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Removing Water from an Azeotropic Ethanol-Water Mixture Through Adsorption

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Removing Water from an Azeotropic Ethanol-Water Mixture Through Adsorption 2015 Removing Water from an Azeotropic Ethanol-Water Mixture through Adsorption A Major Qualifying Project Proposal Submitted to: William Clark, David DiBiasio, and Stephen Kmiotek Mackenzie Alameda, Kathryn Bumila, Ivette Carino, and Gabrielle McIninch This report represents the work of WPI undergraduate students submitted to the faculty as evidence of completion of a degree requirement. WPI routinely publishes these reports on its website without editorial or peer review. For more information about the projects program at WPI, please see http://www.wpi.edu/academics/ugradstudies/project-learning.html Abstract Adsorption was explored as a mechanism to further separate azeotropic ethanol-water mixtures to produce pure ethanol for biofuel use. A bench-scale adsorption column was designed and tested. The variables in the experiment were the type of adsorbent, the amount of adsorbent, and the flow rate. The results showed that using 60 grams of Zeolite 3A at 5mL/minute produced optimal adsorption. An adsorption experiment was designed for the Unit Operations II Laboratory at Worcester Polytechnic Institute. 1 Acknowledgements This team received great support and advice throughout this project and would like to acknowledge the following people for their contributions. Project Advisor, Professor Stephen Kmiotek Project Advisor, Professor William Clark Project Advisor, Professor David DiBiasio Unit Operations Lab Manager and Machine Shop Staff Member, Tom Partington Professor Robert Thompson 2 Table of Contents Abstract ........................................................................................................................................... 1 Acknowledgements ......................................................................................................................... 2 Table of Contents ............................................................................................................................ 3 Table of Figures .............................................................................................................................. 5 Problem Statement .......................................................................................................................... 6 Background ..................................................................................................................................... 8 Concept of Adsorption ................................................................................................................ 8 Desorption ................................................................................................................................... 8 Basic Equations for Adsorption ................................................................................................ 10 Adsorption Forces ..................................................................................................................... 10 Adsorption Rate in Porous Adsorbents ..................................................................................... 10 Adsorption Equilibrium ............................................................................................................ 11 Adsorption Isotherms ................................................................................................................ 11 Adsorbents ................................................................................................................................ 15 Activated Carbons ................................................................................................................. 16 Activated Alumina ................................................................................................................ 16 Silica Gel ............................................................................................................................... 16 Zeolite ................................................................................................................................... 17 Organic Material ................................................................................................................... 19 Adsorption Systems .................................................................................................................. 19 Azeotropic Ethanol-Water Mixture .......................................................................................... 20 Methodology ................................................................................................................................. 22 Objective 1 ................................................................................................................................ 22 Column Design specifications .............................................................................................. 22 Experiment Design................................................................................................................ 23 Method for Measuring Ethanol Concentration ..................................................................... 24 Preliminary Testing ............................................................................................................... 25 Objective 2 ................................................................................................................................ 27 Objective 3 ................................................................................................................................ 28 Results and Discussion ................................................................................................................. 30 Error .............................................................................................................................................. 37 3 Air Bubbles ............................................................................................................................... 37 Packing Geometry ..................................................................................................................... 37 Sealing....................................................................................................................................... 38 Timing of Samples .................................................................................................................... 38 Different Starting Solutions ...................................................................................................... 38 Evaporation ............................................................................................................................... 39 Conclusions and Recommendations ............................................................................................. 40 Deliverables .................................................................................................................................. 42 Unit Operations II Experiment.................................................................................................. 42 References ..................................................................................................................................... 47 Appendix ....................................................................................................................................... 49 Appendix A: Double Interpolation of Alcohol Tables ............................................................. 49 Appendix B: Data Tables .......................................................................................................... 50 Zeolite 4A data Tables .......................................................................................................... 50 Zeolite 3A Data Tables ......................................................................................................... 58 Rice Data Tables ................................................................................................................... 66 4 Table of Figures Figure 1 shows the types of adsorption based on isotherm properties. ........................................ 12 Figure 2 illustrates isotherm graphs demonstrating the different types of adsorption by plotting amount adsorbed vs. vapor pressure. The red represents the adsorption and the green represent desorption. ..................................................................................................................................... 12 Figure 3 is a graph of ethanol-water distillation, demonstrating azeotrope which occurs at 95.6% mass ethanol. ................................................................................................................................. 21 Figure 4 is a diagram of the final column design.......................................................................... 23 Figure 5 shows the experimental set up. ....................................................................................... 24 Figure 6 is an example of an alcohol table used to determine ethanol concentrations. ................ 26 Figure 7 is a graph depicting the density meter testing results. .................................................... 27 Figure 8 shows the results of the Zeolite 3A experiments at five milliliters per minute. The independent variable among the three experiments was the amount of adsorbent, which ranged from twenty, forty, and sixty grams. ............................................................................................. 32 Figure 9 is a plot of the results of the Zeolite
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