The experimental results obtained in the lab will provide the data that will be treated and analysed during the problems solving classes
Evaluation method
In order to go to exam, the students need to attend all the laboratory classes and all the solving problems classes . Using the experimental data obtained in the laboratory some problems are solved and discussed in the classes and a report need to be presented . The students will continuosly evaluated by 2 mini tests and a seminar.
The final grade is 80% of the tests grade +20% seminar.
The minimum grade to be suceed is 9 for first test .