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ESTERIFICATION USING SULFONATED HYDROTHERMAL CARBON CATALYST IN A CONTINUOUS-FLOW MODE

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title
ESTERIFICATION USING SULFONATED HYDROTHERMAL CARBON CATALYST IN A CONTINUOUS-FLOW MODE
author
FRALEY Jr, NORMAN Eugene
abstract
ABSTRACTThis work is the continuation of prior work in developing and using sulfonated hydrothermal carbon (SHTC) as a heterogeneous catalyst for the esterification of waste grease into advanced biofuels. The work was advanced by transitioning from stirred tank reactor (STR) to a continuous-flow reactor (CFR). We hypothesized that SHTC used in continuous flow mode would provide additional benefits over traditional batch reaction for the conversion of oleic acid (OA) and methanol (MeOH) into the methyl oleate ester (FAME). The CFR was built to precisely control temperature, flow rate, and reactant blending composition. The result was a system that allowed us to perform the esterification at temperatures higher than boiling methanol, a practical upper limit for the batch reaction process. CFR operational performance was investigated to characterize the reaction space for the system by examining reactor residence time, the molar ratio of reactants, and the presence of water at various operating temperatures. To assist in CFR operation, we discovered and verified the use of conductivity detection as a tool to monitor leachate evolution and demonstrated linear response to the sulfur concentration of the SHTC. The leachate from the solid catalyst was highly reactive in the esterification reaction. The reactive nanoparticulate colloidal suspension was isolated, characterized, and determined to be SHTC from 20 nm to 200 nm in size. SHTC can be effectively used in a continuous flow manner, providing conversions >90% at MeOH:OA molar ratios > 12:1 in 11 minutes of residence time when using dry methanol at 100 ºC.
subject
Biofuels
continuous-flow
esterification
packed-bed
solid acid catalysis
sulfonated hydrothermal carbon
contributor
Lachgar, Abdessadek (committee chair)
Meiburg, Albert (committee member)
Dos Santos, Patricia C. (committee member)
King, Bruce (committee member)
Wright, Marcus W (committee member)
date
2022-05-24T08:36:10Z (accessioned)
2022 (issued)
degree
Chemistry (discipline)
embargo
2027-06-01 (terms)
2027-06-01 (liftdate)
identifier
http://hdl.handle.net/10339/100762 (uri)
language
en (iso)
publisher
Wake Forest University
type
Dissertation

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