{"id":63,"date":"2021-03-17T17:09:12","date_gmt":"2021-03-17T21:09:12","guid":{"rendered":"https:\/\/seniordesign.digitalscholar.rochester.edu\/che2021\/?p=63"},"modified":"2022-04-13T11:39:49","modified_gmt":"2022-04-13T15:39:49","slug":"dementors","status":"publish","type":"post","link":"https:\/\/www.hajim.rochester.edu\/senior-design-day\/dementors\/","title":{"rendered":"Packed Bed Reactors for Academic Experimentation"},"content":{"rendered":"\n
\"\"
Figure 1. A picture of Team Dementors next to the built setup. From left to right: Emilio, Ahmad, Thien, and Clive. <\/figcaption><\/figure><\/div>\n\n\n\n

Introduction<\/h2>\n\n\n\n

Project Name:<\/strong> Packed Bed Reactors for Academic Experimentation<\/p>\n\n\n\n

Authors: <\/strong>Ahmad El Gazzar, Thien Hung Nguyen, Clive Onyango, Emilio Vega-Ramos<\/em>.<\/p>\n\n\n\n

Project Sponsor<\/strong>: Professor Marc Porosoff.<\/a><\/em><\/p>\n\n\n\n

\"\"
Professor Marc Porosoff, the Project Sponsor, is an Assistant Professor in the Chemical Engineering Department at the University of Rochester.<\/figcaption><\/figure><\/div>\n\n\n\n

Campus Mentors: <\/strong>Professor F. Doug Kelley, Jeffery Lefler, and Clair Cunningham. <\/em><\/p>\n\n\n\n

Customers: <\/strong>ChE 246 Principal Investigator and ChE Undergraduate Students. <\/em><\/p>\n\n\n\n

\n
Project Motivation<\/summary>
\n
  • \"\"<\/figure><\/li>
  • \"\"<\/figure><\/li><\/ul>
    Figure 2. Currently available reactor systems. Continuously-stirred tank reactors (left) and tubular reactors (right). <\/figcaption><\/figure>\n\n\n\n

    <\/p>\n\n\n\n

    Currently, undergraduate Chemical Engineering students have access to homogeneous reactor systems shown in Figure 2. There is a need to incorporate packed-bed systems with gaseous phase reactants for a more enriched laboratory experience. A system containing four stainless steel reactors has been proposed to allow for the exploration of effects of pressure, temperature, catalyst weight, and flow rates on the performance metrics of the reverse-water gas shift reaction (RWGS) shown in Equation 1.<\/p>\n\n\n\n

    CO2<\/sub> + H2<\/sub> \u21cc<\/strong> CO + H2<\/sub>O (Equation 1)<\/p>\n<\/div><\/details><\/div>\n<\/div>\n\n\n\n

    Table 1. Website directory.<\/p>\n\n\n\n

    Page <\/strong><\/td>Content<\/strong><\/td><\/tr>
    1<\/td>Introduction<\/td><\/tr>
    2<\/a><\/td>Project Background<\/td><\/tr>
    3<\/a><\/td>Technical Approach<\/td><\/tr>
    4<\/a><\/td>Results<\/td><\/tr>
    5<\/a><\/td>Conclusions and Future Work<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

    <\/p>\n\n\n\n\n\n\n\n

    Project Background<\/h2>\n\n\n\n
    \n
    <\/div>\n<\/div>\n\n\n\n

    Sponsor (Professor Marc Porosoff) Requirements<\/h4>\n\n\n\n

    A safe<\/strong>, reproducible<\/strong>, and intuitive <\/strong>systems with the following features: <\/p>\n\n\n\n

    • Multi-channel design to allow for testing of 3-5 catalyst loadings in a single experiment.<\/li>
    • Reliable heating mechanism, allowing for isothermal conditions within reactors.<\/li>
    • Ability to monitor pressure within reactors.<\/li>
    • Ability to control reactants’ flow rates.<\/li>
    • In-line gas chromatograph (GC) for seamless products analysis. <\/li><\/ul>\n\n\n\n
      \"\"
      Figure 3. The process flow diagram (PFD) provided initially by the Project Sponsor. <\/figcaption><\/figure><\/div>\n\n\n\n

      Stakeholder Considerations<\/h4>\n\n\n\n
      \"\"
      Figure 4. Design considerations from key stakeholders.<\/figcaption><\/figure><\/div>\n\n\n\n\n\n\n\n

      Technical Approach<\/h2>\n\n\n\n

      With the process flow diagram (PFD) provided by the Project Sponsor and stakeholder considerations shown on Page 2, the team developed a block flow diagram (BFD) to approach the problem. <\/p>\n\n\n\n

      \"\"
      Figure 5. A simple block flow diagram (BFD) of the developed system. The main components include a tube furnace for heating, GC for product analysis, and a computer for data analysis. <\/figcaption><\/figure><\/div>\n\n\n\n

      A more detailed version of our approach is shown in Figure 6. Go to Page 4 to see how this drawing ended up in real life! <\/p>\n\n\n\n

      \"\"
      Figure 6. Final process flow diagram (PFD) developed by Team Dementors. This shows all the components that were included in the build process. <\/figcaption><\/figure><\/div>\n\n\n\n

      In the following section, some components of the systems will be discussed along with the team’s technical approach to each component. <\/p>\n\n\n\n

      Gas Chromatograph<\/h4>\n\n\n\n

      A big task that Team Dementors took on was the repair of an old GOW-MAC gas chromatograph (GC). The major component that was burnt out in the GC was the thermal conductivity detector (TCD) that is essential in the process to identify the reaction products. The following gallery shows some of the steps included in the repair process. <\/p>\n\n\n\n

      \"\"
      Figure 7. GOW-MAC GC with the front panel open for repair and TCD filaments replacement. <\/figcaption><\/figure><\/div>\n\n\n\n
      \"\"
      Figure 8. The newly purchased TCD filaments after installation in the GOW-MAC TCD cell. <\/figcaption><\/figure><\/div>\n\n\n\n
      \"\"
      Figure 9. The column oven of the GOW-MAC GC. The column on the left was created and packed by Team Dementors. <\/figcaption><\/figure><\/div>\n\n\n\n

      The following flowchart shows the steps taken to repair the GC. <\/p>\n\n\n\n

      \"\"
      Figure 10. A flowchart illustrating the steps taken to repair the GOW-MAC GC. <\/figcaption><\/figure><\/div>\n\n\n\n

      Reactors Scaffold<\/h4>\n\n\n\n

      In order to offer rigid support to the reactors inside the tube furnace, the team designed several versions of a reactors scaffold. Figure 11 shows the progression of the scaffold as well as the implementation. <\/p>\n\n\n\n

      \"\"
      Figure 11. The process of creating a reactors scaffold. The final design was selected, as it offers easy replacement to the reactors without having to deal with the large reactor end caps. <\/figcaption><\/figure><\/div>\n\n\n\n

      Insulation<\/h4>\n\n\n\n

      Thermal insulation was added downstream of the reactors. It is composed of mineral wool to reduce heat loss by conduction and aluminum foil to reduce heat loss by convection and radiation. The insulation has two roles: <\/p>\n\n\n\n

      • Prevent exposed tubing from reaching high temperatures.<\/li>
      • Keep product water in the gaseous phase until it is removed by the drying bed.<\/li><\/ul>\n\n\n\n
        \"\"
        Figure 12. Insulation downstream of reactors. It is composed of mineral wool and aluminum foil.<\/figcaption><\/figure><\/div>\n\n\n\n

        Drying Tube<\/h4>\n\n\n\n

        A desiccant bed was included to ensure liquid water does not enter the GC. The bed consists of Drierite (CaSO4<\/sub>), an indicating agent that is blue when unsaturated and pink when at capacity.<\/p>\n\n\n\n

        The team tested several drying tube options. The final choice shown in Figure 13 was selected for its transparency and high-pressure tolerance. <\/p>\n\n\n\n

        • \"\"<\/figure><\/li>
        • \"\"<\/figure><\/li><\/ul>
          Figure 13. Drying tube packed with Drierite indicating agent.<\/figcaption><\/figure>\n\n\n\n\n\n\n\n

          Results<\/h2>\n\n\n\n

          Final Prototype<\/h4>\n\n\n\n

          The final prototype of our approach is shown in Figure 14. <\/p>\n\n\n\n

          \"\"
          Figure 14. The final setup of the reactors system. The main components are labeled on the figure. <\/figcaption><\/figure><\/div>\n\n\n\n

          Testing the GC<\/h4>\n\n\n\n

          After going through the process of repairing the GC and given the importance of an in-line GC, as desired by the Project Sponsor, it was essential to test the GC. The reactant gases were analyzed using the GOW-MAC GC. The three different peaks indicate the presence of three distinct gases, as expected.<\/p>\n\n\n\n

          \"\"
          Figure 15. The GOW-MAC GC output using LabVIEW. The chromatogram is for a 60% Ar, 30% H2<\/sub>, and 10% CO2<\/sub> mixture. A 2 mL sample loop was used for this injection. The carrier gas is He with a flow rate of 18 mL\/min. The stationary phase is Porapak Type Q 80-100 Mesh. A 4-feet column was used with its temperature set at 30 \u00b0<\/strong>C. <\/figcaption><\/figure><\/div>\n\n\n\n

          The chromatogram results from the GOW-MAC GC were confirmed by using discrete injections into a Buck-Scientific GC. The chromatogram from the Buck-Scientific GC is shown in Figure 16. <\/p>\n\n\n\n

          \"\"
          Figure 16. The Buck-Scientific GC output. The chromatogram is for a 60% Ar, 30% H2<\/sub>, and 10% CO2<\/sub> mixture. A 6 mL discrete injection was analyzed. The carrier gas is He with a flow rate of 21.8 mL\/min. The stationary phase is Porapak Type Q 80-100 Mesh. A 4-feet column was used with its temperature set at 80 \u00b0<\/strong>C. The three observed peaks agree with those detected by the GOW-MAC GC. <\/figcaption><\/figure><\/div>\n\n\n\n

          To put this together, a reactor was loaded with a P-K-Mo2<\/sub>C catalyst and run for 2 hours. However, due to the large amount of time needed to obtain products with this catalyst, no products were observed in the span of two hours. The results are shown in Figure 17. <\/p>\n\n\n\n

          \"\"
          Figure 17. P-K-Mo2<\/sub>C was used as a catalyst loading (left). The initial chromatogram (middle) matches that of the reactants gases. After 120 mins on stream (right), no new peaks were observed. <\/figcaption><\/figure><\/div>\n\n\n\n

          Due to the oxophilic<\/strong> nature<\/strong> <\/strong>of the transition metal carbides (P-K-Mo2<\/sub>C), no products were formed after 120 mins on stream. Juneau et al.[1]<\/sup> collected data after reduction for 2 hours at 300 psi and 300 \u00b0C and after exposure to stream for 7-12 hrs.<\/p>\n\n\n\n\n\n\n\n

          Conclusions<\/h2>\n\n\n\n

          Team Dementors was able to develop a safe, reproducible, and intuitive packed-bed reactors system that is bound to enrich the undergraduate ChE Laboratory experience at the University of Rochester. The system consists of gas manifolds that connect to four reactors, a tube furnace that offers uniform heating of the reactors, a drying tube downstream of the reactors to extract product water, and a GOW-MAC GC, which was repaired by Team Dementors, for product analysis. The developed system offers undergraduate students the tools necessary to investigate heterogeneous reactions, allowing them to generate results similar to the ones shown in Figure 18.<\/p>\n\n\n\n

          \"\"
          Figure 18. RWGS reaction data was extracted from the work done by Juneau et al.[1]<\/sup> and processed in Minitab to offer a context on how the built setup would benefit undergraduate ChE students. <\/figcaption><\/figure><\/div>\n\n\n\n

          Future Work<\/h2>\n\n\n\n
          • Replace needle valves with ball valves<\/strong> at reactors entrance\/exits.<\/li>
          • Adapt a drying bed <\/strong>with higher operating pressures <\/strong>or install heating tape <\/strong>downstream of reactors.<\/li>
          • Install flow meters<\/strong> with high operating pressures <\/strong>upstream of the reactors.<\/strong><\/li>
          • Use a heating block <\/strong>rather than a tube furnace for departmental needs.<\/li>
          • Use catalysts<\/strong> that require minimal preparation <\/strong>time.<\/li>
          • Install a sliding door <\/strong>to inhibit the students from accidentally touching hot tubing.<\/li><\/ul>\n\n\n\n

            Acknowledgments<\/h2>\n\n\n\n

            We would like to thank the Project Sponsor, Professor Marc Porosoff<\/strong>, for his invaluable feedback and flexibility throughout the semester. The team expresses its special thanks to the ChE 255 instructors’ team for their availability, support, and feedback. Thanks to Professor Melodie Lawton<\/strong> and Professor Fred Kelley <\/strong>for their regular feedback and for helping us steer the project in the right direction at several points in the semester. Thanks to Rachel Monfredo<\/strong> for all her help, especially with creating the columns and replacing the TCD filaments for the GOW-MAC GC. Thanks to Clair Cunningham <\/strong>for his help with the amplifier circuit that allowed us to obtain a signal out of the GOW-MAC GC. Special thanks to Jeffrey Lefler<\/strong> for his help with sourcing many of the materials needed for this build project.<\/p>\n\n\n\n

            References<\/h2>\n\n\n\n[1] Juneau, M., Vonglis, M., Hartvigsen, J., Frost, L., Bayerl, D., Dixit, M., . . . Porosoff, M. D. (2020). Assessing the viability of K-MO2C for reverse water\u2013gas shift Scale-up: Molecular to laboratory to pilot scale. Energy & Environmental Science,<\/em> 13<\/em>(8), 2524-2539. doi:10.1039\/d0ee01457e<\/p>\n\n\n\n

            <\/p>\n","protected":false},"excerpt":{"rendered":"

            This project aims to design and build a multi-channel reverse water gas shift reactor system that allows for exploration of heterogeneous catalysis.
            \nAhmad El Gazzar, Thien Hung Nguyen, Clive Onyango, Emilio Vega-Ramos<\/p>\n","protected":false},"author":6242,"featured_media":41932,"comment_status":"open","ping_status":"open","sticky":false,"template":"templates\/template-full-width.php","format":"standard","meta":{"_coblocks_attr":"","_coblocks_dimensions":"","_coblocks_responsive_height":"","_coblocks_accordion_ie_support":"","_monsterinsights_skip_tracking":false,"_monsterinsights_sitenote_active":false,"_monsterinsights_sitenote_note":"","_monsterinsights_sitenote_category":0,"footnotes":""},"categories":[4442,76,3046,3076,3086],"tags":[5462,5472,5482,5492,5502,5512,5522,5532],"coauthors":[8612],"class_list":["post-63","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-archive","category-che-archive","category-manufacturing-archive","category-material-science-archive","category-process-engineering-archive","tag-catalysis","tag-catalytic-reactors","tag-chemical-kinetics","tag-gas-chromatography","tag-heterogenous-catalysis","tag-reactor","tag-reactor-design","tag-reverse-water-gas-shift-reactor"],"acf":[],"yoast_head":"\nPacked Bed Reactors for Academic Experimentation - Senior Design Day<\/title>\n<meta name=\"robots\" content=\"index, follow, max-snippet:-1, max-image-preview:large, max-video-preview:-1\" \/>\n<link rel=\"canonical\" href=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/dementors\/\" \/>\n<link rel=\"next\" href=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/dementors\/2\/\" \/>\n<meta property=\"og:locale\" content=\"en_US\" \/>\n<meta property=\"og:type\" content=\"article\" \/>\n<meta property=\"og:title\" content=\"Packed Bed Reactors for Academic Experimentation - Senior Design Day\" \/>\n<meta property=\"og:description\" content=\"This project aims to design and build a multi-channel reverse water gas shift reactor system that allows for exploration of heterogeneous catalysis. 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