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Catalytic Decomposition of Nitric Oxide and Carbon Monoxide Gases Using CATALYTIC DECOMPOSITION OF NITRIC OXIDE AND CARBON MONOXIDE GASES USING NANOFIBER BASED FILTER MEDIA OF VARYING DIAMETERS A Thesis Presented to The Graduate Faculty of The University of Akron In Partial Fulfillment of the Requirements for the Degree Master of Science Renee L. Petty August 2010 CATALYTIC DECOMPOSITION OF NITRIC OXIDE AND CARBON MONOXIDE GASES USING NANOFIBER BASED FILTER MEDIA OF VARYING DIAMETERS Renee L. Petty Thesis Approved: Accepted: _________________________ _________________________ Advisor Department Chair Dr. George G. Chase Dr. Lu-Kwang Ju _________________________ _________________________ Committee Member Dean of the College Dr. Edward A. Evans Dr. George K. Haritos _________________________ _________________________ Committee Member Dean of the Graduate School Dr. Bi-Min Zhang Newby Dr. George R. Newkome _________________________ Date ii ABSTRACT Nitrogen Oxide (NO) and carbon monoxide (CO) are major pollutants in the exhaust streams of automobiles, power plants, and other combustion processes. The growing concerns for the environment have resulted in increasingly restrictive emission standards. The removal of NO and CO from exhaust gases is a challenging task. One method for harmful gas removal is using a catalyst for dissociation. This work explored an alternative method for catalytic reduction of NO. Polymer solutions with palladium catalyst and ceramic precursors were electrospun to form polymer nanofibers. These nanofibers were heated to form ceramic nanofibers with catalyst nanoparticles and were mixed with microfibers to form a nonwoven fibrous catalyst support structure. The concentration of the polymer was varied to create nanofibers with diameters ranging from 100 to 700 nm with a constant mass of catalyst particles per mass of fiber. The effect of the fiber diameter on the corresponding catalyst structure performance was tested. A surface area comparison test was completed to determine whether the reactions occur strictly on the surface of the catalyst or if diffusion occurs. An aging comparison was also completed which tested 1 week old catalytic filters compared to 6 months old. A conventional catalytic converter was iii tested to verify the performance was similar to the catalytic fibrous filter media containing only palladium. Experiments were carried out using a lab reactor to expose the media to a mixture of gases simulating an exhaust stream at room temperature to a maximum of 450oC. The reactor exhaust concentrations are measured using gas chromatography (GC) to determine the catalyst performance. Results indicated that the catalytic reaction performance was about the same for fiber sizes ranging from 100 to 700 nm on a mass basis with a reduction temperature of 325 – 350oC. The surface area comparison filter reduced at 275oC which showed that both surface catalyst particles and particles within the fibers are available for reaction. Furthermore, a conventional catalytic converter reduced at approximately 325oC which exhibits comparable catalytic performance with the catalytic filters. Model theory and equations were also developed for decomposition reactions of NO and CO using elementary reactions. iv ACKNOWLEDGEMENTS I would like to thank Dr. George Chase for all of his support during this research. I learned so much both personally and academically from him and I will use those skills in my future. I would also like to thank Mempro Ceramics Corporation for providing the materials and equipment to conduct this research. I would also like to sincerely thank Sneha Swaminathan for continuous support and knowledge about the project as well as project set-up and organization. I would like to thank my fiancé, Michael Coe, for his help with this Thesis and for his unconditional love and support while I was finishing my education. I would also like to thank my good friend Linda Kuhajda for her help with this Thesis. I am also thankful for the whole multiphase group for making my education a wonderful experience. I would also like to give a special thanks to Mr. Frank Pelc and Gabriel Manzo for their help throughout my research. I would like to thank Dr. Edward Evans and Dr. Bi-Min Newby for being on my committee and giving me valuable input and helping with my Thesis. v TABLE OF CONTENTS Page LIST OF TABLES…………………………………………………………….……………………………………………....x LIST OF FIGURES…………………………………………………………….……..……………………………………..xi CHAPTER I. INTRODUCTION……………………………………………………………………………………………………..…..1 1.1 Background and overview of work………………………………………...……………………….….1 1.2 Problem statement………………………………………………………….….……………………………..4 1.3 Objectives…………………………………………………………………...….....................................5 1.4 Hypothesis……………………………………………………………………………………………………….…5 1.5 Thesis outline…………………………………………………………...……………………………………..…6 II. LITERATURE REVIEW…………………………………………………………….......................................8 2.1 Introduction……………………………………...…………………………………………………………..…..8 2.2 Formation of nitrogen oxide in combustion processes…….……………………………….10 2.3 Current available technology and mechanisms for NOx reduction……….…………..11 2.4 Conventional catalytic converter……………………………………….……………………………..16 2.5 Deactivation of catalysts…………………………………………………………………………………..20 vi 2.6 Benefit and technological importance of the catalytic filter with nanofibers…….21 2.7 Introduction to electrospinning…………………………………….…………..........................23 2.8 Technology for the high production of nanofibers and applications……...…………25 III. DESIGN OF EXPERIMENT…………………………………………...…………...................................32 3.1 Experimental set-up for electrospinning……………………………………………………………32 3.2 Calcining Polymer nanofibers……………………………………………………………………………35 3.3 Vacuum mold set-up for making filter medium…………………………………………………36 3.4 Flowing hydrogen reduction apparatus……………………………………………...…………….38 3.5 Catalytic reaction experimental set-up….………….………………………………………………40 3.6 Instruments…………………………..…………………………………….…...................................43 IV. SYNTHESIS OF PALLADIUM SUPPORTED ON CERAMIC NANOFIBERS AND MAKING FILTER MEDIA...……………………………………………...………………………………………………………45 4.1 Palladium nanoparticles supported by alumina nanofibers synthesized by electrospinning……………….…………………………………………..……………………………………45 4.2 Ceramic fibrous filter media incorporated with electrospun nanofibers……………51 V. REACTION OF NITRIC OXIDE AND CARBON MONOXIDE USING FILTER MEDIA..……….56 5.1 Introduction…………………………………………………………………………………………………….56 5.2 Reactions on 100 nm nanofibers with palladium catalyst……………………….…………63 5.3 Reactions on 250 nm nanofibers with palladium catalyst……………………….…………69 5.4 Reactions on 300 nm nanofibers with palladium catalyst……………………….…………73 5.5 Reactions on 350 nm nanofibers with palladium catalyst……………………….…………77 vii 5.6 Reactions on 700 nm nanofibers with palladium catalyst……………………….…………81 5.7 Reactions on 700 nm nanofibers with same surface area as 100 nm fibers………85 5.8 Reactions on 100 nm nanofibers for aging analysis…………………………………………..91 5.9 Reactions with catalytic converter…………………………………………………………………….98 5.10 Discussion and Conclusions…………………………………………………………………………..101 VI. CONCLUSIONS AND FUTURE WORK…………………..…………………………………………………107 6.1 Conclusions……………..……………………………………………………………………………………..107 6.2 Recommended future work………………………………………..………………………………….110 REFERENCES…………………………………………………….…………...……………………………………………112 APPENDICIES……………………………………………………………………………………………………………...115 APPENDIX A. ADDITIONAL INFORMATION ON THE SYNTHESIS AND CHARACTERIZATION OF CERAMIC NANOFIBERS….…...…………………………………………………………….116 APPENDIX B. FLOWING HYDROGEN REDUCTION APPARATUS OPERATING PROCEDURE…...........................................................................................120 APPENDIX C. GC OPERATING PROCEDURE……………………………………………………………….122 APPENDIX D. GC CALIBRATION…………………………………………………………………………………124 APPENDIX E. CATALYTIC FILTER RAW DATA OBTAINED FROM GC…………………………….133 APPENDIX F. ERROR ANALYSIS………………………………………………......................................158 APPENDIX G. EQUIPMENT TROUBLESHOOTING………………………………………………………161 APPENDIX H. CATALYTIC FILTER IDENTIFICATION TABLE………………………………………….164 APPENDIX I. ELEMENTARY REACTION MODEL FOR NITRIC OXIDE AND CARBON MONOXIDE REACTIONS……………………………………………………………………....166 viii I.1 Introduction………………………………………………………………….………………………………..166 I.2 Basis for Assumptions..........................................................................................169 I.3 Development of model equations………………..…………………….…....…………………….182 APPENDIX J. CHARACTERIZATION OF CATALYTIC CONVERTER.......................................204 ix LIST OF TABLES Table Page 2.1 Summary of EPA current vehicle emission standards (PM is particulate matter)…………………………………………………………………………………………………………….9 2.2 Typical emissions from gasoline and diesel engines………………………………………..11 2.3 Proposed mechanisms for NO and CO reactions on palladium catalyst..............13 4.1 Slurry ingredients to make catalytic filter.............................................................52 5.1 Proposed elementary reaction mechanism with detailed kinetic data on Pt (1 1 1)...............................................................................................................58 5.2 Test conditions for the 100 nm nanofibers with palladium catalyst....................63 5.3 Test conditions for the 250 nm nanofibers with palladium catalyst....................70 5.4 Test conditions for the 300 nm nanofibers with palladium catalyst....................74 5.5 Test conditions for the 350 nm nanofibers with palladium catalyst....................78
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