Design and operation of microchemical systems for multistep chemical syntheses

This thesis focused on advancing the microchemical field from single device based demonstrations to systems that can perform multi-step series and parallel synthesis. Few examples of micro-separators and micro-pumps suited for miniaturized lab-on-a-chip systems for organic syntheses exist, so the first half of this thesis developed systems for these micro-unit-operations, while the second half demonstrated multistep microchemical operations enabled by these systems. In-line continuous separation devices are developed that enabled removal of unreacted reagents/byproducts, making it possible to realize a series of reactions without leaving the microreactor environment. Differences in surface forces and preferential wettability characteristics of fluoropolymers are used for phase separation. Such microseparators are used to demonstrate 100% separation of two phase flows of hexane and water, toluene and water, dichloromethane and water, and hexane and methanol. Integrated liquid-liquid extraction devices are microfabricated that performed two -phase contacting by segmented flow, followed by separation - resulting in single stage extraction. Single stage extraction of N,N-dimethylformamide from dichloromethane to water, and from diethyl ether to water is demonstrated. The development of separators allows microreactors to be connected to microseparators to form microreactor networks enabling reactions and separations in succession. The starting reagents are loaded in syringes and syringe pumps push fluid through the train of microdevices. However, this pumping scheme is limited by pressure constraints at the pump drives as well as the microseparators. Therefore, there is a need to develop in-line pumps to sustain the microdevice network. Pressure-driven flow is employed for the operation of micropumps. An enclosure with the liquid is pressurized with helium gas, causing the liquid to flow. The dynamics of pressurizing and de-pressurizing an enclosure are modeled and confirmed by experiments. Active and passive control schemes to provide constant flowrate of the liquid are developed and implemented. Different schemes are developed to use the gas pressure to manipulate the flow path of liquids.

Department dc:contributor.department

Massachusetts Institute of Technology. Dept. of Chemical Engineering.

Grantor dc:publisher

Massachusetts Institute of Technology

Year dc:date.issued

2008

Author dc:creator

• Sahoo, Hemantkumar

Advisor dc:contributor.advisor

• Klavs F. Jensen.

• Chemical Engineering.

Statement dc:rights

• M.I.T. theses are protected by copyright. They may be viewed from this source for any purpose, but reproduction or distribution in any format is prohibited without written permission. See provided URL for inquiries about permission.

Licence dc:rights.uri

• http://dspace.mit.edu/handle/1721.1/7582

Language dc:language.iso

eng

Handle dc:identifier.uri

http://hdl.handle.net/1721.1/45923

OAI identifier oai:identifier

oai:dspace.mit.edu:1721.1/45923