Goran Jovanovic Oregon State University School of Chemical, Biological, and Environmental Engineering

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1 Microreactor Technologies for Production of Advanced Liquid Biofuels Goran Jovanovic Oregon State University School of Chemical, Biological, and Environmental Engineering Sweet Spot of Microtechnology In Affiliation With: MBI Microproducts Breakthrough Institute ONAMI Oregon Nanoscience And Microtechnologies Institute

2 Microtechnology The study, development, and application of devices whose operation is based on the scale of microns. (A human hair is approximately 100 microns thick. Image source:

3 Nature s Microtechnology Nature has selected the micro scale for the realization of many biological processes. Leaf Alveoli Kidney

4 What is Microtechnology Good For? Production of information lab-on-chip Production of services pacemaker kidney dialyzer Production of energy and bulk material chemicals fuel upgrade biofuels nanoparticles

5 Microreactors for Biodiesel Production Microreactors for Production H2O2 Microreactor for Desulphurization of Fuels Microseparators for Liquid-Liquid Extraction Microreactors for Production of Veins and Arteries Microscale-Based Blood Oxygenation Microreactor for Destruction of Toxic Waste Microtechnology-Based Water Desalination Microsensor for Detection of Human Pathogens in Food and Water Microtechnology-Based Hydrogen Storage Microtechnology-Based Gas-to-Liquid FT Process 5

6 Hydrogenation of bio-oils H2 H2 H2 H2 H2 H2

7 Transesterification of bio-oils CH3OH CH3OH CH3OH k1 k3 k2 Glycerol TG DG MG k 1 k 3 k 2 Biodiesel Biodiesel Biodiesel

8 Micro-Scale Reactors First MECS micro-reactor, OSU 1999

9 Microreactors Plate Gasket Flow separator Quartz window Teflon spacer

10 Microreactors

11 Experimental Setup Stock solution of methanol with dissolved NaOH in 10 ml syringe ON/OFF Syringe Pump Microreactor Soybean Oil in 60 ml syringe Biodiesel Phase Glycerol Phase

12 Various Views - Biodiesel Microreactor Biodiesel Heating Fluid Methanol Crude Oil Glycerol

13 Single Stage Biodiesel Microreactor Oil Inlet Manifold Reaction Channels Oil/Glycerol Phase Separation Chamber Methanol Inlets Glycerol Outlet Oil/Biodiesel Phase Outlet to Second Stage

14 Two Stage Biodiesel Microreactor Second Stage First Stage Oil Inlet Second Stage Product Glycerol Stream Heating Fluid Inlet/Outlet Second Stage Product Biodiesel Outlet Second Stage Methanol Inlet First State Methanol Inlet Biodiesel Heating Fluid First Stage Methanol Crude Oil Glycerol First Stage Product Glycerol Stream

15 Exploded View - Biodiesel Microreactor Second Stage Methanol Inlet/Manifold Heating Fluid Inlet/Outlet Second Stage Second Stage Product Biodiesel Outlet Second Stage Product Glycerol Outlet Second Stage Oil Phase Manifold First Stage Oil Phase Outlet First Stage Second Stage Reaction Channels Second State Separation Chamber First State Separation Chamber First Stage Product Glycerol Outlet Fluid Driven Thermal Plate First Stage Reaction Channels First Stage Methanol Inlet/Manifold Biodiesel Oil Inlet/Manifold Heating Fluid Methanol Crude Oil Glycerol

16 Micro-Reactor Design The plate is 267mm X 187mm in size and made from 0.5mm thick (316) stainless steel. The overall channel length is 16,740mm Major design consideration was to preserve the gas-liquid segmented flow in the microchannels. The solution chosen was to implement a single, long microchannel on a horizontal plane that wraps back and forth on a single plate (It could be used as a device with multiple, parallel channels).

17 d1 d2 Catalyst Reactant-H2 Phase 1 Reaction Reactant TG and intermediates 1 dn TG Rate: Sc dt = k C H 2 CTG at wall d4 d3 at wall mol m2 s cat

18 Fluid input hole Hole for clamp bolt Alignment hole (for bonding) Catalyst deposition hole

19 Installed Micro-Reactor Assembly Thermal Input tube insulation Output tube

20 Hydrothermal Treatment of Plate Microreactor in Heated Enclosure

21 Ci CTGo Triglycerides Diglycerides Fatty Acids Monoglycerides Alkanes Residence Time [min]

22 Integrated and Parallel processing 2m Groups of Laminae create one Block-Stage 1m

23 Advantages of Microtechnology Advantages arising from Fundamental Phenomena; Advantages arising from Parallel Architecture; Advantages arising from Commercial Applications; Advantages in the area of Safety and Security.

24 Fundamental Advantages of Microtechnology Intensification of Heat and Mass Transport - Small scale - Short time of mass and heat transport (τ =l2/d) Reduced Size times reduction in hardware volume over conventional technology; times reduction in hardware mass; - Shifts size-energy trade-offs toward higher efficiency; - Able to integrate heat exchanges with reactors and separators simplifying processes. Large surface to volume ratio ( m2/m3) Changes chemical product distribution

25 Fundamental Advantages of Microtechnology Low Pressure Drop Reduces power for pumps, fans, and blowers; Gravity independence Gravity effect diminish to surface and hydrodynamics forces as size of channels decreases; High Degree of Reaction Control Minimizing unwanted environmental and side reactions; Minimize unwanted reversible reactions; Enables processing of very energetic reactants; Intensification of chemical kinetics (the last frontier in mass transport) Extremely High Quench Rates Small reactant volumes mean less mass or energy required to quench; Extremely rapid heat transport enables fast thermal discharge.

26 Advantages of Microtechnology-Parallel Architecture Fast screening of materials, catalyst and processes Flexibility in capacity and in design - Provides for deployment at wide range of scales; - Facilitates gradual expansion of capacity as scale of operations grows by adding more modules; Operating robustness and controllability - Enhances reliability, allowing problems to be isolated and repaired. Mass Production of Microscale Components - Microlamination process enables mass production; - Bonded stacks can contain multiple processes; - Multiple processes in a single device reduces field assembly and testing.

27 Commercial Advantages of Microtechnology Lower capital investment; Lower operating cost; Faster transfer of research to commercial production; Earlier start of production at lower cost - Reduces life-cycle costs through early testing at implementation scale; Easier scale up (numbering -up) to production capacity; Distributed technology implementation (distributed production); Integration of micro-technologies with other systems; Lower cost of transportation of material and energy; Replacing batch with continuous processes.

28 Safety and Security Advantages Small channel inhibits flame/explosion front propagation; Small volumes translate to low energy content stored; Smaller volume less hazardous materials in the process.

29 Sweet Spot of Microtechnology Large surface to volume ratio Flexibility in capacity and design Sweet Spot Distributed production Integration with other systems

30 People. Ideas. Innovation. Thank you for your attention!

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