2015 Fiscal Year Research-status Report
Development of Reactive Separation Technology Employing the Synergy of Sub/Supercritical H2O-CO2 System
Project/Area Number |
15K06559
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Research Institution | Kumamoto University |
Principal Investigator |
キタイン アルマンド 熊本大学, 自然科学研究科, 助教 (50504693)
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Project Period (FY) |
2015-04-01 – 2018-03-31
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Keywords | reactive separation / supercritical fluid / polyphenols / hydrolysis / hesperidin |
Outline of Annual Research Achievements |
The reaction process employing the synergy of subcritical H2O and supercritical CO2 was applied to hydrolysis of citrus bioflavonoids (hesperidin, HPD) into its aglycones (hesperetin, HPT). Using a batch reactor, we were successful in hydrolyzing HPD into HPT under hydrothermal conditions with supercritical CO2. The formation of intermediate product such as hesperetin-beta-glucoside could be minimized by reducing the amount of water.The highest yield of HPT of about 40.0 % was obtained at T=160 oC, P=15 MPa in 4 h. A semi-batch reactor system was also developed to study reaction and separation process employing the mixture of supercritical CO2 and subcritical H2O. Extraction of HPT was carried out by simply passing supercritical CO2 through the reaction products. Results confirmed the possibility of separating HPT from the mixture, and higher yield can be obtained by simply manipulating the pressure and temperature of CO2.Reaction kinetics was developed and parameters were also estimated. The solubilities of both HPD and HPT in supercritical CO2 were also investigated, and results confirmed HPT to have higher solubility than HPD.It was likely that the moisture content of CO2 also had an effect on solubility.International research collaboration with the group of Prof. Maria Jose Corcero of Valladolid University (Spain) on the solubility evaluation and minimization of the effect of transient time on reaction has also been started.
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Current Status of Research Progress |
Current Status of Research Progress
2: Research has progressed on the whole more than it was originally planned.
Reason
Overall, the research is progressing rather smoothly according to proposed schedule. However, the developed MATLAB program that calculates kinetic parameters needs revisions in some portion. A more systematic approach to solubility evaluation is also needed for a more accurate determination of the parameters required for subsequent modeling of the process.
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Strategy for Future Research Activity |
The solubility of HPD and HPT in supercritical CO2 will be evaluated using the dynamic approach. Several experiments will be conducted in order to come up with an accurate estimate of the commonly referred “Chrastil Solubility Model” parameters. The formulated reaction kinetics and solubility model parameters will then be used for computational analysis of the proposed reactive-separation method. Reactive-separation experiments will be carried out at the condition close to the optimum temperature, pressure and time determined previously. A combined reaction-separation model will be developed, while employing reaction kinetic and solubility parameters previously estimated. Other thermodynamic and physical properties of materials will be estimated using the commonly used equation of states. Model development and computational analysis based on the obtained laboratory-scale data are important for more rigorous and detailed scientific analysis and future commercialization of this proposed novel method. The reactive-separation technology that will be developed based on the hydrolysis of hesperidin will also be tested to other citrus flavanone glycosides, such as neohesperidin to produce hesperetin, naringin and narirutin to produce naringenin.Collaboration with leading international scientists in this field will also be pursued.
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Causes of Carryover |
This is an amount saved from purchasing discounted equipment (i. e. HPLC gradient system, PDA, and degasser).
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Expenditure Plan for Carryover Budget |
It is expected that more experimental runs will be carried out in the next fiscal year, thus this amount will be used for the purchase of consumables.
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Research Products
(3 results)