scholarly journals Influence of Reaction Parameters on the Gelation of Silanised Linseed Oil

Materials ◽  
2020 ◽  
Vol 13 (23) ◽  
pp. 5376
Author(s):  
Ewelina Depczyńska ◽  
Waldemar Perdoch ◽  
Bartłomiej Mazela
Keyword(s):  
Molar Mass ◽  
Linseed Oil ◽  
Gel Permeation Chromatography ◽  
Elevated Pressure ◽  
High Reactivity ◽  
Reaction Products ◽  
1H And 13C Nmr ◽  
The Subject ◽  
Silylation Reaction ◽  
Flame Ionisation

The subject of this work was to characterize the catalytic course of the linseed oil silylation reaction with vinyltrimethoxysilane (VTMOS), carried out under elevated pressure and temperature conditions, and an explanation of the reasons for rapid gelation of the reaction product. To explain and describe the process, analytical methods were used, i.e., 1H and 13C NMR (nuclear magnetic resonance), GC-FID (gas chromatography coupled with flame ionisation detection), and GPC (gel permeation chromatography). Reaction products were monitored after 3, 6 and 12 h. The molar mass of the VTMOS-modified oil in only 3 h was comparable with the molar mass of the product obtained by conventional polymerisation. An increase in the reaction time resulted in further transformations resulting from the hydrolysis and condensation reactions taking place. In contrast to reactivity of soybean oil, the silanisation of linseed oil occurred much faster and without the need for cross-linking catalysts. The reason for the high reactivity of linseed oil to VTMOS and rapid gelation of the resulting product was primarily the amount of double bonds present in linseed oil and their high availability, in particular the double bond in the acid linolenic acid located at the C16 carbon.

scholarly journals The Impact of Biomass and Acid Loading on Methanolysis during Two-Step Lignin-First Processing of Birchwood

Catalysts ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 750
Author(s):  
Panos D. Kouris ◽  
Xiaoming Huang ◽  
Xianhong Ouyang ◽  
Dannie J. G. P. van Osch ◽  
Geert J. W. Cremers ◽  
...  
Keyword(s):  
Quantum Coherence ◽  
Gel Permeation Chromatography ◽  
Elevated Pressure ◽  
High Reactivity ◽  
Sugar Release ◽  
Cellulose Pulp ◽  
Biomass Ratio ◽  
Reductive Treatment ◽  
The Impact ◽  
Acid Loading

We optimized the solvolysis step in methanol for two-step lignin-first upgrading of woody biomass. Birchwood was first converted via sulfuric acid methanolysis to cellulose pulp and a lignin oil intermediate, which comprises a mixture of lignin oligomers and C5 sugars in the methanol solvent. The impact of reaction temperature (140–200 °C), acid loading (0.24–0.81 wt%, dry biomass), methanol/biomass ratio (2.3/1–15.8/1 w/w) and reaction time (2 h and 0.5 h) was investigated. At high biomass loadings (ratio < 6.3/1 w/w), operation at elevated pressure facilitates delignification by keeping methanol in the liquid phase. A high degree of delignification goes together to a large extent with C5 sugar release, mostly in the form of methyl xylosides. Gel permeation chromatography and heteronuclear single quantum coherence NMR of lignin fractions obtained at high acid (0.81 wt%) and low biomass (15.8/1 w/w) loading revealed extensive cleavage of β-O-4′ bonds during acidolysis at 180 °C for 2 h. At an optimized methanol/biomass ratio of 2.3/1 w/w and acid loading (0.24 wt%), more β-O-4′ bonds could be preserved, i.e., about 33% after 2 h and 47% after 0.5 h. The high reactivity of the extracted lignin fragments was confirmed by a second hydrogenolysis step. Reductive treatment with Pd/C under mild conditions led to disappearance of ether linkages and molecular weight reduction in the hydrotreated lignin oil.

scholarly journals Molar mass determination of lignins and characterization of their polymeric structures by multi-detector gel permeation chromatography

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Evamaria C. Gaugler ◽  
Wolfgang Radke ◽  
Andrew P. Vogt ◽  
Dawn A. Smith
Keyword(s):  
Molar Mass ◽  
Lithium Bromide ◽  
Gel Permeation Chromatography ◽  
Mass Determination ◽  
Organosolv Lignin ◽  
Gel Permeation ◽  
Softwood Kraft Lignin ◽  
Polymeric Structures

AbstractMolar masses, Mark-Houwink-Sakurada (MHS) exponents, and refractive index increments (dn/dc) for three lignins were determined without derivatization by multi-detector gel permeation chromatography (GPC) in dimethylformamide (DMF) with 0.05 M lithium bromide (LiBr). The lack of effectiveness of fluorescence filters on molar mass determination by GPC-multi-angle laser light scattering (MALS) was confirmed for softwood kraft lignin (Indulin AT) and revealed for mixed hardwood organosolv lignin (Alcell) as well as soda straw/grass lignin (Protobind 1000). GPC with viscometry detection confirmed that these lignins were present as compact molecules. The MHS exponent α for Indulin AT and Alcell was in the order of 0.1. Additionally, the intrinsic viscosity of Protobind 1000 for a given molar mass was much lower than that of either Alcell or Indulin AT. This is the first report of dn/dc values for these three lignins in DMF with 0.05 M LiBr.

scholarly journals An SEM Investigation of the Pozzolanic Activity of a Waste Catalyst from Oil Refinery

2012 ◽  
Vol 18 (S5) ◽  
pp. 75-76
Author(s):  
C. Costa ◽  
P. Marques ◽  
P. A. Carvalho
Keyword(s):  
Zeolite Y ◽  
Active Phase ◽  
Pozzolanic Reaction ◽  
High Reactivity ◽  
Oil Refinery ◽  
Engineering Properties ◽  
Partial Replacement ◽  
Reaction Products ◽  
Fcc Catalyst ◽  
Cement Based Materials

The most active phase of the fluid catalytic cracking (FCC) catalyst, used in oil refinery, is zeolite-Y which is an aluminosilicate with a high internal and external surface area responsible for its high reactivity. Waste FCC catalyst is potentially able to be reused in cement-based materials - as an additive - undergoing a pozzolanic reaction with calcium hydroxide (Ca(OH)2) formed during cement hydration. This reaction produces additional strength-providing reaction products i.e., calcium silicate hydrate (C-S-H) and hydrous calcium aluminates (C-A-H) which exact chemical formula and structure are still unknown. Partial replacement of cement by waste FCC catalyst has two key advantages: (1) lowering of cement production with the associated pollution reduction as this industry represents one of the largest sources of man-made CO2 emissions, and (2) improving the mechanical properties and durability of cement-based materials. Despite these advantages, there is a lack of fundamental knowledge on pozzolanic reaction mechanisms as well as spatial distribution of porosity and solid phases interactions at the microstructural level and consequently their relationship with macroscopical engineering properties of catalyst/cement blends.

Nitroxides as reaction intermediates

1982 ◽  
Vol 60 (12) ◽  
pp. 1414-1420 ◽  
Author(s):  
Hans Gunter Aurich
Keyword(s):  
Electron Spin Resonance ◽  
Electron Spin ◽  
Isopropyl Alcohol ◽  
High Reactivity ◽  
Reaction Intermediates ◽  
Reaction Products ◽  
Nitronyl Nitroxide ◽  
Reaction Conditions ◽  
Spin Resonance ◽  
Secondary Reactions

Vinyl nitroxides 4 are obtained by oxidation of the nitrones 3, as was shown by esr studies and by identification of the reaction products. The formation of 4d–f is even observed in oxidation of the hydroxylamines 1d–f, nitroxides 2d–f and nitrones 3d–f being the intermediates. The high reactivity of the vinyl nitroxides 4 at their β-position is illustrated by the reactions of 4a with various compounds affording the nitroxides 7–10, respectively. Compound 4c reacts with its precursor 3c to give 11, 12, or 13, depending on the reaction conditions. From oxidation of 3a, c, and e the dimerization products 5a, c, and e, respectively, could be isolated. Whereas further oxidation of 5d yields 6d, the acyl nitroxides 14a and c are formed in the oxidation of 5a and c, respectively.The formation of quinone 23 in the reaction of 2-methyl-2-nitrosopropane with potassium tert-butoxide in isopropyl alcohol in the presence of oxygen is discussed. The nitroxide 20 has been detected in the reaction mixture. Imines 24 react with nitrosobenzene giving nitroxides 26. These are further oxidized by nitrosobenzene to afford nitrones 27. Whereas 27a and b could be isolated, 27c and d undergo further reaction yielding the diimines 30c and d along with dinitrone 29.The formation and reactions of imino nitroxides 31 and of the nitronyl nitroxide 41 are discussed. Electron spin resonance studies revealed the high reactivity of the imidazolyl-1,3-dioxides 46 and the imidazolyl-1-oxides 50, which easily form radicals 47–49 and 51, respectively, which are derived from secondary reactions.

scholarly journals Synthesis and Characterization of a Multifunctional Conjugated Polymer

2018 ◽  
Vol 2018 ◽  
pp. 1-9 ◽  
Author(s):  
Emerson C. G. Campos ◽  
Cristiano Zanlorenzi ◽  
Bruno F. Nowacki ◽  
Gabriela M. Miranda ◽  
Denis A. Turchetti ◽  
...  
Keyword(s):  
Conjugated Polymer ◽  
Molar Mass ◽  
Photophysical Properties ◽  
Gel Permeation Chromatography ◽  
Thermal Characterization ◽  
Polymer Structure ◽  
Synthesis And Characterization ◽  
Metallic Ions ◽  
Scanning Calorimetry

This work reports the synthesis and characterization of a conjugated polymer based on fluorene and terpyridine, namely, poly[(9,9-bis(3-((S)-2-methylbutylpropanoate))fluorene-alt-6,6′-(2,2′:6′,2′′-terpyridin-6-yl)] (LaPPS71). The structure was characterized by 1H and 13C nuclear magnetic resonance (NMR) and Fourier-transform infrared (FTIR) spectroscopy. The molar mass was measured by gel permeation chromatography (GPC). As thermal characterization, the glass transition temperature (Tg) was measured by differential scanning calorimetry (DSC). The polymer structure contains two sites capable of complexation with metallic ions, affording the possibility of obtainment of independent or electronically coupled properties, depending on the complexation site. The photophysical properties were fully explored in solution and solid state, presenting ideal results for the preparation of various metallopolymers, in addition to potential application as a metamaterial, due to the presence of the chiral center in the side chains of the polymer.

scholarly journals Effect of PEEK degradation on commingled fabrics consolidation

2021 ◽  
Author(s):  
Lisa Feuillerat ◽  
Olivier De Almeida ◽  
Jean-Charles Fontanier ◽  
Fabrice Schmidt
Keyword(s):  
Melt Spinning ◽  
Molar Mass ◽  
Degradation Kinetics ◽  
Gel Permeation Chromatography ◽  
Raw Material ◽  
High Porosity ◽  
Absorption Bands ◽  
Mass Distributions ◽  
Key Factor ◽  
Lower Molar

The effects of PEEK degradation on consolidation of commingled semi-finished products have been investigated. Two commingled semi-finished products provided by two different suppliers have been studied and compared to a powdered fabric based on the same PEEK grade. Both were manufactured from aligned AS4 carbon and PEEK yarns but the first product referred as the NCF1 has a lower commingling level than the second one identified as the NCF2. Contrary to what could be expected, under the same processing conditions, consolidation of the NCF1 and the NCF2 systematically results in a high porosity content, above 10%. Fourier Transform Infrared spectrophotometry (FTIR) in ATR mode and Gel Permeation Chromatography (GPC) have shown small molecular structure modifications of PEEK yarns compared to the raw material, such as a shift of molar mass distributions towards lower molar mass and the appearance of C-H absorption bands attributed to non-aromatic alkanes. These modifications have been attributed to sizing of PEEK filament. Calorimetric (DSC) and rheological analyses have demonstrated that the presence of sizing in the semi-finished products have huge consequences on the degradation kinetics. The crystallization temperature decreases and the viscosity increases significantly. This acceleration of the degradation kinetics is the reason of the poor consolidation behavior during composite manufacturing. The conditions of melt spinning extrusion under which the neat PEEK is transformed into filament are therefore a key factor of PEEK degradation.

scholarly journals Degradable Polymer Stars Based on Tannic Acid Cores by ATRP

Polymers ◽  
2019 ◽  
Vol 11 (5) ◽  
pp. 752 ◽  
Author(s):  
Julia Cuthbert ◽  
Saigopalakrishna S. Yerneni ◽  
Mingkang Sun ◽  
Travis Fu ◽  
Krzysztof Matyjaszewski
Keyword(s):  
Tannic Acid ◽  
Molar Mass ◽  
Gel Permeation Chromatography ◽  
Degradable Polymers ◽  
Degradable Polymer ◽  
Cytotoxicity Assays ◽  
Before And After ◽  
Phenolic Esters ◽  
Ft Ir ◽  
Waste Accumulation

Degradable polymers are crucial in order to reduce plastic environmental pollution and waste accumulation. In this paper, a natural product, tannic acid was modified to be used as a polymer star core. The tannic acid was modified with atom transfer radical polymerization (ATRP) initiators and characterized by 1H NMR, FT-IR, and XPS. Twenty-five arm polymer stars were prepared by photoinduced ATRP of poly(methyl methacrylate) (PMMA) or poly(oligo(ethylene oxide) methacrylate) (molar mass Mw = 300 g/mol) (P(OEO300MA)). The polymer stars were degraded by cleaving the polymer star arms attached to the core by phenolic esters under mild basic conditions. The stars were analyzed before and after degradation by gel permeation chromatography (GPC). Cytotoxicity assays were performed on the P(OEO300MA) stars and corresponding degraded polymers, and were found to be nontoxic at the concentrations tested.

scholarly journals Alendronate Release from UHMWPE-Based Biomaterials in Relation to Particle Size of the GUR Powder for Manufacturing

Materials ◽  
2019 ◽  
Vol 12 (11) ◽  
pp. 1832
Author(s):  
Michael Seidenstuecker ◽  
Julia Weber ◽  
Sergio H. Latorre ◽  
Brigitte Straub ◽  
Ulrich Matthes ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Particle Size ◽  
Strong Influence ◽  
Molar Mass ◽  
Negative Influence ◽  
Release Behavior ◽  
Elongation At Break ◽  
Continuous Release ◽  
The Subject ◽  
Ultra High Molecular Weight

Ultra-high molecular weight polyethylene (UHMWPE) is widely used in endoprosthetics and has been the subject of countless studies. This project investigates the dependence of alendronate (AL) release on the molecular weight of the UHMWPE used (GUR1020 and GUR1050). A 0.5 wt% AL was added to the UHMWPE during the production of the moldings. In addition to the 14-day release tests, biocompatibility tests such as live dead assay, cell proliferation assay (WST) and Lactate dehydrogenase test (LDH) with MG-63 cells as well as a tensile test according to DIN EN ISO 527 were carried out. The released AL concentration was determined by HPLC. A continuous release of the AL was observed over the entire period of 2 weeks. In addition, a correlation between molar mass and AL release was demonstrated. The GUR1020 showed a release four times higher than the GUR1050. Both materials have no negative influence on the proliferation of MG-63 cells. This was also confirmed in the live/dead assay by the increase in cell count. No cytotoxicity was detected in the LDH test. The addition of 0.5 wt% AL increased the elongation at break for GUR1020 by 23% and for GUR1050 by 49%. It was demonstrated that the choice of UHMWPE has an influence on the release of AL. The particle size in particular has a strong influence on the release behavior.

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