Pilot Scale Production, Characterization, and Optimization of Epoxidized Vegetable Oil-Based Resin
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Abstract
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.