college of engineering chemical, biological, and ......college of engineering chemical, biological,...

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Chemical, Biological, and Environmental Engineering COLLEGE OF ENGINEERING REFERENCES: Ikhazuangbe, P. M., & Oni, A. B. (2015). Reaction rate and rate constant of the hydrolysis of ethyl acetate with sodium hydroxide. American Journal of Scientific and Industrial Research, 1-4. Kitson, P. J., Marie, G., Francoia, J., Zalesskiy, S. S., Sigerson, R. C., Mathieson, J. S., & Cronin, L. (2018). Digitization of multistep organic synthesis in reactionware for on-demand pharmaceuticals. Science,359(6373), 314-319. OVERALL CHEMICAL PROCESS FLOW DIAGRAM WHAT IS A CSTR? A CSTR is a Continuous Stirred Tank Reactor CSTRs are commonly used in industry as they convert reactants to useful chemicals in an uninterrupted process. An “ideal” CSTR is well mixed and has a uniform concentration within the reactor. Smaller CSTRs behave less ideally. 3D PRINTING OF SMALL-SCALE STIRRED TANK REACTOR MIXING STUDY Figure 6. Pulse test: 1 mL of red food coloring is injected into the 0.75 L CSTR and the absorbance of effluent samples are taken over time. Reactants Products MOTIVATION The goal of this project is to design a 3D printed system that can be customized for any desired reaction on a smaller scale (to minimize waste). Kitson et al. designed a series of reactors with the goal of making highly specialized chemicals/pharmaceuticals. MATERIALS COMPATIBILITY Ethyl acetate known to dissolve many polymers. Compatibility charts show several polymers are resistant, however only a few are printable Nylon filament resistant to pure ethyl acetate, ABS shows resistance to 0.1 M ethyl acetate which allows for cheaper printing. ACKNOWLEDGEMENTS: Dr. Skip Rochefort for guidance and lab space/equipment. Conor Harris for 3D printing assistance. Andy Brickman for providing DAQ equipment and pump setup. John Cochran for providing access to lab equipment. Plural Inc. for providing nylon filament, printing profiles. Dr. Phil Harding for guidance and design suggestions. C 4 H 8 O 2 + NaOH → C 2 H 3 NaO 2 + C 2 H 5 OH Figure 7. Step test: 0.026 M NaCl solution starts at initial time at 0.1 L/min while DI water is fed through at 0.1 L/min. Conductivity is being measured with time. 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 0 20 40 60 80 100 120 140 Conversion Volumetric Flow Rate (mL/min) Volume = 1.5 L Volume = 0.75 L Volume = 0.50 L Volume = 0.25 L Figure 2. Predictions of conversions for different size CSTRs for the saponification of ethyl acetate. Side View Top View Angle View 3D MODEL OF REACTOR 3D MODEL OF PROPOSED SYSTEM Figure 3. A process flow diagram of the experimental system to be 3D printed. Quick connects allow three different volumes of reactors (0.75, 0.5 and 0.25 L) to be easily switched out. Side View Top View Angle View Figure 5. The SolidWorks design of the CSTR. Barbed fittings allow for quick replacement. A L/D ratio of 1 was held constant for all designs. Barbed fittings for inlet and outlet streams allow for easy replacement. Figure 4. The SolidWorks design for the experimental system to be 3D printed with dimensions of 17.8” x 7.6” x 14”. The stir plate and products reservoir have been integrated into the bottom of the design. Figure 8. ABS, Taulman 3D Bridge Nylon, and 3DXTech Nylon filaments after 1 hour of exposure to 0.1 M and pure ethyl acetate. Kaylee Duchateau, Bryce Beattie, Kendra Connell How well will the smaller reactors mix? How well will the smaller reactors respond to changes? Figure 1. The 3D printed system used to make specialized pharmaceuticals [Kitson, et al.]. Centrifugal Pump FI Centrifugal Pump FI 0.1 M Ethyl Acetate (1 L) 0.1 M Sodium Hydroxide (1 L) Rotameter (20-100 mL/min) 3D printed CSTR ABS (0.75 L) Magnetic Stir Plate Magnetic Stir Bar Products Reservoir LabQuest DAQ LoggerPro Software (Laptop) 3D printed CSTR ABS (0.25 L) 3D printed CSTR ABS (0.50 L) Rotameter (20-100 mL/min) Vernier Conductivity Probe (0-20,000 μS/cm) Typical chemical processes consist of feed sources, pumps to move fluid, and instrumentation to monitor flow/concentration. REACTION OF INTEREST Saponification of ethyl acetate Kinetic data for this reaction is readily available, and is also used for CHE 415 lab (along with many universities around the US). CBEE_11

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Page 1: COLLEGE OF ENGINEERING Chemical, Biological, and ......COLLEGE OF ENGINEERING Chemical, Biological, and Environmental Engineering REFERENCES: • Ikhazuangbe, P. M., & Oni, A. B. (2015)

C h e m i c a l , B i o l o g i c a l , a n d E n v i r o n m e n t a l E n g i n e e r i n gC O L L E G E O F E N G I N E E R I N G

REFERENCES:

• Ikhazuangbe, P. M., & Oni, A. B. (2015). Reaction rate and rate

constant of the hydrolysis of ethyl acetate with sodium hydroxide.

American Journal of Scientific and Industrial Research, 1-4.

• Kitson, P. J., Marie, G., Francoia, J., Zalesskiy, S. S., Sigerson, R. C.,

Mathieson, J. S., & Cronin, L. (2018). Digitization of multistep organic

synthesis in reactionware for on-demand

pharmaceuticals. Science,359(6373), 314-319.

OVERALL CHEMICAL PROCESS FLOW DIAGRAM

WHAT IS A CSTR?• A CSTR is a Continuous Stirred Tank Reactor

• CSTRs are commonly used in industry as they convert reactants to useful chemicals in an uninterrupted process.

• An “ideal” CSTR is well mixed and has a uniform concentration within the reactor. Smaller CSTRs behave less ideally.

3D PRINTING OF SMALL-SCALE STIRRED TANK REACTOR

MIXING STUDY

Figure 6. Pulse test: 1 mL of red food coloring is

injected into the 0.75 L CSTR and the absorbance of

effluent samples are taken over time.

Reactants

Products

MOTIVATION• The goal of this project is to design a 3D printed

system that can be customized for any desired reaction on a smaller scale (to minimize waste).

• Kitson et al. designed a series of reactors with the goal of making highly specialized chemicals/pharmaceuticals.

MATERIALS COMPATIBILITY

• Ethyl acetate known to dissolve many polymers. Compatibility charts show several polymers are resistant, however only a few are printable

• Nylon filament resistant to pure ethyl acetate, ABS shows resistance to 0.1 M ethyl acetate which allows for cheaper printing.

ACKNOWLEDGEMENTS:

• Dr. Skip Rochefort for guidance and lab space/equipment.

• Conor Harris for 3D printing assistance.

• Andy Brickman for providing DAQ equipment and pump setup.

• John Cochran for providing access to lab equipment.

• Plural Inc. for providing nylon filament, printing profiles.

• Dr. Phil Harding for guidance and design suggestions.

C4H8O2 + NaOH → C2H3NaO2 + C2H5OH

Figure 7. Step test: 0.026 M NaCl solution starts at

initial time at 0.1 L/min while DI water is fed through at 0.1 L/min. Conductivity is being measured with time.

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

0 20 40 60 80 100 120 140

Con

ve

rsio

n

Volumetric Flow Rate (mL/min)

Volume = 1.5 L

Volume = 0.75 L

Volume = 0.50 L

Volume = 0.25 L

Figure 2. Predictions of conversions for different size CSTRs for the saponification of ethyl acetate.

Side View Top View Angle View

3D MODEL OF REACTOR

3D MODEL OF PROPOSED SYSTEM

Figure 3. A process flow diagram of the experimental system to be 3D printed. Quick connects allow three different volumes of reactors (0.75, 0.5 and 0.25 L) to be easily switched out.

Side View Top View Angle View

Figure 5. The SolidWorks design of the CSTR. Barbed fittings allow for quick replacement. A L/D ratio of 1 was held constant for all designs. Barbed fittings for inlet and outlet streams allow for easy replacement.

Figure 4. The SolidWorks design for the experimental system to be 3D printed with dimensions of 17.8” x 7.6” x 14”. The stir plate and products reservoir have been integrated into the bottom of the design.

Figure 8. ABS, Taulman 3D Bridge Nylon, and 3DXTech Nylon filaments after 1 hour of exposure to 0.1 M and pure ethyl acetate.

Kaylee Duchateau, Bryce Beattie, Kendra Connell

How well will the smaller reactors mix?

How well will the smaller reactors respond to changes?

Figure 1. The 3D printed system used to make specialized pharmaceuticals [Kitson, et al.].

Centrifugal Pump

FI

Centrifugal Pump

FI

0.1 M Ethyl Acetate(1 L)

0.1 M Sodium Hydroxide

(1 L)

Rotameter(20-100 mL/min)

3D printed CSTRABS

(0.75 L)

Magnetic Stir Plate

Magnetic Stir Bar

Products Reservoir

LabQuestDAQ

LoggerPro Software(Laptop)

3D printed CSTRABS

(0.25 L)

3D printed CSTRABS

(0.50 L)

Rotameter(20-100 mL/min)

Vernier Conductivity Probe

(0-20,000 µS/cm)

Typical chemical processes consist of feed sources, pumps to move fluid, and instrumentation to monitor flow/concentration.

REACTION OF INTEREST• Saponification of ethyl acetate

• Kinetic data for this reaction is readily available, and is also used for CHE 415 lab (along with many universities around the US).

CBEE_11