Shixue Ren

Separation and characterization of lignin from bio-ethanol production residue

In order to develop an adequate method to separate lignin from bio-ethanol production residue, solvent extraction was conducted by using benzyl alcohol, dioxane and ethanol. Compared to the conventional alkali-solution and acid-isolation method, benzyl alcohol and dioxane extraction could reach higher lignin yield of 71.55% and 74.14% respectively. FTIR and XRD analysis results indicate that sodium hydroxide solution dissolved most of the lignin in the raw material. However, the low lignin yield by this method may be attributed to the products loss during the complex separation process. GPC and (1)H NMR results revealed that the dioxane-lignin had closer molecular weight with alkali-lignin, lower S/G ratio (0.22) and higher OHPh/OHAl ratio (0.45) with respect to benzyl alcohol-lignin. The results divulge that the lignin products separated from bio-ethanol production residue by dioxane extraction had fairly potential application with better chemical activity.

Hydrogenolysis and Activation of Soda Lignin Using [BMIM]Cl as a Catalyst and Solvent

To improve the reactivity of the soda lignin, an acid ionic liquid 1-butyl-3-mthylimidazolium chloride ([BMIM]Cl) was used as the catalyst and solvent to degrade the soda lignin through hydrogenolysis. Structural elucidation of the lignin samples was conducted by using a combination of analytical methods including chemical analysis, ultraviolet spectrophotometry (UV spectrophotometry), Fourier transform infrared spectroscopy (FT-IR spectra), two-dimensional heteronuclear single quantum coherence nuclear magnetic resonance (2D-HSQC NMR) techniques, and gel permeation chromatography (GPC). The antioxidant activities of the lignin samples were evaluated using the diammonium 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonate) (ABTS+) radical scavenging and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging methods. The degradation mechanism was proposed based on the characterization results. The optimal reaction condition was as follows: the concentration of [BMIM]Cl in the solution was 10 wt %, the hydrogen initial pressure was 3 MPa, and the solution was heated for 4 h at 90 °C. After the reaction, the total hydroxyl content of the soda lignin increased by 81.3%, while the phenolic hydroxyl content increased by 23.1%. At the same time, the weight-average molar mass of the soda lignin sample decreased from 8220 to 6450 g/mol with an improved antioxidant activity. In addition, approximately 56.7% of the β-O-4 linkages were degraded in the lreaction. The main effect of the acid ionic liquid [BMIM]C1 was related to the cleavage of β-O-4 linkages. This study has shown the potential of using the catalyzed soda lignin as a natural polymer antioxidant.

Correlation between Solubility Parameters and Properties of Alkali Lignin/PVA Composites

Although lignin blending with thermoplastic polymers has been widely studied, the usefulness of the lignin–polymer composites is limited by the poor compatibility of the two components. In the present study, alkali lignin/PVA composite membranes were prepared by incorporating 10%, 15%, 20% and 25% alkali lignin into the composites. The thermodynamic parameters of the composites were measured using inverse gas chromatography (IGC). Composite membranes with 10%, 15%, 20%, and 25% alkali lignin had solubility parameters of 17.51, 18.70, 16.64 and 16.38 (J/cm3)0.5, respectively, indicating that the solubility parameter firstly increased, and then decreased, with increasing proportions of alkali lignin. When the alkali lignin content was 15%, the composites had the largest solubility parameters. The composite membrane with an alkali lignin content of 15% had a tensile strength of 18.86 MPa and a hydrophilic contact angle of 89°. We have shown that the solubility parameters of blends were related to mechanical and hydrophilic properties of the composites and the relationships have been verified experimentally and theoretically.

Quantitative Analysis of Relationship between Hansen Solubility Parameters and Properties of Alkali Lignin/Acrylonitrile–Butadiene–Styrene Blends

Blends of alkali lignin and acrylonitrile–butadiene–styrene (ABS) resin are physically mixed and injected into the injection molding system. Although the components of the blend are bound together by intermolecular forces, noticeable phase separation still occurs. In the present study, inverse gas chromatography technology was used to characterize the Hansen solubility parameters of alkali lignin/ABS blends. The relationship between the Hansen solubility parameters and thermodynamic properties was then determined. Hansen solubility parameters, at room temperature, of alkali lignin/ABS blends containing 0, 10, 20, and 30 wt % alkali lignin were 17.40, 19.20, 18.98, and 17.37 (J/cm3)0.5, respectively. Hansen solubility parameters of the blends were shown, both experimentally and theoretically, to be related to their mechanical and thermal properties.