Comparative Study of Two Types of Alkali Lignin from Different Origin

2011 ◽  
Vol 299-300 ◽  
pp. 747-750
Author(s):  
Li Hong Zhao ◽  
Hong Jun Sun
Keyword(s):  
Functional Groups ◽  
Chemical Characterization ◽  
Gel Permeation Chromatography ◽  
Proton Nuclear Magnetic Resonance ◽  
Alkali Lignin ◽  
H Nmr ◽  
Physico Chemical ◽  
Ft Ir ◽  
L1 And L2 ◽  
Different Origin

The physico-chemical characterization of two types of alkali lignin from different origin, namely L1 and L2, were studied by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance spectrometry (1H NMR) and gel permeation chromatography (GPC) analysis. FT-IR spectra show that they have the characteristics of absorption peaks of syringyl and guaiacyl. 1H NMR spectra indicate that acetylated L1 exhibits higher content of aromatic protons than L2, as the former is mainly composed by G units. L2 presents high quantities of methoxyl groups. GPC results show that L1 has much higher weight average than L2. They had similar functional groups, however, there were differences in the relative contents of functional groups.

scholarly journals Isolation and physico-chemical characterization of lignins from ultrasound irradiated fast-growing poplar wood

BioResources ◽  
2010 ◽  
Vol 6 (1) ◽  
pp. 414-433
Author(s):  
Tong-Qi Yuan ◽  
Shaoni Sun ◽  
Feng Xu ◽  
Run-Cang Sun
Keyword(s):  
Chemical Characterization ◽  
Gel Permeation Chromatography ◽  
Populus Tomentosa ◽  
Poplar Wood ◽  
Fast Growing ◽  
Organosolv Lignin ◽  
Physico Chemical ◽  
Populus Tomentosa Carr ◽  
Ft Ir

Ultrasonic irradiation with organic solvents and alkaline extractions were carried out on a fast-growing poplar wood, triploid of Populus tomentosa Carr., in an attempt to develop efficient lignin isolation procedures. Four organosolv and three alkaline lignin fractions were successively isolated and comparatively characterized by sugar analysis, alkaline nitrobenzene oxidation, gel permeation chromatography (GPC), Fourier transform infra-red spectroscopy (FT-IR), quantitative 13C, and 2D HSQC nuclear magnetic resonance (NMR) spectroscopy, as well as thermogravimetric analysis (TGA). The results showed that the ultrasonic treatments and sequential extractions with three different concentrations of NaOH led to a release of 90.9% of the original lignin. The four organosolv lignin preparations obtained under the ultrasound-assisted extractions were degraded significantly and contained more carbohydrate and non-condensed syringyl units when compared to the three alkaline lignin preparations. Furthermore, the analyses confirmed that L5, the lignin preparation with the highest yield (44.6% of the original lignin), was partially acylated at the γ-carbon of the side-chain preferentially over syringyl units. The percentage of lignin acylation of β-O-4’ linkages was about 14%. The amount of β-O-4’, β-β’, and –OCH3 were estimated to be about 0.31/Ar, 0.06/Ar, and 1.73/Ar, respectively. The ratio of S/G was calculated to be 2.0.

Cellulose triacetate from different sources: modification assessment through thermal and chemical characterization

Holzforschung ◽  
2020 ◽  
Vol 74 (5) ◽  
pp. 505-512 ◽  
Author(s):  
Lucca C. Malucelli ◽  
Diego Lomonaco ◽  
Marco A.S.C. Filho ◽  
Washington L.E. Magalhães
Keyword(s):  
Chemical Characterization ◽  
Cellulose Triacetate ◽  
Industrial Applications ◽  
Proton Nuclear Magnetic Resonance ◽  
Common Source ◽  
Cellulose Derivatives ◽  
Cellulose Content ◽  
H Nmr ◽  
Ft Ir ◽  
Different Sources

AbstractModification techniques have been widely employed to improve cellulose properties, thus increasing the diversity of industrial applications. While wood pulp cellulose is the most common source for industrial production, little has been studied about the effects of the cellulose source and its purity on modification. Therefore, this article investigates the influence of cellulose source (e.g. wood or cotton) on its modification (acetylation), by estimating the obtained degree of substitution (DS) through Fourier-transform infrared (FT-IR), proton nuclear magnetic resonance (1H NMR) and back titration. The intense reduction in samples’ crystallinity after acetylation was a result of breakage of inter- and intra-molecular hydrogen bonds, thus confirming acetylation. Although Avicel showed the highest cellulose content and was virtually free of hemicellulose and lignin, this did not affect the acetylation degree, as all samples were successfully triacetylated. The techniques used in this study were ideal for detecting acetylation and estimating the DS, which makes them good tools for modification studies of cellulose derivatives.

A light-colored hydroxypropyl sulfonated alkali lignin for utilization as a dye dispersant

Holzforschung ◽  
2016 ◽  
Vol 70 (2) ◽  
pp. 109-116 ◽  
Author(s):  
Yanlin Qin ◽  
Wenjie Mo ◽  
Lixuan Yu ◽  
Dongjie Yang ◽  
Xueqing Qiu
Keyword(s):  
Gel Permeation Chromatography ◽  
Heat Stability ◽  
Proton Nuclear Magnetic Resonance ◽  
Hydroxyl Groups ◽  
Crosslinking Reaction ◽  
Sodium Lignosulfonate ◽  
Alkali Lignin ◽  
H Nmr ◽  
Light Yellow ◽  
Reaction Processes

Abstract A light-colored hydroxypropyl sulfonated alkali lignin (HSAL) was synthesized based on pine alkali lignin (AL) by grafted-sulfonation and crosslinking reaction processes. The reactions were evaluated by gel-permeation chromatography (GPC), infrared (IR) and proton nuclear magnetic resonance (1H-NMR) spectroscopy. The sulfonic group content and the molecular weight (Mw) of HSAL significantly increased, while the phenolic hydroxyl groups diminished by around 80% compared to AL. The color of HSAL turned to light yellow compared to the dark brown color of AL, that is, it stained less the fiber. The dispersity, heat stability, and dye uptake of dye bath with HSAL was significantly improved compared to sodium lignosulfonate, sulfomethylated AL, and dispersants of the naphthalene series.

Enhanced Thermal Stability of Esterified Lignin in Different Solvent Mediums

2018 ◽  
Vol 9 (1) ◽  
pp. 39-49 ◽  
Author(s):  
Sharifah Nurul Ain Syed Hashim ◽  
Sarani Zakaria ◽  
Chin Hua Chia ◽  
Sharifah Nabihah Syed Jaafar
Keyword(s):  
Thermal Stability ◽  
Alkaline Solution ◽  
Room Temperature ◽  
Hydroxyl Groups ◽  
Aqueous Alkaline Solution ◽  
Alkali Lignin ◽  
Weight Percentage ◽  
H Nmr ◽  
Ft Ir ◽  
Thermal Stability Of

In this study, soda alkali lignin from oil palm empty fruit bunch (EFB-AL) and kenaf core (KC-AL) are esterified with maleic anhydride under two different conditions, namely i) pyridine at temperature of 120°C for 3h and ii) aqueous alkaline solution at room temperature for 4h. As a result, the weight percentage gain (WPG) of the esterified EFB-AL (EFB-EL) and esterified KC-AL (KC-EL) in pyridine demonstrated a higher compared to aqueous alkaline solution. The FT-IR results of EFB-EL and KC-EL in both solvents exhibited some changes at the carbonyl and hydroxyl groups. Furthermore, the esterification process induced the carboxylic peak to appear in both alkali lignin samples. The outcome is confirmed by conducting H-NMR analysis, which demonstrated ester and carboxylic acid peaks within the spectral analysis. Finally, the TGA results showed both EFB-EL and KC-EL that are exposed to aqueous alkaline actually possessed better thermal stability and higher activation energy (Ea) compared to the esterified samples in pyridine.

Synthesis of Macromolecular Coupling Agent and its Effects on Polystyrene Composites

2014 ◽  
Vol 1053 ◽  
pp. 268-275
Author(s):  
Hong Wen Zhang ◽  
Shi Long Zhou ◽  
Yang Zhang ◽  
Yan Jiang ◽  
Qiang Yu
Keyword(s):  
Composite Materials ◽  
Gel Permeation Chromatography ◽  
Ultraviolet Spectrum ◽  
Butyl Methacrylate ◽  
Coupling Agents ◽  
Resonance Spectroscopy ◽  
H Nmr ◽  
Comprehensive Performance ◽  
Ft Ir ◽  
The Impact

Different molecular weight of block coupling agents with well-defined structures have been synthesized successfully by atom transfer radical polymerization (ATRP) from styrene (St), butyl methacrylate (BMA) and 3-methoxyacryloyl-propyltrimethoxyl silicon (KH-570) are as monomer. The structures and compositions of macromolecular coupling agents have been characterized by means of infrared spectrum (FT-IR), ultraviolet spectrum (UV), nuclear magnetic resonance spectroscopy (1H-NMR) and gel permeation chromatography (GPC). And their effects on the polystyrene/silica (PS/SiO2) composite materials have been studied. The results show that interface compatibility and mechanical properties of composite materials containing macromolecule coupling agents are improved significantly. The composite materials with block macromolecular coupling agents possess more excellent comprehensive performance. Furthermore, the impact strength increased by 110% when comparing with composite materials which are not modified by the coupling agents.

Cationic copolymerization of 1,3-pentadiene with α-pinene

2014 ◽  
Vol 34 (7) ◽  
pp. 583-589 ◽  
Author(s):  
Ai-Yuan Li ◽  
Xiang-Dong Sun ◽  
Hui-Bo Zhang ◽  
Yong-Chun Zhang ◽  
Bin Wang ◽  
...  
Keyword(s):  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Polymerization Temperature ◽  
Scanning Calorimetry ◽  
Gardner Color ◽  
H Nmr ◽  
Cationic Copolymerization ◽  
Ft Ir ◽  
Better Than ◽  
C Nmr

Abstract The cationic copolymerization of 1,3-pentadiene (PD) with α-pinene (AP) initiated by aluminum trichloride (AlCl3) was carried out in N-pentane solvent. The effects of the polymerization temperature and the comonomer composition on the yield of the copolymer, softening point, Gardner color scale and number-average molecular weight (Mn) are discussed. The performance of the copolymer was better than that of AP homopolymer (PAP) and PD homopolymer (PPD). The structure of the copolymer was characterized by Fourier transform infrared spectroscopy (FT-IR), 1H-nuclear magnetic resonance (1H-NMR), 13C-NMR, differential scanning calorimetry (DSC) and gel permeation chromatography (GPC). In addition, the reactivity ratios for AP (M1) and PD (M2) determined by the Kelen-Tudos method from low-conversion data are r1=0.58 and r2=5.92, respectively.

Halogenated sunflower oil as a precursor for synthesis of polysulfide polymer

e-Polymers ◽  
2016 ◽  
Vol 16 (1) ◽  
pp. 33-39 ◽  
Author(s):  
Samira Moqadam ◽  
Mehdi Salami-Kalajahi
Keyword(s):  
Sunflower Oil ◽  
Proton Nuclear Magnetic Resonance ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
X Ray ◽  
H Nmr ◽  
Ft Ir ◽  
Harsh Conditions ◽  
Thermal Stability Of ◽  
Polysulfide Polymer

AbstractPolysulfide polymers usually are prepared by the reaction of different dihalide compounds with disodium polysulfides. In this field, dihalides are expensive and produced from halogenation of organic compounds by different methods with harsh conditions. To overcome this problem, in this work, sunflower oil as polyunsaturated oil was used as precursor to produce polyhalide compound. In this field, double bonds of oil were applied as functional groups to halogenate the sunflower via benzoyl peroxide-catalyzed reaction with hydrochloric acid. Also, Na2S3 was synthesized via the reaction between sulfur and sodium hydroxide. Then, halogenated oil was reacted with Na2S3 to produce sunflower oil-based polysulfide polymer. Fourier transform infrared spectroscopy (FT-IR) and proton nuclear magnetic resonance (1H NMR) were used to characterize the structure of sunflower oil and synthesized polysulfide polymer. The content of halogenation was also obtained via energy-dispersive X-ray spectroscopy (EDX). Thermal stability of synthesized polymer was determined by means of thermal gravimetric analysis (TGA) and glass transition temperature was investigated by differential scanning calorimetry (DSC).

Reduction-Degradable Shell Cross-Linked Micelle with pH-Responsive Cores Prepared via Click Chemistry

2016 ◽  
Vol 848 ◽  
pp. 527-531
Author(s):  
Lu Bin Lin ◽  
Qing Yun Yu ◽  
Zhuo Qun Gu ◽  
Xiao Ze Jiang ◽  
Mei Fang Zhu
Keyword(s):  
Click Chemistry ◽  
Self Assembly ◽  
Gel Permeation Chromatography ◽  
Proton Nuclear Magnetic Resonance ◽  
Poly Ethylene Glycol ◽  
H Nmr ◽  
Transmission Electron ◽  
Assembly Behavior ◽  
Poly Ethylene ◽  
Novel Drug

A well-defined poly [(ethylene glycol)-block-2-(dimethylamino) ethyl methacrylate-block-2-(diethylamino) methacrylate] (PEG-b-DMA-b-DEA) triblock copolymer was synthesized via atom transfer radical polymerization (ATRP) by successively polymerization of DMA and DEA monomers using a PEG-based macroinitiator, and obtained copolymer was then converted to be PEG-b-P(DMA-co-QDMA)-b-PDEA copolymer with “clickable” moieties in the middle block by the quaternization with propargyl bromide. Those copolymers prepared were characterized by proton Nuclear Magnetic Resonance (1H NMR) and Gel Permeation Chromatography (GPC), and its self-assembly behavior and subsequently fixation with bis-(azidoethyl) disulfide via click chemistry resulting reduction-sensitive shell-cross-linked (SCL) micelle in purely aqueous solution were investigated by Transmission Electron Microscopy (TEM) and Dynamic Light Scattering (DLS). The results show the micellar structure could be effectively cross-linked via click chemistry and also be dissociated at reduction condition, which may realize it's potential application as novel drug delivery carriers.

Quantitative Analysis of Polyacrylamide Grafted on Polylactide Film Surfaces Employing Spectroscopic Techniques

2017 ◽  
Vol 71 (11) ◽  
pp. 2457-2468
Author(s):  
Mijanur Rahman ◽  
Pakorn Opaprakasit
Keyword(s):  
Quantitative Analysis ◽  
Proton Nuclear Magnetic Resonance ◽  
Spectroscopic Techniques ◽  
H Nmr ◽  
Initiator System ◽  
Ft Ir ◽  
Time Ease ◽  
Standard Techniques ◽  
Good Agreement ◽  
Ft Ir Spectroscopy

Standard techniques for quantitative measurement of polyacrylamide (PAm) contents grafted on polylactide (PLA) film substrates, P(LA- g-Am- co-MBAm), which are commonly used as cell culture substrates or scaffolds, and pH-sensitive absorbents have been developed with X-ray photoelectron (XPS), proton-nuclear magnetic resonance (1H-NMR), and Fourier transform infrared (FT-IR) spectroscopy. The techniques are then applied to examine P(LA- g-Am- co-MBAm) samples prepared from two separate photo-initiator/co-initiator systems. Efficiency and accuracy of the techniques are compared. The results from all techniques are in good agreement, indicating high analysis precisions, although FT-IR technique provides additional advantages, in terms of short analysis time, ease of sample preparation, and accessibility of a machine. The results indicate that the riboflavin (RF) initiator system has higher grafting efficiency than its camphorquinone (CQ) counterpart. These standard techniques can be applied in the analysis of these materials and further modified for quantitative analysis of other grafting systems.

Characterization of Epoxidized Rubber Seed Oil

2017 ◽  
Vol 728 ◽  
pp. 295-300
Author(s):  
Jutamas Kantee ◽  
Somjai Kajorncheappunngam
Keyword(s):  
Seed Oil ◽  
Proton Nuclear Magnetic Resonance ◽  
Epoxide Ring ◽  
Rubber Seed Oil ◽  
Spectra Analysis ◽  
Rubber Seed ◽  
H Nmr ◽  
Infrared Spectrometer ◽  
Ft Ir

Epoxidation of rubber seed oil was carried out using a peroxyacid generated in situ from glacial acetic acid and hydrogen peroxide to produce epoxidized rubber seed oil. The maximum relative conversion to oxirane of 88 % could be obtained at 60 °C after a reaction time of 7 hours. The presence of oxirane ring of epoxidized rubber seed oil was confirmed by fourier transform infrared spectrometer (FT-IR) and proton nuclear magnetic resonance (1H NMR) spectra analysis which displayed a disappearance of double bonds peak in rubber seed oil and an existing of epoxide ring peak in epoxidized rubber seed oil.

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