Characterization of a lignin-based gel responsive to aqueous binary solvents and pH

A lignin-based gel (AL-PE gel) was obtained from hardwood acetic acid lignin (AL) and poly(ethylene glycol) diglycidyl ether (PE) as a cross-linker at a high AL concentration, while the reaction at a lower AL concentration yielded an amphipathic derivative (am-AL-PE). The gel has been reported to swell in aqueous ethanol but shrink in pure water and ethanol. In the present work, swelling behaviors in other aqueous binary solvents and the swelling mechanism were investigated to explore novel lignin-based functional materials, such as stimuli-and/or environment-responsive gels. The AL-PE gel swelled in aqueous methanol, isopropanol, acetone, and tetrahydrofuran, and the order of swelling in the solvents was consistent with that of the am-AL-PE. Spin-spin relaxation time (T 2 ) measurements with 1H NMR analysis of the gel in aqueous acetone revealed that gel swelling was closely related to an increasing T 2 of acetone bound to the gel network. The nature of the lignin moiety in the gel also enabled a pH response, and the amphipathic nature of the gel provided it with a function as an absorbent for cationic surfactants. The results of this study can contribute to the valorization of lignin as a main component for solvent sensors and environmental purification materials.

Preparation of electrode for electric double layer capacitor from electrospun lignin fibers

Lignin-based activated carbon fibers (ACFs) were prepared by electrospinning of hardwood acetic acid lignin (HW-AAL) solution followed by thermostabilization, carbonization, and steam activation. The thermostabilization process was able to be remarkably shortened from 38 h to 3 h with hexamethylenetetramine (hexamine) in binary solvents, AcOH/CCl4 (8/2), when compared with conventional thermostabilization processes. The resultant ACFs possessed higher specific surface area (2185 m2 g-1) than those from commercial activated carbon and electrospun lignin fibers without hexamine. These ACFs also exhibited good electrical capacitance (133.3 F g-1 at a current density of 1 A g-1) as electrodes of electric double layer capacitor (EDLC) are efficient not only due to their large surfaces area but also due to their porous structure with well-developed micropores (diameter: 0.5–1.3 nm). High energy density and power density of this EDLC (42 Wh kg-1 and 91 kW kg-1, respectively) were also achieved.

Fractionation and characterization of lignin-carbohydrate complexes (LCCs) of Eucalyptus globulus in residues left after MWL isolation. Part II: Analyses of xylan-lignin fraction (X-L)

The residual wood meal left after milled wood lignin (MWL) isolation [milled wood residue (MWR)] of 5-year-old Eucalyptus globulus was fractionated to afford a xylan-lignin fraction (X-L) in 2.9% yield (based on MWR) by the method reported previously. X-L was further fractionated with the lignin solvent 1,4-dioxane/water (9:1, v/v) to give a soluble fraction (XL-F1; 24.0%) and an insoluble fraction (XL-F1-residue; 74.6%; both yields based on X-L). XL-F1-residue was further extracted with the good xylan solvent dimethyl sulfoxide and the soluble fraction was termed XL-F2 (43.0%; based on the XL-F1-residue). XL-F1 was mainly composed of lignin with a small amount of xylan and it is similar to purified MWL, whereas XL-F2 was mainly composed of xylan with some amount of lignin and it is similar to a fraction that was prepared by the extraction of crude MWL with acetic acid [lignin-carbohydrate complex (LCC)-AcOH]. The two-dimensional heteronuclear single quantum coherence nuclear magnetic resonance spectra of XL-F1 and XL-F2 were interpreted that the former has α-ether-type lignin-carbohydrate (LC) linkages and the latter might have LC linkages of the phenyl glycoside type, which are different from those in LCC-AcOH.

Preparation and characterization of acetic acid lignin-based epoxy blends

Lignin-based epoxy resin (LER) was prepared from phenolated lignin (PL) and epichlorohydrin (ECH) in the presence of sodium hydroxide. The eucalyptus acetic acid lignin (AAL) was first reacted with phenol in the presence of sulfuric acid to obtain PL. Then, PL was reacted with ECH in aqueous sodium hydroxide to obtain LER. LER was mixed with diglycidyl ether of bisphenol A (E-44) and then cured with triethylenetetramine (TETA). The initial thermal degradation temperature (Td) of the cured epoxy blends decreased with the increase in LER content. The residue ratio at 500 °C of the cured epoxy blends (R500), however, increased with the LER content. The maximum adhesive shear strength of the cured epoxy blends was obtained at 20 wt% of LER. The water absorption of epoxy blends increased with increasing the content of LER. SEM photos showed that increasing the content of LER increased inhomogeneity and porosity of epoxy blends.