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Keywords = HMF (5-hydroxymethyl furfural)

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24 pages, 3140 KiB  
Article
Physicochemical and Sensory Evaluation of Romanian Monofloral Honeys from Different Supply Chains
by Elena Daniela Bratosin, Delia Mirela Tit, Manuela Bianca Pasca, Anamaria Lavinia Purza, Gabriela Bungau, Ruxandra Cristina Marin, Andrei Flavius Radu and Daniela Gitea
Foods 2025, 14(13), 2372; https://doi.org/10.3390/foods14132372 - 4 Jul 2025
Viewed by 407
Abstract
Honey quality and authenticity are influenced by floral origin, processing, and storage, with implications for composition and sensory appeal. This study offers a comparative assessment of eight monofloral honey samples, representing five botanical varieties: acacia, linden, rapeseed, lavender, and thyme. For acacia, linden, [...] Read more.
Honey quality and authenticity are influenced by floral origin, processing, and storage, with implications for composition and sensory appeal. This study offers a comparative assessment of eight monofloral honey samples, representing five botanical varieties: acacia, linden, rapeseed, lavender, and thyme. For acacia, linden, and rapeseed, both producer-sourced and commercial honeys were analyzed, while lavender and thyme samples were available only from local beekeepers. The botanical origin of each sample was confirmed using morphological markers of pollen grains. Physicochemical characterization included acidity, pH, moisture content, refractive index, hydroxymethyl furfural (HMF), proline concentration, and carbohydrate profiling by HPLC-RID. Acacia honey exhibited the lowest acidity and HMF levels, alongside the highest fructose/glucose (F/G) ratios, indicating superior freshness, lower crystallization risk, and a sweeter flavor profile. In contrast, rapeseed honey showed elevated glucose levels and the lowest F/G ratio, confirming its tendency to crystallize rapidly. All samples recorded proline concentrations well above the quality threshold (180 mg/kg), supporting their authenticity and proper maturation. The estimated glycemic index (eGI) varied between 43.91 and 62.68 and was strongly inversely correlated with the F/G ratio (r = −0.98, p < 0.001). Sensory evaluation highlighted acacia honey from producers as the most appreciated across visual, tactile, and flavor attributes. Correlation analyses further revealed consistent links between sugar composition and both physical and sensory properties. Overall, the findings reinforce the value of integrated analytical and sensory profiling in assessing honey quality and authenticity. Full article
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17 pages, 3998 KiB  
Article
Contributions of Oxide Support Reducibility for Selective Oxidation of 5-Hydroxymethylfurfural over Ag-Based Catalysts
by Haichen Lai, Gaolei Shi, Liuwei Shen and Xingguang Zhang
Catalysts 2025, 15(3), 248; https://doi.org/10.3390/catal15030248 - 5 Mar 2025
Cited by 1 | Viewed by 880
Abstract
As a type of sustainable and renewable natural source, biomass-derived 5-hydroxymethyl furfural (HMF) can be converted into high-value chemicals. This study investigated the interactions between silver (Ag) and oxide supports with varied reducibility and their contributions to tuning catalytic performance in the selective [...] Read more.
As a type of sustainable and renewable natural source, biomass-derived 5-hydroxymethyl furfural (HMF) can be converted into high-value chemicals. This study investigated the interactions between silver (Ag) and oxide supports with varied reducibility and their contributions to tuning catalytic performance in the selective oxidation of HMF. Three representatives of manganese dioxide (MnO2), zirconium dioxide (ZrO2), and silicon dioxide (SiO2) were selected to support the Ag active sites. The catalysts were characterized by techniques such as STEM (TEM), Raman, XPS, H2-TPR, and FT-IR spectroscopy to explore the morphology, Ag dispersion, surface properties, and electronic states. The catalytic results demonstrated that MnO2 with the highest reducibility exhibited superior catalytic performance, achieving 75.4% of HMF conversion and 41.6% of selectivity for 2,5-furandicarboxylic acid (FDCA) at 120 °C. In contrast, ZrO2 and SiO2 exhibited limited oxidation capabilities, mainly producing intermediate products like FFCA and/or HMFCA. The oxidation ability of these catalysts was governed by support reducibility, because it determined the density of oxygen vacancies (Ov) and surface hydroxyl groups (OOH), and eventually influenced the catalytic activity, as demonstrated by the reaction rate: Ag/MnO2 (3214.5 molHMF·gAg−1·h−1), Ag/ZrO2 (2062.3 molHMF·gAg−1·h−1), and Ag/SiO2 (1394.4 molHMF·gAg−1·h−1). These findings provide valuable insights into the rational design of high-performance catalysts for biomass-derived chemical conversion. Full article
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29 pages, 10851 KiB  
Review
Small Molecules Effective for Conversion of Lignocellulosic Biomass to Furfural and Its Derivatives
by Ivana Vojtová, Petr Leinweber and Tomáš Weidlich
Catalysts 2024, 14(11), 791; https://doi.org/10.3390/catal14110791 - 6 Nov 2024
Cited by 1 | Viewed by 1963
Abstract
This review summarizes recent applications of small organic and inorganic molecules as catalysts or solvents (chemical hands and scissors) in the production of furfural (FA), 5-(hydroxymethyl)furfural (HMF), and 5-(chloromethyl)furfural (CMF). The possible transformation of lignocellulosic biomass into a one-pot configuration and two-step technique [...] Read more.
This review summarizes recent applications of small organic and inorganic molecules as catalysts or solvents (chemical hands and scissors) in the production of furfural (FA), 5-(hydroxymethyl)furfural (HMF), and 5-(chloromethyl)furfural (CMF). The possible transformation of lignocellulosic biomass into a one-pot configuration and two-step technique based on the preliminary separation of hemicellulose, lignin and cellulose with the subsequent hydrolysis of separated polysaccharides is compared and discussed. Interestingly, these rather simple and cheap molecules are catalytically active and enable a high rate of conversion of polysaccharides into furfural and its derivatives. Usually, elevated pressure and reaction temperatures above 150 °C are necessary for effective hydrolysis and dehydration of in situ formed monosaccharides; nevertheless, ionic liquids or deep eutectic solvents enable a significant decrease in the reaction temperature and performance of the discussed process at ambient pressure. Full article
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22 pages, 4635 KiB  
Review
Recent Trends in the Synthesis of Monomers for Furanoate Polyesters and Their Nanocomposites’ Fabrication as a Sustainable Packaging Material
by Johan Stanley, Lidija Fras Zemljič, Dimitra A. Lambropoulou and Dimitrios N. Bikiaris
Sustainability 2024, 16(19), 8632; https://doi.org/10.3390/su16198632 - 5 Oct 2024
Cited by 3 | Viewed by 2443
Abstract
Furanoate polyesters are an extremely promising new class of materials for packaging applications, particularly furanoate-based nanocomposites, which have gained a high interest level in research and development in both academia and industries. The monomers utilised for the synthesis of furanoate-based polyesters were derived [...] Read more.
Furanoate polyesters are an extremely promising new class of materials for packaging applications, particularly furanoate-based nanocomposites, which have gained a high interest level in research and development in both academia and industries. The monomers utilised for the synthesis of furanoate-based polyesters were derived from lignocellulosic biomass, which is essential for both eco-friendliness and sustainability. Also, these polyesters have a lower carbon footprint compared to fossil-based plastics, contributing to greenhouse gas reduction. The furanoate-based nanocomposites exhibit enhanced performance characteristics, such as high thermal stability, excellent mechanical strength, superior barrier resistance, and good bacteriostatic rate, making them suitable for a wide range of industrial applications, especially for food-packaging applications. This paper reviews the recent trends in the synthesis routes of monomers, such as the various catalytic activities involved in the oxidation of 5(hydroxymethyl)furfural (HMF) into 2,5-furandicarboxylic acid (FDCA) and its ester, dimethyl furan-2,5-dicarboxylate (DMFD). In addition, this review explores the fabrication of different furanoate-based nanocomposites prepared by in situ polymerization, by melt mixing or solvent evaporation methods, and by using different types of nanoparticles to enhance the overall material properties of the resulting nanocomposites. Emphasis was given to presenting the effect of these nanoparticles on the furanoate polyester’s properties. Full article
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29 pages, 7614 KiB  
Review
Advancements in Non-Thermal Processing Technologies for Enhancing Safety and Quality of Infant and Baby Food Products: A Review
by Nasim Pasdar, Parisa Mostashari, Ralf Greiner, Anissa Khelfa, Ali Rashidinejad, Hadi Eshpari, Jim M. Vale, Seyed Mohammad Taghi Gharibzahedi and Shahin Roohinejad
Foods 2024, 13(17), 2659; https://doi.org/10.3390/foods13172659 - 23 Aug 2024
Cited by 8 | Viewed by 4509
Abstract
Breast milk is the main source of nutrition during early life, but both infant formulas (Ifs; up to 12 months) and baby foods (BFs; up to 3 years) are also important for providing essential nutrients. The infant food industry rigorously controls for potential [...] Read more.
Breast milk is the main source of nutrition during early life, but both infant formulas (Ifs; up to 12 months) and baby foods (BFs; up to 3 years) are also important for providing essential nutrients. The infant food industry rigorously controls for potential physical, biological, and chemical hazards. Although thermal treatments are commonly used to ensure food safety in IFs and BFs, they can negatively affect sensory qualities, reduce thermosensitive nutrients, and lead to chemical contaminant formation. To address these challenges, non-thermal processing technologies such as high-pressure processing, pulsed electric fields, radio frequency, and ultrasound offer efficient pathogen destruction similar to traditional thermal methods, while reducing the production of key process-induced toxicants such as furan and 5-hydroxymethyl-2-furfural (HMF). These alternative thermal processes aim to overcome the drawbacks of traditional methods while retaining their advantages. This review paper highlights the growing global demand for healthy, sustainable foods, driving food manufacturers to adopt innovative and efficient processing techniques for both IFs and BFs. Based on various studies reviewed for this work, the application of these novel technologies appears to reduce thermal processing intensity, resulting in products with enhanced sensory properties, comparable shelf life, and improved visual appeal compared to conventionally processed products. Full article
(This article belongs to the Special Issue Feature Review on Food Nutrition)
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15 pages, 1360 KiB  
Article
Bioconversion of Furanic Compounds by Chlorella vulgaris—Unveiling Biotechnological Potentials
by Ricarda Kriechbaum, Oliver Spadiut and Julian Kopp
Microorganisms 2024, 12(6), 1222; https://doi.org/10.3390/microorganisms12061222 - 18 Jun 2024
Cited by 1 | Viewed by 1198
Abstract
Lignocellulosic biomass is abundant on Earth, and there are multiple acidic pretreatment options to separate the cellulose, hemicellulose, and lignin fraction. By doing so, the fermentation inhibitors 5-Hydroxymethylfurfural (HMF) and furfural (FF) are produced in varying concentrations depending on the hydrolyzed substrate. In [...] Read more.
Lignocellulosic biomass is abundant on Earth, and there are multiple acidic pretreatment options to separate the cellulose, hemicellulose, and lignin fraction. By doing so, the fermentation inhibitors 5-Hydroxymethylfurfural (HMF) and furfural (FF) are produced in varying concentrations depending on the hydrolyzed substrate. In this study, the impact of these furanic compounds on Chlorella vulgaris growth and photosynthetic activity was analyzed. Both compounds led to a prolonged lag phase in Chlorella vulgaris growth. While the photosynthetic yield Y(II) was not significantly influenced in cultivations containing HMF, FF significantly reduced Y(II). The conversion of 5-Hydroxymethylfurfural and furfural to 5-Hydroxymethyl-2-Furoic Acid and 2-Furoic Acid was observed. In total, 100% of HMF and FF was converted in photoautotrophic and mixotrophic Chlorella vulgaris cultivations. The results demonstrate that Chlorella vulgaris is, as of now, the first known microalgal species converting furanic compounds. Full article
(This article belongs to the Special Issue The Application Potential of Microalgae in Green Biotechnology)
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16 pages, 1671 KiB  
Article
Kinetic Modeling of Cornstalk Cellulose Hydrolysis in Supercritical Water: A Comparative Study of the Effects of Temperature and Residence Time on Derivative Production
by Muhammad Muzamal Ashfaq, Oksana Zholobko and Xiang-Fa Wu
Processes 2023, 11(10), 3030; https://doi.org/10.3390/pr11103030 - 21 Oct 2023
Cited by 1 | Viewed by 1836
Abstract
Kinetic modeling is essential in understanding and controlling the process of cellulose hydrolysis for producing value-added cellulose derivatives. This study aims to adopt a set of dominate kinetic ordinary differential equations of cornstalk cellulose hydrolysis in supercritical water for mechanism-based prediction of the [...] Read more.
Kinetic modeling is essential in understanding and controlling the process of cellulose hydrolysis for producing value-added cellulose derivatives. This study aims to adopt a set of dominate kinetic ordinary differential equations of cornstalk cellulose hydrolysis in supercritical water for mechanism-based prediction of the production of cellulose, glucose, fructose, glyceraldehyde, erythrose, 5-hydroxymethyl furfural, glycolaldehyde, threose, aldose, and other cellulose derivatives from cornstalks under processing conditions with a pressure of 89 MPa and a temperature of 378 °C, as considered in a recent experimental study in the literature. The yield rates of several cellulose derivatives, e.g., glucose, fructose, 5-HMF, and erythrose as predicted by the present model, are close to those of experimental measurements. The model is further used to predict the yield rates of a few new cellulose derivatives, e.g., glycolaldehyde, threose, and aldose, that are potentially generated in cornstalk cellulose hydrolysis in supercritical water. The present model and computational simulations can be utilized as a rational tool to predict, control, and optimize the derivative yields in cellulose hydrolysis in supercritical water via tuning the process parameters, and, therefore, are useful for the optimal production of targeted bio-based fuels and chemicals from cornstalks and other agricultural and municipal wastes. Full article
(This article belongs to the Topic Advances in Biomass Conversion)
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14 pages, 3717 KiB  
Review
An Overview on Production of Lignocellulose-Derived Platform Chemicals Such as 5-Hydroxymethyl Furfural, Furfural, Protocatechuic Acid
by Pravin P. Upare, Rachel E. Clarence, Hyungsub Shin and Byung Gyu Park
Processes 2023, 11(10), 2912; https://doi.org/10.3390/pr11102912 - 4 Oct 2023
Cited by 12 | Viewed by 3355
Abstract
Furan derivatives such as 5-hydroxymethyl furfural (HMF) and furfural (FA) and aromatic acids such as protocatechuic acid (PCA) represent the most essential classes of intermediates derived from lignocellulosic biomass. These bio-based compounds are potential feedstocks for producing bio-based chemicals and fuels. However, the [...] Read more.
Furan derivatives such as 5-hydroxymethyl furfural (HMF) and furfural (FA) and aromatic acids such as protocatechuic acid (PCA) represent the most essential classes of intermediates derived from lignocellulosic biomass. These bio-based compounds are potential feedstocks for producing bio-based chemicals and fuels. However, the derivatives of these bio-based compounds are useful in their antioxidative, antibacterial, and anti-aging activities. Protocatechuic acid (PCA, 2,3-dihydroxybenzoic acid), derived from lignin biomass, is also one of the essential bio-derived aromatic intermediates with an active acid and hydroxyl group, which can elevate it into an important class of potential platform chemicals for the production of value-added chemicals, such as HMF and furfuryl alcohol (FAL). The platform compounds are indeed the most used furan-based feedstocks since their chemical structure allows the preparation of various high-value-added chemicals. The related catalytic techniques are well known for the upgradation of biomass into these platform chemicals and their conversion into value-added chemicals. In this short review, we aim to briefly discuss biomass conversion into FA, HMF, and PCA and related heterogeneous catalytic processes. In addition, a few potential ongoing research trends are also proposed to provide some ideas for the further preparation of bio-based innovative derivatives in a much more green, simple, efficient, and economical way. Full article
(This article belongs to the Special Issue Biomass Pretreatment for Thermochemical Conversion)
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19 pages, 3075 KiB  
Article
Whole-Genome Sequence and Fermentation Characteristics of Enterobacter hormaechei UW0SKVC1: A Promising Candidate for Detoxification of Lignocellulosic Biomass Hydrolysates and Production of Value-Added Chemicals
by Santosh Kumar, Eric Agyeman-Duah and Victor C. Ujor
Bioengineering 2023, 10(9), 1090; https://doi.org/10.3390/bioengineering10091090 - 16 Sep 2023
Cited by 7 | Viewed by 2726
Abstract
Enterobacter hormaechei is part of the Enterobacter cloacae complex (ECC), which is widespread in nature. It is a facultative Gram-negative bacterium of medical and industrial importance. We assessed the metabolic and genetic repertoires of a new Enterobacter isolate. Here, we report the whole-genome [...] Read more.
Enterobacter hormaechei is part of the Enterobacter cloacae complex (ECC), which is widespread in nature. It is a facultative Gram-negative bacterium of medical and industrial importance. We assessed the metabolic and genetic repertoires of a new Enterobacter isolate. Here, we report the whole-genome sequence of a furfural- and 5-hydroxymethyl furfural (HMF)-tolerant strain of E. hormaechei (UW0SKVC1), which uses glucose, glycerol, xylose, lactose and arabinose as sole carbon sources. This strain exhibits high tolerance to furfural (IC50 = 34.2 mM; ~3.3 g/L) relative to Escherichia coli DH5α (IC50 = 26.0 mM; ~2.5 g/L). Furfural and HMF are predominantly converted to their less-toxic alcohols. E. hormaechei UW0SKVC1 produces 2,3-butanediol, acetoin, and acetol, among other compounds of industrial importance. E. hormaechei UW0SKVC1 produces as high as ~42 g/L 2,3-butanediol on 60 g/L glucose or lactose. The assembled genome consists of a 4,833,490-bp chromosome, with a GC content of 55.35%. Annotation of the assembled genome revealed 4586 coding sequences and 4516 protein-coding genes (average length 937-bp) involved in central metabolism, energy generation, biodegradation of xenobiotic compounds, production of assorted organic compounds, and drug resistance. E. hormaechei UW0SKVC1 shows considerable promise as a biocatalyst and a genetic repository of genes whose protein products may be harnessed for the efficient bioconversion of lignocellulosic biomass, abundant glycerol and lactose-replete whey permeate to value-added chemicals. Full article
(This article belongs to the Special Issue Biological Production of Value-Added Products)
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14 pages, 1320 KiB  
Article
Iron(III) Sulfate-Mediated Synthesis of 2,5-Furandicarboxylic Acid Dimethyl Ester from Galactaric Acid
by Giacomo Trapasso, Beatriz Chícharo, Thomas Gherardi, Davide Redolfi-Bristol and Fabio Aricò
Catalysts 2023, 13(7), 1114; https://doi.org/10.3390/catal13071114 - 17 Jul 2023
Cited by 11 | Viewed by 3562
Abstract
2,5-furandicarboxylic acid (FDCA) is one of the most studied bio-based monomers, being considered the best substitute for fossil-derived terephthalic acid in plastic production. FDCA is employed in the preparation of polyethylene furanoate (PEF), demonstrating superior mechanical and thermal proprieties compared to the widely [...] Read more.
2,5-furandicarboxylic acid (FDCA) is one of the most studied bio-based monomers, being considered the best substitute for fossil-derived terephthalic acid in plastic production. FDCA is employed in the preparation of polyethylene furanoate (PEF), demonstrating superior mechanical and thermal proprieties compared to the widely used polyethylene terephthalate (PET). Nevertheless, FDCA synthesis mostly relies on the oxidation of the bio-based platform chemical hydroxymethyl furfural (HMF), whose notoriously instable nature renders FDCA yield and industrial scale-up production complicated. On the contrary, FDCA esters are less studied, even though they have greater solubility in organic media, which would favor their isolation and potential application as monomers for PEF. On these premises, we report herein an alternative green synthetic approach to FDCA methyl ester (FDME) using galactaric acid as the substrate, dimethyl carbonate (DMC) as the green media, and Fe2(SO4)3 as the heterogeneous Lewis acid. Optimization of the reaction conditions allowed the selective production of FDME in a 70% isolated yield; product purification was achieved via flash column chromatography over silica. Furthermore, it was possible to employ up to 5.0 g of galactaric acid in a single reaction, leading to a good isolated yield of FDME. Full article
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17 pages, 6686 KiB  
Article
Catalytic Conversion of Carbohydrates into 5-Hydroxymethylfurfural by Phosphotungstic Acid Encapsulated in MIL-101 (Cr, Sn) Catalyst in Deep Eutectic Solvents
by Wei Mao, Jiawen Hao, Lingyu Zeng, Hao Wang, Hao Xu and Jinghong Zhou
Int. J. Mol. Sci. 2023, 24(14), 11480; https://doi.org/10.3390/ijms241411480 - 14 Jul 2023
Cited by 3 | Viewed by 1829
Abstract
Herein, we report the synthesis of bimetal–organic frameworks (BMOFs) with both Brønsted and Lewis acidities, in which phosphotungstic acid (PTA) was encapsulated in BMOFs. It is efficient in converting starch to 5-hydroxymethyl-furfural (HMF) in deep eutectic solvents (DESs) such as choline chloride and [...] Read more.
Herein, we report the synthesis of bimetal–organic frameworks (BMOFs) with both Brønsted and Lewis acidities, in which phosphotungstic acid (PTA) was encapsulated in BMOFs. It is efficient in converting starch to 5-hydroxymethyl-furfural (HMF) in deep eutectic solvents (DESs) such as choline chloride and formic acid. The highest yield of HMF (37.94%) was obtained using P0.5/BMOFs1.0 to catalyze starch in a mixed solvent system comprising DESs and ethyl acetate (EAC) (v/v; 2:3) at 180 °C and a reaction time of 10 min. Employing a DES as a cocatalyst and solvent reduced the use of organic solvents. The catalyst showed adequate reusability, and the HMF yield only decreased by 2.88% after six cycles of reuse compared with that of the initial catalyst. This study demonstrates the application potential of BMOFs in the conversion of biomass to useful molecules with commercial and/or research value. Full article
(This article belongs to the Special Issue Bio-Polymer Materials and Bio-Refinery 2.0)
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16 pages, 3971 KiB  
Article
Innovative Synthetic Approaches for Sulphate-Promoted Catalysts for Biomass Valorisation
by Alessia Giordana, Cristina Pizzolitto, Elena Ghedini, Michela Signoretto, Lorenza Operti and Giuseppina Cerrato
Catalysts 2023, 13(7), 1094; https://doi.org/10.3390/catal13071094 - 12 Jul 2023
Cited by 1 | Viewed by 1725
Abstract
In the present research, we report on an innovative and quick procedure for the synthesis of metal oxides: a sol-gel procedure which is followed by two steps that are assisted by microwaves (MW) heating. First, MW heating promotes gel drying and successively permits [...] Read more.
In the present research, we report on an innovative and quick procedure for the synthesis of metal oxides: a sol-gel procedure which is followed by two steps that are assisted by microwaves (MW) heating. First, MW heating promotes gel drying and successively permits the calcination of the xerogel in a few minutes, using a susceptor that rapidly reaches high temperatures. The procedure was employed for the synthesis of zirconium dioxide (ZrO2), and MW-assisted calcination enables the collection of tetragonal ZrO2, as confirmed by different experimental techniques (PXRD, HR-TEM and Raman spectroscopy). Using this MW-assisted sol-gel procedure, a promoted sulphated zirconia (SZ) has been obtained. Both the nature and strength of SZ surface acidity have been investigated with FTIR spectroscopy using CO and 2,6-dimethylpyridine (2,6-DMP) as probe molecules. The obtained materials were tested as catalysts in acid hydrolysis of glucose to give 5-(hydroxymethyl)furfural (5-HMF). One of the obtained catalysts exhibited a better selectivity towards 5-HMF with respect to SZ material prepared by a classical precipitation route, suggesting that this procedure could be employed to obtain a well-known catalyst with a less energy-consuming procedure. Catalytic results also suggest that good selectivity to 5-HMF can be achieved in aqueous media in the presence of weak Lewis and Brønsted sites. Full article
(This article belongs to the Special Issue Advanced Materials for Application in Catalysis)
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13 pages, 6154 KiB  
Article
Microwave-Assisted Catalytic Conversion of 5-HMF for Biofuel Additives by Molybdophosphoric Acid Encapsulated KCC-1
by Srinivasan Vinju Vasudevan, Jin Cai, Junming Xu, Hongjian Lin, Hongliang Wang and Quan Bu
Catalysts 2023, 13(6), 969; https://doi.org/10.3390/catal13060969 - 2 Jun 2023
Cited by 2 | Viewed by 1920
Abstract
In this work, the microwave-assisted reaction of 5-hydroxymethylfurfural (5-HMF) into valuable ether and acylated production formation was investigated with the help of molybdophosphoric acid encapsulated dendritic fibrous silica (KCC-1) as a catalyst. XRD, N2 adsorption-desorption, SEM, FT-IR, NH3-TPD, and TEM [...] Read more.
In this work, the microwave-assisted reaction of 5-hydroxymethylfurfural (5-HMF) into valuable ether and acylated production formation was investigated with the help of molybdophosphoric acid encapsulated dendritic fibrous silica (KCC-1) as a catalyst. XRD, N2 adsorption-desorption, SEM, FT-IR, NH3-TPD, and TEM were used to analyze the physicochemical and structural properties of the synthesized catalysts. The microwave etherification of 5-HMF with ethanol was tested using synthesized catalysts. The effects of the reaction temperature, reaction time, catalytic amount, and microwave power were investigated. The resulting MPA-KCC-1 and IMPA-KCC-1 catalysts demonstrated excellent activity for the etherification of 5-HMF with ethanol, producing 5-(hydroxymethyl) furfural diethyl acetal (HMFDEA) and 5-(ethoxymethyl)furfural diethyl acetal (EMFDEA) products selectively. The significant advantages of the work are the selective production of EMFDEA at 82%, the catalyst can be easily removed via filtration, and the catalyst activity remains nearly intact even after five reaction cycles. Full article
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15 pages, 1122 KiB  
Article
Biosynthesis of Furfurylamines in Batch and Continuous Flow by Immobilized Amine Transaminases
by Tobias Heinks, Luisa M. Merz, Jan Liedtke, Matthias Höhne, Luuk M. van Langen, Uwe T. Bornscheuer, Gabriele Fischer von Mollard and Per Berglund
Catalysts 2023, 13(5), 875; https://doi.org/10.3390/catal13050875 - 11 May 2023
Cited by 8 | Viewed by 4224
Abstract
Building blocks with amine functionality are crucial in the chemical industry. Biocatalytic syntheses and chemicals derived from renewable resources are increasingly desired to achieve sustainable production of these amines. As a result, renewable materials such as furfurals, especially furfurylamines like 5-(hydroxymethyl)furfurylamine (HMFA) and [...] Read more.
Building blocks with amine functionality are crucial in the chemical industry. Biocatalytic syntheses and chemicals derived from renewable resources are increasingly desired to achieve sustainable production of these amines. As a result, renewable materials such as furfurals, especially furfurylamines like 5-(hydroxymethyl)furfurylamine (HMFA) and 2,5-di(aminomethyl)furan (DAF), are gaining increasing attention. In this study, we identified four different amine transaminases (ATAs) that catalyze the reductive amination of 5-(hydroxymethyl)furfural (HMF) and 2,5-diformylfuran (DFF). We successfully immobilized these ATAs on glutaraldehyde-functionalized amine beads using multiple binding and on amine beads by site-selective binding of the unique Cα-formylglycine within an aldehyde tag. All immobilized ATAs were efficiently reused in five repetitive cycles of reductive amination of HMF with alanine as co-substrate, while the ATA from Silicibacter pomeroyi (ATA-Spo) also exhibited high stability for reuse when isopropylamine was used as an amine donor. Additionally, immobilized ATA-Spo yielded high conversion in the batch syntheses of HMFA and DAF using alanine (87% and 87%, respectively) or isopropylamine (99% and 98%, respectively) as amine donors. We further demonstrated that ATA-Spo was effective for the reductive amination of HMF with alanine or isopropylamine in continuous-flow catalysis with high conversion up to 12 days (48% and 41%, respectively). Full article
(This article belongs to the Special Issue Supported Biocatalysts for Sustainable Chemistry)
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13 pages, 4611 KiB  
Article
Eco-Friendly Catalytic Synthesis of Top Value Chemicals from Valorization of Cellulose Waste
by Onofrio Losito, Michele Casiello, Caterina Fusco, Helena Mateos Cuadrado, Antonio Monopoli, Angelo Nacci and Lucia D’Accolti
Polymers 2023, 15(6), 1501; https://doi.org/10.3390/polym15061501 - 17 Mar 2023
Cited by 4 | Viewed by 2482
Abstract
The total amount of cellulose from paper, wood, food, and other human activity waste produced in the EU is in the order of 900 million tons per year. This resource represents a sizable opportunity to produce renewable chemicals and energy. This paper reports, [...] Read more.
The total amount of cellulose from paper, wood, food, and other human activity waste produced in the EU is in the order of 900 million tons per year. This resource represents a sizable opportunity to produce renewable chemicals and energy. This paper reports, unprecedently in the literature, the usage of four different urban wastes such as cigarette butts, sanitary pant diapers, newspapers, and soybean peels as cellulose fonts to produce valuable industrial intermediates such as levulinic acid (LA), 5-acetoxymethyl-2-furaldehyde (AMF), 5-(hydroxymethyl)furfural (HMF), and furfural. The process is accomplished by the hydrothermal treatment of cellulosic waste using both Brønsted and Lewis acid catalysts such as CH3COOH (2.5–5.7 M), H3PO4 (15%), and Sc(OTf)3 (20% w:w), thus obtaining HMF (22%), AMF (38%), LA (25–46%), and furfural (22%) with good selectivity and under relatively mild conditions (T = 200 °C, time = 2 h). These final products can be employed in several chemical sectors, for example, as solvents, fuels, and for new materials as a monomer precursor. The characterization of matrices was accomplished by FTIR and LCSM analyses, demonstrating the influence of morphology on reactivity. The low e-factor values and the easy scale up render this protocol suitable for industrial applications. Full article
(This article belongs to the Special Issue Bioresource-Derived Composites for Diverse Applications)
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