scholarly journals Effects of Gamma-Valerolactone Assisted Fractionation of Ball-Milled Pine Wood on Lignin Extraction and Its Characterization as Well as Its Corresponding Cellulose Digestion

2020 ◽  
Vol 10 (5) ◽  
pp. 1599
Author(s):  
Muhammad Ajaz Ahmed ◽  
Jae Hoon Lee ◽  
Arsalan A. Raja ◽  
Joon Weon Choi
Keyword(s):  
Quantum Coherence ◽  
Removal Rate ◽  
Value Added ◽  
Crystallinity Index ◽  
Gel Permeation Chromatography ◽  
Heteronuclear Single Quantum Coherence ◽  
Nmr Spectrum ◽  
Molecular Weights ◽  
Lignin Removal ◽  
Lignin Extraction

Gamma-valerolactone (GVL) was found to be an effective, sustainable alternative in the lignocellulose defragmentation for carbohydrate isolation and, more specifically, for lignin dissolution. In this study, it was adapted as a green pretreatment reagent for milled pinewood biomass. The pretreatment evaluation was performed for temperature (140–180 °C) and reaction time (2–4 h) using 80% aqueous GVL to obtain the highest enzymatic digestibility of 92% and highest lignin yield of 33%. Moreover, the results revealed a positive correlation (R2 = 0.82) between the lignin removal rate and the crystallinity index of the treated biomass. Moreover, under the aforementioned conditions, lignin with varying molecular weights (150–300) was obtained by derivatization followed by reductive cleavage (DFRC). 2D heteronuclear single quantum coherence nuclear magnetic resonance (2D-HSQC-NMR) spectrum analysis and gel permeation chromatography (GPC) also revealed versatile lignin properties with relatively high β-O-4 linkages (23.8%–31.1%) as well as average molecular weights of 2847–4164 with a corresponding polydispersity of 2.54–2.96, indicating this lignin to be a heterogeneous feedstock for value-added applications of biomass. All this suggested that this gamma-valerolactone based pretreatment method, which is distinctively advantageous in terms of its effectiveness and sustainability, can indeed be a competitive option for lignocellulosic biorefineries.

scholarly journals Oxidative Depolymerization of Cellulolytic Enzyme Lignin over Silicotungvanadium Polyoxometalates

Polymers ◽  
2019 ◽  
Vol 11 (3) ◽  
pp. 564 ◽  
Author(s):  
Wenbiao Xu ◽  
Xiangyu Li ◽  
Junyou Shi
Keyword(s):  
Cellulosic Ethanol ◽  
Quantum Coherence ◽  
Value Added ◽  
Gel Permeation Chromatography ◽  
Catalytic Performance ◽  
Cellulolytic Enzyme ◽  
Hydrolysis Lignin ◽  
Heteronuclear Single Quantum Coherence ◽  
Highly Active ◽  
Gel Permeation

The aim of this study was to explore the catalytic performance of the oxidative depolymerization of enzymatic hydrolysis lignin from cellulosic ethanol fermentation residue by different vanadium substituted Keggin-type polyoxometalates (K5[SiVW11O40], K6[SiV2W10O40], and K6H[SiV3W9O40]). Depolymerized products were analyzed by gel permeation chromatography (GPC), gas chromatography–mass spectrometer (GC/MS), and two-dimensional heteronuclear single quantum coherence nuclear magnetic resonance (2D HSQC NMR) analysis. All catalysts showed an effective catalytic activity. The best result, concerning the lignin conversion and lignin oil production, was obtained by K6[SiV2W10O40], and the highest yield of oxidative depolymerization products of 53 wt % was achieved and the main products were monomer aromatic compounds. The HSQC demonstrated that the catalysts were very effective in breaking the β-O-4 structure, the dominant linkage in lignin, and the GPC analysis demonstrated that the molecular of lignin was declined significantly. These results demonstrate the vanadium substituted silicotungstic polyoxometalates were of highly active and stable catalysts for lignin conversion, and this strategy has the potential to be applicable for production of value-added chemicals from biorefinery lignin.

scholarly journals Optimization of Lignin Extraction Variables by Response Surface Methodology from Pine Saw Dust, and Quantification of Major Structural Units in Isolated Lignin Fraction

2021 ◽  
Vol 11 (4) ◽  
pp. 1739
Author(s):  
Muhammad Ajaz Ahmed ◽  
Jae Hoon Lee ◽  
Joon Weon Choi
Keyword(s):  
Response Surface Methodology ◽  
Response Surface ◽  
Quantum Coherence ◽  
Resonance Spectrum ◽  
Quadratic Model ◽  
Molecular Weights ◽  
Solids Loading ◽  
A Value ◽  
Lignin Extraction ◽  
Lignin Fraction

A synergistic combination of dioxane, acetic acid, and HCl was investigated for lignin extraction from pine wood biomass. After initial screening of reagent combination, response surface methodology (RSM) was used to optimize the lignin yield with respect to the variables of time 24–72 h, solids loading 5–15%, and catalyst dose 5–15 mL. A quadratic model predicted 8.33% of the lignin yield, and it was further confirmed experimentally and through the analysis of variance (ANOVA). Lignin at optimum combination exhibited features in terms of derivatization followed by reductive cleavage (DFRC) with a value of (305 µmol/gm), average molecular weights of 4358 and polydispersity of 1.65, and 2D heteronuclear single quantum coherence nuclear magnetic resonance spectrum (2D-HSQC NMR) analysis showing relative β-O-4 linkages (37.80%). From here it can be suggested that this fractionation can be one option for high quality lignin extraction from lignocellulosic biomass.

scholarly journals Solvothermal-Based Lignin Fractionation From Corn Stover: Process Optimization and Product Characteristics

2021 ◽  
Vol 9 ◽  
Author(s):  
Punjarat Khongchamnan ◽  
Wanwitoo Wanmolee ◽  
Navadol Laosiripojana ◽  
Verawat Champreda ◽  
Nopparat Suriyachai ◽  
...  
Keyword(s):  
Corn Stover ◽  
Quantum Coherence ◽  
Solid Phase ◽  
Value Added ◽  
Structural Features ◽  
Solvent Mixture ◽  
Single Step ◽  
Resonance Spectroscopy ◽  
Optimal Conditions ◽  
Lignin Removal

Fractionation of lignocellulosic is a fundamental step in the production of value-added biobased products. This work proposes an initiative to efficiently extract lignin from the corn stover using a single-step solvothermal fractionation in the presence of an acid promoter (H2SO4). The organic solvent mixture used consists of ethyl acetate, ethanol, and water at a ratio of 30: 25:45 (v/v), respectively. H2SO4 was utilized as a promoter to improve the performance and selectivity of lignin removal from the solid phase and to increase the amount of recovered lignin in the organic phase. The optimal conditions for this extraction, based on response surface methodology (RSM), are a temperature of 180°C maintained for 49.1 min at an H2SO4 concentration of 0.08 M. The optimal conditions show an efficient reaction with 98.0% cellulose yield and 75.0% lignin removal corresponding to 72.9% lignin recovery. In addition, the extracted lignin fractions, chemical composition, and structural features were investigated using Fourier transform infrared spectroscopy, thermogravimetric analysis, elemental analysis, and two-dimensional heteronuclear single quantum coherence nuclear magnetic resonance spectroscopy (2D-HSQC NMR). The results indicate that the recovered lignin primarily contains a β-O-4 linking motif based on 2D-HSQC spectra. In addition, new C–C inter-unit linkages (i.e., β-β, and β-5) are not formed in the recovered lignin during H2SO4-catalyzed solvothermal pretreatment. This work facilitates effective valorization of lignin into value-added chemicals and fuels.

Quantitative structural characterization of the lignins from the stem and pith of bamboo (Phyllostachys pubescens)

Holzforschung ◽  
2013 ◽  
Vol 67 (6) ◽  
pp. 613-627 ◽  
Author(s):  
Jia-Long Wen ◽  
Shao-Long Sun ◽  
Bai-Liang Xue ◽  
Run-Cang Sun
Keyword(s):  
Quantum Coherence ◽  
Flavonoid Compound ◽  
Phyllostachys Pubescens ◽  
Heteronuclear Single Quantum Coherence ◽  
Single Quantum ◽  
Structural Units ◽  
Diaryl Ethers ◽  
Molecular Weights ◽  
C Nmr

Abstract Milled wood lignins (MWL) were isolated from the stem (MWLS) and pith (MWLP) of bamboo (Phyllostachys pubescens). The nonacetylated and acetylated bamboo MWLs were investigated by Fourier transform infrared, quantitative 13C-nuclear magnetic resonance (NMR), 2D heteronuclear single quantum coherence (HSQC) NMR, and 31P-NMR spectroscopy. The MWL consists of p-hydroxyphenyl (1–2%), guaiacyl (21–31%), and syringyl (67–78%) units associated with p-coumarates and ferulates. A modified quantitative 13C-NMR and 2D-HSQC analysis has demonstrated that the predominant intermonomeric linkages are of the type β-O-4 (45–49 per 100 C9 units, i.e., per C900) along with small amounts of other structural units such as resinols (3.6–7.4 per C900), tetrahydrofuran (2.0–2.3 per C900), phenylcoumaran (2.8–4.5 per C900), spirodienones (1.3–2.3 per C900), and α,β-diaryl ethers (2.8–2.9 per C900). MWLP contained more p-coumarates than MWLS. The various degrees of γ-acylation (17–27%) were positively associated with S/G ratios in the lignins; however, γ-acylation was inversely correlated to the ratio between β-β and β-O-4 side chains in these lignin fractions. Moreover, a flavonoid compound (tricin) was also detected in the MWLS but not in MWLP. The two MWLs are very similar in terms of molecular weights and the contents of OHphen and OHaliph.

scholarly journals N-[7-Chloro-4-[4-(phenoxymethyl)-1H-1,2,3-triazol-1-yl] quinoline]-acetamide

Molbank ◽  
10.3390/m1213 ◽  
2021 ◽  
Vol 2021 (2) ◽  
pp. M1213
Author(s):  
Paolo Coghi ◽  
Jerome P. L. Ng ◽  
Ali Adnan Nasim ◽  
Vincent Kam Wai Wong
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Quantum Coherence ◽  
Biologically Active ◽  
Proton Nuclear Magnetic Resonance ◽  
Dipolar Cycloaddition ◽  
Heteronuclear Single Quantum Coherence ◽  
Pharmacokinetic Properties ◽  
Nuclear Magnetic

The 1,2,3-triazole is a well-known biologically active pharmacophore constructed by the copper-catalyzed azide–alkyne cycloaddition. We herein reported the synthesis of 4-amino-7-chloro-based [1,2,3]-triazole hybrids via Cu(I)-catalyzed Huisgen 1,3-dipolar cycloaddition of 4-azido-7-chloroquinoline with an alkyne derivative of acetaminophen. The compound was fully characterized by Fourier-transform infrared (FTIR), proton nuclear magnetic resonance (1H-NMR), carbon-13 nuclear magnetic resonance (13C-NMR), heteronuclear single quantum coherence (HSQC), ultraviolet (UV) and high-resolution mass spectroscopies (HRMS). This compound was screened in vitro with different normal and cancer cell lines. The drug likeness of the compound was also investigated by predicting its pharmacokinetic properties.

scholarly journals Recycling Waste Cotton Cloths for the Isolation of Cellulose Nanocrystals: A Sustainable Approach

Polymers ◽  
2021 ◽  
Vol 13 (4) ◽  
pp. 626
Author(s):  
Siti Hajar Mohamed ◽  
Md. Sohrab Hossain ◽  
Mohamad Haafiz Mohamad Kassim ◽  
Mardiana Idayu Ahmad ◽  
Fatehah Mohd Omar ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Cellulose Nanocrystals ◽  
Value Added ◽  
Crystallinity Index ◽  
Attenuated Total Reflection ◽  
Cellulose Content ◽  
Scanning Calorimetry ◽  
Good Thermal Stability ◽  
Alkaline Pulping ◽  
Hydrolysis Of Cellulose

There is an interest in the sustainable utilization of waste cotton cloths because of their enormous volume of generation and high cellulose content. Waste cotton cloths generated are disposed of in a landfill, which causes environmental pollution and leads to the waste of useful resources. In the present study, cellulose nanocrystals (CNCs) were isolated from waste cotton cloths collected from a landfill. The waste cotton cloths collected from the landfill were sterilized and cleaned using supercritical CO2 (scCO2) technology. The cellulose was extracted from scCO2-treated waste cotton cloths using alkaline pulping and bleaching processes. Subsequently, the CNCs were isolated using the H2SO4 hydrolysis of cellulose. The isolated CNCs were analyzed to determine the morphological, chemical, thermal, and physical properties with various analytical methods, including attenuated total reflection-Fourier transform-infrared spectroscopy (ATR-FTIR), field-emission scanning electron microscopy (FE-SEM), energy-filtered transmission electron microscopy (EF-TEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). The results showed that the isolated CNCs had a needle-like structure with a length and diameter of 10–30 and 2–6 nm, respectively, and an aspect ratio of 5–15, respectively. Additionally, the isolated CNCs had a high crystallinity index with a good thermal stability. The findings of the present study revealed the potential of recycling waste cotton cloths to produce a value-added product.

scholarly journals Synthesis and In Vitro Antimicrobial Evaluation of Photoactive Multi—Block Chalcone Conjugate Phthalimide and 1,8-Naphthalimide Novolacs

Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1859
Author(s):  
Periyan Durairaju ◽  
Chinnasamy Umarani ◽  
Govindasami Periyasami ◽  
Perumberkandigai Adikesavan Vivekanand ◽  
Mostafizur Rahaman
Keyword(s):  
Spectroscopic Analysis ◽  
Photophysical Properties ◽  
Gel Permeation Chromatography ◽  
13C Nmr Spectroscopy ◽  
Antimicrobial Activities ◽  
Microbial Activities ◽  
E Coli ◽  
Molecular Weights ◽  
Antimicrobial Evaluation

Herein we report new multiblock chalcone conjugate phthalimide and naphthalimide functionalized copolymers with a topologically novel architecture synthesis using nucleophilic substitution and polycondensation methodology. The structures of the synthesized novolacs were elucidated on the basis of their spectroscopic analysis including FTIR, 1H NMR, and 13C NMR spectroscopy. Further, the number-average and weight-average molecular weights of the novolac polymers were determined by gel permeation chromatography (GPC). We examined the solubility of the synthesized polymers in various organic solvents including CHCl3, CH3CN, THF, H2O, CH3OH, DMSO, and DMF and found they are insoluble in both methanol and water. The novolac polymers were evaluated for their photophysical properties and microbial activities. The investigation of the antimicrobial activities of these polymers reveals significant antimicrobial activity against the pathogens E. coli, S. aureus, C. albicans, and A. niger.

Probing the molecular weights of sweetgum and pine kraft lignin fractions

TAPPI Journal ◽  
2021 ◽  
Vol 20 (6) ◽  
pp. 381-391
Author(s):  
JULIANA M. JARDIM ◽  
PETER W. HART ◽  
LUCIAN LUCIA ◽  
HASAN JAMEEL
Keyword(s):  
Molecular Weight ◽  
Black Liquor ◽  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Systematic Investigation ◽  
Kraft Pulping ◽  
Molecular Weights ◽  
Lignin Recovery ◽  
Lignin Reactivity ◽  
Kinetics Of

The present investigation undertook a systematic investigation of the molecular weight (MW) of kraft lignins throughout the pulping process to establish a correlation between MW and lignin recovery at different extents of the kraft pulping process. The evaluation of MW is crucial for lignin characterization and utilization, since it is known to influence the kinetics of lignin reactivity and its resultant physicochemical properties. Sweetgum and pine lignins precipitated from black liquor at different pHs (9.5 and 2.5) and different extents of kraft pulping (30–150 min) were the subject of this effort. Gel permeation chromatography (GPC) was used to deter- mine the number average molecular weight (Mn), mass average molecular weight (Mw), and polydispersity of the lignin samples. It was shown that the MW of lignins from both feedstocks follow gel degradation theory; that is, at the onset of the kraft pulping process low molecular weightlignins were obtained, and as pulping progressed, the molecular weight peaked and subsequently decreased. An important finding was that acetobromination was shown to be a more effective derivatization technique for carbohydrates containing lignins than acetylation, the technique typically used for derivatization of lignin.

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