scholarly journals Accelerated aging of bio-oil from lignin conversion in subcritical water

TAPPI Journal ◽  
2017 ◽  
Vol 16 (03) ◽  
pp. 123-141 ◽  
Author(s):  
Huyen Nguyen Lyckeskog ◽  
Cecilia Mattsson ◽  
Lars Olausson ◽  
Sven-Ingvar Andersson ◽  
Lennart Vamling ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Aging Process ◽  
Subcritical Water ◽  
Accelerated Aging ◽  
Weight Fraction ◽  
Hydrothermal Liquefaction ◽  
Bio Oil ◽  
Nuclear Magnetic

Accelerated aging of bio-oil derived from lignin was investigated at different aging temperatures (50°C and 80°C) and times (1 hour, 1 day, 1 week, and 1 month). The bio-oil used was produced by the hydrothermal liquefaction of kraft lignin, using phenol as the capping agent, and base (potassium carbonate and potassium hydroxide) and zirconium dioxide as the catalytic system in subcritical water. Elemental composition, molecular weight (by using gel permeation chromatography), and chemical composition (by using gas chromatography–mass spectrometry and 2D nuclear magnetic resonance [18.8 T, DMSO-d6]) of the bio-oil were measured to gain better understanding of the changes that occurred after being subjected to an accelerated aging process. The ligninderived hydrothermal liquefaction bio-oil was quite stable compared with biomass-pyrolysis bio-oil. The yield of the low molecular weight fraction (light oil) decreased from 64.1% to 58.1% and that of tetrahydrofuran insoluble fraction increased from 16.5% to 22.2% after aging at 80°C for 1 month. Phenol and phenolic dimers (Ar–CH2–Ar) had high reactivity compared with other aromatic substituents (i.e., methoxyl and aldehyde groups); these may participate in the polymerization/condensation reactions in the hydrothermal liquefaction bio-oil during accelerated aging. Moreover, the 2D heteronuclear single quantum coherence nuclear magnetic resonance spectra of the high molecular weight fraction (heavy oil) in the aged raw oil in the aromatic region showed that the structure of this fraction was a combination of phenol-alkyl patterns, and the guaiacol cross-peaks of Ar2, Ar5, and Ar6 after aging indicate that a new polymer was formed during the aging process.

scholarly journals Cleavage of the Graft Bonds in PVDF–g–St Films by Boiling Xylene Extraction and the Determination of the Molecular Weight of the Graft Chains

Polymers ◽  
2019 ◽  
Vol 11 (7) ◽  
pp. 1098 ◽  
Author(s):  
Chen ◽  
Seko
Keyword(s):  
Molecular Weight ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Thermal Degradation ◽  
Gel Permeation Chromatography ◽  
Extraction Time ◽  
Gel Permeation ◽  
Irradiation Graft ◽  
Nuclear Magnetic

To determine the molecular weight of graft chains in grafted films, the polystyrene graft chains of PVDF–g–St films synthesized by a pre-irradiation graft method are cleaved and separated by boiling xylene extraction. The analysis of the extracted material and the residual films by FTIR, nuclear magnetic resonance (NMR), and gel permeation chromatography (GPC) analyses indicates that most graft chains are removed from the PVDF–g–St films within 72 h of extraction time. Furthermore, the molecular weight of the residual films decreases quickly within 8 h of extraction and then remains virtually unchanged up to 72 h after extraction time. The degradation is due to the cleavage of graft bonds, which is mainly driven by the thermal degradation and the swelling of graft chains in solution. This allows determination of the molecular weight of graft chains by GPC analysis of the extracted material. The results indicate that the PVDF–g–St prepared in this study has the structure where one or two graft chains hang from each PVDF backbone.

Structural studies of the capsular polysaccharide from Haemophilus pleuropneumoniae serotype 2

1987 ◽  
Vol 65 (5) ◽  
pp. 414-422 ◽  
Author(s):  
Eleonora Altman ◽  
Jean-Robert Brisson ◽  
Malcolm B. Perry
Keyword(s):  
Molecular Weight ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
High Molecular Weight ◽  
Capsular Polysaccharide ◽  
Structural Studies ◽  
High Molecular Weight Polymer ◽  
Molecular Weight Polymer ◽  
Structure Formula ◽  
Nuclear Magnetic

The capsular polysaccharide of Haemophilus pleuropneumoniae serotype 2 (ATCC 27089) is composed of D-glucose (two parts), D-galactose (one part), glycerol (one part), and phosphate (one part). Hydrolysis, dephosphorylation, methylation, enzymic studies, and 1H and 13C nuclear magnetic resonance experiments showed that the polysaccharide is a high molecular weight polymer of a tetrasaccharide repeating units, linked by monophosphate diester and having the following structure:[Formula: see text]

The high molecular weight polyphloroglucinols of the marine brown alga Fucusvesiculosus L. 1H and 13C nuclear magnetic resonance spectroscopy

1985 ◽  
Vol 63 (2) ◽  
pp. 304-313 ◽  
Author(s):  
A. Gavin McInnes ◽  
Mark A. Ragan ◽  
Donald G. Smith ◽  
John A. Walter
Keyword(s):  
Molecular Weight ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Magnetic Resonance Spectroscopy ◽  
Nuclear Magnetic Resonance Spectroscopy ◽  
High Molecular Weight ◽  
Resonance Spectroscopy ◽  
13C Nuclear Magnetic Resonance ◽  
Before And After ◽  
Nuclear Magnetic

1H and 13C nuclear magnetic resonance spectroscopy of the high-molecular-weight (> 104) polyphenol fraction from Fucusvesiculosus, before and after acetylation or methylation, demonstrates that it is composed of phloroglucinol units (48.9 ± 3.5%) and 2,2′,4,4′,6,6′-hexahydroxybiphenyl, 2,2′,2″,4,4′,4″,6,6′,6″-nonahydroxy-1,1′:3′1″-terphenyl, and related quater-and polyphenyl groups (together, 51.1 ± 3.5%) linked by ether bonds, each bond involving the carbinol and methine carbons of different units and the formal loss of a molecule of hydrogen. The polymer is highly branched, with ca. 20 – 22% of the constituent units being chain termini; there is no evidence for large rings of units. Approximately 5 – 10% of the phloroglucinol and 54 – 82% of the directly bonded units occur on the exterior of the molecule, whereas the interior backbone consists predominantly of ether-linked phloroglucinol units.

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