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Fast Microwave-Assisted Hydrothermal Synthesis of Pure Layered ?-MnO? for Multivalent Ion Intercalation.

ABSTRACT: This work reports on the synthesis of layered manganese oxides (?-MnO?) and their possible application as cathode intercalation materials in Al-ion and Zn-ion batteries. By using a one-pot microwave-assisted synthesis route in 1.6 M KOH (MnVII:MnII = 0.33), a pure layered ?-MnO? birnessite phase without any hausmannite traces was obtained after only a 14 h reaction time period at 110 °C. Attempts to enhance crystallinity level of as-prepared birnessite through increasing of reaction time up to 96 h in 1.6 M KOH failed and led to decreases in crystallinity and the emergence of an additional hausmannite phase. The influence of MnII:OH- ratio (1:2 to 1:10) on phase crystallinity and hausmannite phase formation for 96 h reaction time was investigated as well. By increasing alkalinity of the reaction mixture up to 2.5 M KOH, a slight increase in crystallinity of birnessite phase was achieved, but hausmannite formation couldn't be inhibited as hoped. The as-prepared layered ?-MnO? powder material was spray-coated on a carbon paper and tested in laboratory cells with Al or Zn as active materials. The Al-ion tests were carried out in EMIMCl/AlCl? while the Zn-Ion experiments were performed in water containing choline acetate (ChAcO) or a ZnSO? solution. Best performance in terms of capacity was yielded in the Zn-ion cell (200 mWh g-1 for 20 cycles) compared to about 3 mAh g-1 for the Al-ion cell. The poor activity of the latter system was attributed to low dissociation rate of tetrachloroaluminate ions (AlCl?-) in the EMIMCl/AlCl? mixture into positive Al complexes which are needed for charge compensation of the oxide-based cathode during the discharge step.

SUBMITTER: Eckert M

PROVIDER: S-EPMC6317168 | biostudies-literature | 2018 Nov

REPOSITORIES: biostudies-literature

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Fast Microwave-Assisted Hydrothermal Synthesis of Pure Layered δ-MnO₂ for Multivalent Ion Intercalation.

Eckert Martin M Peters Willi W Drillet Jean-Francois JF

Materials (Basel, Switzerland) 20181128 12

This work reports on the synthesis of layered manganese oxides (δ-MnO₂) and their possible application as cathode intercalation materials in Al-ion and Zn-ion batteries. By using a one-pot microwave-assisted synthesis route in 1.6 M KOH (MnVII:MnII = 0.33), a pure layered δ-MnO₂ birnessite phase without any hausmannite traces was obtained after only a 14 h reaction time period at 110 °C. Attempts to enhance crystallinity level of as-prepared birnessite ...[more]

PMID: 30487398

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Project description:The exploitation of unavoidable food supply chain wastes resulting from primary and secondary processing for chemicals, materials, and bioenergy is an important concept in the drive towards circular-based, resource-efficient biorefineries rather than petroleum refineries. The potential production of hydrogels (materials) from unavoidable food supply chain wastes, which are naturally rich in biopolymers such as cellulose, hemicellulose, pectin, and lignin, represents an interesting opportunity. However, these intertwined and interconnected biopolymers require separation and deconstruction prior to any useful application. Thus, this study aims to explore the formation of hydrogels from defibrillated celluloses (MW-DFCs) produced via acid-free stepwise microwave hydrothermal processing of blackcurrant pomace residues. Initially, pectin was removed from blackcurrant pomace residues (MW, 100-160 °C), and the resultant depectinated residues were reprocessed at 160 °C. The pectin yield increased from 2.36 wt.% (MW, 100 °C) to 3.07 wt.% (MW, 140 °C) and then decreased to 2.05 wt.% (MW, 160 °C). The isolated pectins were characterized by attenuated total reflectance infrared spectroscopy (ATR-IR), thermogravimetric analysis (TGA), and 13C NMR (D2O). The cellulosic-rich residues were reprocessed (MW, 160 °C) and further characterized by ATR-IR, TGA, and Klason lignin analysis. All the MW-DFCs contained significant lignin content, which prevented hydrogel formation. However, subsequent bleaching (H2O2/OH-) afforded off-white samples with improved gelling ability at the concentration of 5% w/v. Confocal laser microscopy (CLSM) revealed the removal of lignin and a more pronounced cellulosic-rich material. In conclusion, the microwave-assisted defibrillation of blackcurrant pomace, an exploitable unavoidable food supply chain waste, affords cellulosic-rich materials with the propensity to form hydrogels which may serve useful applications when put back into food products, pharmaceuticals, cosmetics, and home and personal care products.

Dataset Information

Fast Microwave-Assisted Hydrothermal Synthesis of Pure Layered ?-MnO? for Multivalent Ion Intercalation.

Publications

Fast Microwave-Assisted Hydrothermal Synthesis of Pure Layered δ-MnO₂ for Multivalent Ion Intercalation.

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