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Date of Award
2015
Publisher
North Dakota State University
Document Type
Dissertation
Degree Awarded
Doctor of Philosophy (PhD)
Program
Agricultural and Biosystems Engineering
Department
Agricultural and Biosystems Engineering
College
Graduate and Interdisciplinary Studies
Faculty Advisor
Wiesenborn, Dennis P.
Description
Novel epoxidized sucrose soyate (ESS) resins perform much better than other vegetable oil-based resins; thus, they are of current interest for commercial scale production and for a wide range of applications in coatings and polymeric materials. However, no work has been published that successfully scaled-up the reaction above a 1 kg batch size. To achieve this goal, canola oil was first epoxidized at a 300 g scale to study the epoxidation rate and thermal profile at different hydrogen peroxide (H2O2) addition rates, bath temperatures, and reaction times. At least 83% conversion of double bonds to oxirane was achieved by 2.5 h, and the reaction temperature was 8-15 oC higher than the water bath temperature within the first 30-40 min of epoxidation. A 38 L stainless steel kettle was modified as a reactor to produce 10 kg of ESS. Twenty 7-10 kg batches of ESS were produced with an overall 87.5% resin yield and > 98% conversion after batch three. The conversion and resin quality were consistent across the batches due to the modifications on the reaction that improved mixing and reaction temperature control within 55-65 oC. The total production time was reduced from 8 to 4 days due to the fabrication of a 40 L separatory funnel for both washing and filtration. A math model was developed to optimize the epoxidation process. This was done by using the Box-Behnken design to model the conversion at various acetic acid, H2O2, and Amberlite ratios and at various reaction temperatures and times. The model had an adjusted R2 of 97.6% and predicted R2 of 96.8%. The model showed that reagent amounts and time can be reduced by 18% without compromising the desired conversion value and quality.
Recommended Citation
Monono, Ewumbua Menyoli, "Pilot Scale Production, Characterization, and Optimization of Epoxidized Vegetable Oil-Based Resin" (2015). Agribusiness and Biosystems Engineering. 43.
https://digitalcommons.ndsu.edu/agribusiness-biosystems-engi/43
Rights
NDSU policy 190.6.2
Rights Link
https://www.ndsu.edu/fileadmin/policy/190.pdf
Handle Identifier
http://hdl.handle.net/10365/24873