Another highlight from the dipolar dephasing spectrum is the important contribution of terminal methyl groups in the alkyl region, which presents significant signals after dipolar filtering, indicating alkyl groups with high mobility, corroborating the results from the Py? MS analysis that indicates a wide range of aliphatic side chains in the pyrolytic products Table 1. The downfield signal at ppm can be assigned to the phenyl units peaks 5, 16, 17, and 19 and to the C? Other peaks are shown at and ppm and are consistent with the presence of carboxyl and carbonyl functional groups, respectively i.
The detailed richness of the sp-hybridized C signals were retained. Another highlight from the dipolar dephasing spectrum is the important contribution of terminal methyl groups in the alkyl region, which presents significant signals after dipolar filtering, indicating alkyl groups with high mobility, corroborating the results from the Py-GC-MS analysis that indicates a wide range of aliphatic side chains in the pyrolytic products Table 1.
The downfield signal at ppm can be assigned to the phenyl units peaks 5, 16, 17, and 19 and to the C-2 of 2-acetyl-furan structures peak 8 Table 1. The detailed richness of the sp 2 -hybridized C region, compared to the symmetrical and featureless aryl signal of high carbonized materials, and the presence of aliphatic and oxygenated functional groups corroborate the low carbonization of the cellulose. This, together with the Py-GC-MS and SEM data, indicates that the produced hydrochar is probably reactive carboxyl functionalities in the sense of cation adsorption, contributing to soil cation exchange capacity.
However, due to the low carbonization temperature, it is not so recalcitrant, and the possible lower C sequestration potential and long term effect of this material in the soil must be taken into account. The NMR technique corroborates Py-GC-MS results, both confirming that the hydrochar product contains intermediated polymer built mainly of furan elements. The cellulose sign is also inconspicuous in the NMR spectra, since signals around 75 ppm - indicative of the presence of hydroxylated methylene groups O-alkyl - were not prominent.
The same results were observed in the pyrolysis analysis. Additionally, a considerable amount of levoglucosan and levoglucosenone Lu et al.
It is important to note that the Py-CG-MS analysis provided a detailed view of the aromatic building blocks, indicating that hydrochar monomers are built on benzofuran-like components, whereas NMR provides valuable information on how these building blocks are connected in the hydrochar structure. The presence of carbonyl groups was detected by both analytical techniques, and the carbonyl function was identified by acetyl groups at the Py-GC-MS analysis, although organic acid groups are not promptly detected by pyrolysis due to decarboxylation during analysis Kaal et al.
From the results obtained in the present study, it is possible to infer that the MAHC was able to carry out until steps 3 and 4; however, without recalcitrant aromatic structures normally seen in charred cellulose. Hydrothermal carbonization is a novel route to produce carbon rich material and its use to produce a soil additive should be considered, mainly due to its functionalized chemical-nature product hydrochar.
The microwave-assisted hydrothermal carbonized product of cellulose hydrochar does not retain the original structure of the cellulose and its chemical composition is not similar to that of common cellulose charcoal, being comprised by products of cellulose hydrolysis, dehydration, and condensation of derivative sugars. The solid hydrochar product is not characterized by condensed aromatic structures that resemble charred materials; instead, it is characterized by clusters of aliphatic and aromatic domain, being the last one built mainly of furan elements.
Microwave-assisted hydrothermal carbonization yields a functionalized carbon rich material similar to that produced by the conventional hydrothermal process, but with milder conditions and shorter-time carbonization. Magic coal from the steam cooker. Max Planck Research , v. Renewable fuels and chemicals by thermal processing of biomass. Chemical Engineering Journal , v. Microwave processing of materials. Annual Review of Materials Science , v. Energy and Fuels , v.
Hydrothermal carbonization of biomass: a summary and discussion of chemical mechanisms for process engineering. Biofuels, Bioproducts and Biorefining , v. Geochimica et Cosmochimica Acta , v. The 'Terra Preta' phenomenon: a model for sustainable agriculture in the humid tropics. Naturwissenschaften , v.
Microwave-assisted hydrothermal carbonization of lignocellulosic materials. Materials Letters , v. KAAL, J.
Sustainable carbon materials from hydrothermal processes / edited by Maria-Magdalena Titirici
Applied Geochemistry , v. Fire-induced transformation of C- and N- forms in different organic soil fractions from a Dystric Cambisol under a Mediterranean pine forest Pinus pinaster.
Soil Biology and Biochemistry , v. Hydrothermal carbonization of biomass residuals: a comparative review of the chemistry, process and applications of wet and dry pyrolysis. Biofuels , v. LIU, Q. Study on the pyrolysis of wood-derived rayon fiber by thermogravimetry - mass spectrometry. Journal of Molecular Structure , v. LU, Q. Catalytic pyrolysis of cellulose with sulfated metal oxides: a promising method for obtaining high yield of light furan compounds.
Bioresource Technology, v. Journal of the Brazilian Chemical Society , v. Carbohydrate Research , v. On the presence of anhydro-oligosaccharides in the sirups from the fast pyrolysis of cellulose. Journal of Analytical and Applied Pyrolysis , v.
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The production of materials by hydrothermal carbonization of cellulose. Carbon , v. NMR Characterization of 13 C-benzene sorbed to natural and prepared charcoals. Environmental Science and Technology , v. Back in the black: hydrothermal carbonization of plant material as an efficient chemical process to treat the CO 2 problem? New Journal of Chemistry , v.
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YAO, C. Hydrothermal dehydration of aqueous fructose solutions in a closed system. Journal of Physical Chemistry C , v. Received on January 28, and accepted on April 3, All the contents of this journal, except where otherwise noted, is licensed under a Creative Commons Attribution License. Update Location. If you want NextDay, we can save the other items for later. Yes—Save my other items for later. No—I want to keep shopping. Order by , and we can deliver your NextDay items by. In your cart, save the other item s for later in order to get NextDay delivery.
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