Progress 10/01/19 to 09/30/20
Outputs
Target Audience:The target audience(s) during the current reporting period was mainly the biofuel industrial companies and the interested governmental agencies such USDA and DOE through publishing our data international journals. Changes/Problems:
Nothing Reported
What opportunities for training and professional development has the project provided?The project has provided training and professional development to one graduate student. How have the results been disseminated to communities of interest?Results has been disseminated for publication in the high impact factor journal. What do you plan to do during the next reporting period to accomplish the goals?All final goals will be completed. Final results will be analyzed, and additional manuscripts will be written.
Impacts
What was accomplished under these goals?
In this study, 5-hydroxymethylfurfural (HMF) was converted into several biodiesel compounds such as 5-(alkoxymethyl)furans (AMFs) and 2,5-bis(alkoxymethyl)furans (BAMFs) through two-step sequential hydrogenation and etherification reactions. In the first step, zinc-iron magnetic nanocatalyst supported on activated carbon (ZnO-Fe3O4/AC) was prepared for the selective hydrogenation of HMF into furfuryl alcohols via Meerwein-Ponndorf-Verley (MPV) reaction in three different hydrogen donor alcohols (ethanol, 1-propanol, and 1-butanol). The important physical properties of the catalyst such as crystallinity, chemical composition, morphology, reduction behavior, and surface area were studied by using several analytical techniques. The effect of hydrogenation parameters such as catalyst concentration, temperature, and time on the selectivity of furfuryl alcohols and HMF conversion were studied. The best hydrogenation results were obtained with 0.2 mmole HMF and 100 mg of catalyst at 200 °C for 12h. In the second step, three commercial Brønsted acid catalysts including Amberlyst 16, Amberlyte IR120, and Dowex 50WX2 were used to convert the hydrogenated products into 5-(alkoxymethyl)furans (AMFs) and 2,5-bis(alkoxymethyl)furans (BAMFs). At the optimum etherification conditions (65°C and 10h), a spectrum of mono-, di-, and tri- ether compounds were obtained. At the end of the second step, 90% of ethoxymethyl, 86.6% of propoxymethyl, and 84% of butoxymethyl ether compounds were obtained with Amberlyst 16, Amberlyte IR120, and Dowex 50WX2 catalysts, respectively. Kinetic study was performed at three different temperatures (453.15, 463.15, and 473.15 K) to determine rate constants and activation energies of the hydrogenation reactions. The hydrogenation catalyst (ZnO-Fe3O4/AC) was recycled and used for five times without a remarkable reduction in its catalytic activity.
Publications
- Type:
Journal Articles
Status:
Published
Year Published:
2020
Citation:
Madduri, S., Elsayed, I., Hassan, E.B., 2020, Novel oxone treated hydrochar for the removal of Pb(II) and methylene blue (MB) dye from aqueous solutions.
- Type:
Theses/Dissertations
Status:
Published
Year Published:
2020
Citation:
Sunith Babu Madurri, 2020,Development of low-cost adsorbents from biomass residues for the removal of organic contaminants and heavy metals from aqueous solutions, Dissertation, Mississippi State University.
- Type:
Journal Articles
Status:
Published
Year Published:
2020
Citation:
Elsayed, I., Jackson, M.A., Hassan, E.B., Catalytic Hydrogenation and Etherification of 5-Hydroxymethylfufual into 2 (alkoxymathyl) 5 mothyfuran and 2,5 bis(alkoxymethyl)furan as potential biofuel additives, Fuel Processing Technology (in press) 2020 106672, https://doi.org/10.1016/j.fuproc.2020.106672
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Progress 10/01/18 to 09/30/19
Outputs
Target Audience:Our target audience(s) during the current reporting period was mainly the biofuel industrial companies and the interested governmental agencies such USDA and DOE through publishing our data international journals. Changes/Problems:
Nothing Reported
What opportunities for training and professional development has the project provided?One Ph.D. graduate student was trained in this project. How have the results been disseminated to communities of interest?Results has been disseminated for publication in the high impact factor journal, and presented in two international conferences. What do you plan to do during the next reporting period to accomplish the goals?We plan to develop another novel catalyst and to prepare high value oxygenated biodiesel additives of furan ethers (Furanics).
Impacts
What was accomplished under these goals?
2,5-bis(hydroxymethyl)furan (BHMF) is the major diol formed from 5-hydroxymethylfurfural (5-HMF) hydrogenation process. It has a significant importance in many applications including the production of resins, fibers, foams, drugs, polymers, ketones and ethers. Through this period, a magnetically recoverable cost-effective bimetallic nanocatalyst supported on activated carbon (CuO-Fe3O4/CC) was successfully synthesized for the selective transformation of 5-HMF into BHMF via Meerwein-Ponndorf-Verley (MPV) reaction using ethanol as a hydrogen donor with the absence of external molecular hydrogen. The prepared catalyst was characterized by XRD, H2-TPR, XPS, ICP-OES, HRTEM-EDX, and N2 adsorption-desorption isothermal analyses (BET and BJH). The effect of various reaction parameters affecting on the selectivity of BHMF and the conversion of HMF such as catalyst concentration, temperature, and time has been studied. The prepared catalyst exhibited a unique catalytic reactivity for the selective hydrogenation of 5-HMF to BHMF. About 33.3% of the active copper iron metals in the prepared catalysts exhibited high catalytic activity. At the optimum reaction conditions, 92.5% of BHMF selectivity and 97.5% conversion of 5-HMF using ethanol as the hydrogen donor with low percentages of byproduct compounds (DMF, 5-MFA and 5-MF) was achieved in ethanol over 1:1 (5-HMF/Catalyst ratio), at 150°C for 5 h. At the end of the hydrogenation reaction, a strong magnet was used to separate the catalyst from the reaction mixture and the catalyst was recycled and used five times without a remarkable decrease in its catalytic activity.
Publications
- Type:
Conference Papers and Presentations
Status:
Other
Year Published:
2019
Citation:
1- Hassan, E., El Sayed, I., Jackson, M. Hydrogen Free Catalytic Hydrogenation of biomass-derived 5-Hydroxymethylfurfural into 2,5-bis(hydroxymethyl)furan using Copper-iron/CC bimetallic catalyst. 73rd International Convention, Forest Products Society. Atlanta, GO. June 25-28, 2019.
- Type:
Conference Papers and Presentations
Status:
Other
Year Published:
2018
Citation:
2- Hassan, E., El Sayed, I., Jackson, M. Application of Fe3O4@SiO2-SO3H magnetic nanocatalyst for glucose dehydration to 5-Hydroxymethylfurfural. Thermal & Catalytic Sciences Symposium (TCS) Auburn University, AL. Oct. 8-10, 2018.
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Progress 10/01/17 to 09/30/18
Outputs
Target Audience:The target audience(s) during the current reporting period was mainly the biofuel industrial companies and the interested governmental agencies such USDA and DOE through publishing our data international journals. Changes/Problems:
Nothing Reported
What opportunities for training and professional development has the project provided?One Ph.D. graduate student has been trained in this project. How have the results been disseminated to communities of interest?Results has been disseminated through a journal article. Collaborative discussions with academic and government researchers have been ongoing. What do you plan to do during the next reporting period to accomplish the goals?We plan to develop a novel catalyst for the selective transformation of hydroxymethylfurfural 5-hydroxymethylfurfural (HMF) to 2,5-dihydroxymethylfuran (DHMF) and the high value oxygenated biodiesel additives of furan ethers (Furanics).
Impacts
What was accomplished under these goals?
A core-shell Fe3O4@SiO2-SO3H nanoparticle acid catalyst was successfully synthesized for dehydration of glucose to form HMF. The magnetically recoverable (Fe3O4@SiO2-SO3H) nanoparticle catalyst was successfully prepared by supporting sulfonic acid groups (SO3H) on the surface of silica-coated Fe3O4 nanoparticles. The prepared catalyst was characterized by FTIR, TGA, XRD, HRTEM-EDX, and N2 adsorption-desorption isothermal analyses. Dehydration of glucose was performed in a biphasic system made up of water and methylisobutylketone (water/MIBK), and the effect of various reaction parameters affecting on the yield of HMF such as biphasic system ratio, catalyst concentration, temperature, time, and dimethylsulfoxide (DMSO) ratio were studied. High HMF yield and glucose conversion were achieved by the application of (water/MIBK) biphasic system with Fe3O4@SiO2-SO3H as a catalyst. In this process, the addition of the catalyst and extracting phase (MIBK) increased the dehydration reaction efficiency of glucose and the HMF yield by limiting the HMF hydration side reaction and removing HMF from the reactive aqueous medium. The process variables, including catalyst concentration, reaction temperature and reaction time, had significant effects on glucose conversion and HMF yield. The optimum reaction conditions were found to be 40% catalyst concentration, 140°C, 24 h, and the use of a biphasic system (water: MIBK) ratio of 1:4. Under such conditions, a glucose conversion of 98% with a HMF yield of 70.5% was achieved. The usage of 40% catalyst is considered to be very low compared with the concentration of catalyst previously used to achieve comparable HMF yield. The effect of DMSO in suppressing hydration reactions and increasing the yield of HMF was not remarkable in this study due to the presence of a very strong Fe3O4@SiO2-SO3H catalyst.
Publications
- Type:
Journal Articles
Status:
Published
Year Published:
2018
Citation:
Elsayed, I., Mashaly, M., Eltaweel, F., Jackson, M.A., Hassan, E. Dehydration of glucose to 5-hydroxymethylfurfural by a core-shell Fe3O4@SiO2-SO3H magnetic nanoparticle catalyst. Fuel 221: 407-416: 2018.
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Progress 07/01/17 to 09/30/17
Outputs
Target Audience:Our target audience(s) during the current reporting period was mainly the biofuel industrial companies and the interested governmental agencies such USDA and DOE through publishing our data international journals. Changes/Problems:
Nothing Reported
What opportunities for training and professional development has the project provided?One Ph.D. graduate student has been trained in this project. How have the results been disseminated to communities of interest?
Nothing Reported
What do you plan to do during the next reporting period to accomplish the goals?We plan to use this catalyst for the conversion of glucose to hydroxymethylfurfural (HMF) and optimize the various reaction conditions affecting on the yield of HMF such as biphasic system ratio, catalyst concentration, temperature and time.
Impacts
What was accomplished under these goals?
All the required chemicals were ordered, catalyst has been prepared and characterized by FTIR, TGA, XRD, TEM and SEM analysis.
Publications
- Type:
Other
Status:
Other
Year Published:
2017
Citation:
{Nothing to report}
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