scholarly journals Preparation and Stabilization of High Molecular Weight Poly (acrylonitrile-co-2-methylenesuccinamic acid) for Carbon Fiber Precursor

Polymers ◽  
2021 ◽  
Vol 13 (22) ◽  
pp. 3862
Author(s):  
Shuxian Zhang ◽  
Yanjin Dang ◽  
Xuepeng Ni ◽  
Chunshun Yuan ◽  
Huifang Chen ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Carbon Fiber ◽  
High Performance ◽  
Gel Permeation Chromatography ◽  
Reactivity Ratio ◽  
Exothermic Peak ◽  
Scanning Calorimetry ◽  
Monomer Feed ◽  
Poly Acrylonitrile ◽  
Carbon Fiber Precursor

Bifunctional comonomer 2-methylenesuccinamic acid (MLA) was designed and synthesized to prepare acrylonitrile copolymer P (AN-co-MLA) using mixed solvent polymerization as a carbon fiber precursor. The effect of monomer feed ratios on the structure and stabilization were characterized by elemental analysis (EA), Fourier transform infrared spectroscopy (FTIR), gel permeation chromatography (GPC), X-ray diffraction (XRD), proton nuclear magnetic (1H NMR), and differential scanning calorimetry (DSC) for the P (AN-co-MLA) copolymers. The results indicated that both the conversion and molecular weight of polymerization reduce gradually when the MLA content is increased in the feed and that bifunctional comonomer MLA possesses a larger reactivity ratio than acrylonitrile (AN). P (AN-co-MLA) shows improved stabilization compared to the PAN homopolymer and poly (acrylonitrile-acrylic acid-methacrylic acid) [P (AN-AA-MA)], showing features such as lower initiation temperature, smaller cyclic activation energy, wider exothermic peak, and a larger stabilization degree, which are due to the ionic cyclization reaction initiated by MLA, confirming that the as-prepared P (AN-co-MLA) is the potential precursor for high-performance carbon fiber.

scholarly journals Synthesis, spinning, and properties of very high molecular weight poly(acrylonitrile-co-methyl acrylate) for high performance precursors for carbon fiber

Polymer ◽  
2014 ◽  
Vol 55 (25) ◽  
pp. 6471-6482 ◽  
Author(s):  
E. Ashley Morris ◽  
Matthew C. Weisenberger ◽  
Stephanie B. Bradley ◽  
Mohamed G. Abdallah ◽  
Sue J. Mecham ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Carbon Fiber ◽  
High Molecular Weight ◽  
Methyl Acrylate ◽  
High Performance ◽  
Poly Acrylonitrile ◽  
Very High ◽  
High Molecular Weight Poly

Synthesis and characterization of novel methacrylate copolymers having pendant piperonyl group: monomer reactivity ratio, thermal degradation kinetics, and biological activity

2021 ◽  
Vol 29 (9_suppl) ◽  
pp. S1432-S1445
Author(s):  
Ibrahim Erol ◽  
Bayram Gencer ◽  
Zeki Gurler
Keyword(s):  
Biological Activity ◽  
Degradation Kinetics ◽  
Gel Permeation Chromatography ◽  
Reactivity Ratio ◽  
Thermal Degradation Kinetics ◽  
Scanning Calorimetry ◽  
Molecular Weights ◽  
Monomer Reactivity Ratio ◽  
Bacteria And Fungi ◽  
Photo Stability

In this study, 2-{[(2H-1,3-benzodioxol-5-yl)methyl]amino}-2-oxoethyl 2-methylprop-2-enoate (BMAOME) monomer was synthesized, and copolymers were prepared with glycidyl methacrylate (GMA). Structural characterizations of the compounds were performed using FTIR, 1H-, and 13C-NMR techniques. Monomer reactivity ratio values were calculated by Finemann–Ross (FR) and Kelen–Tudos (KT) methods. The Tg value of the polymers was determined by differential scanning calorimetry (DSC) and their thermal stability was determined by thermogravimetric analysis (TGA). The molecular weights (w and n) and polydispersity index of the polymers were determined by gel permeation chromatography. The Ea value of thermal decomposition was determined by using the Ozawa and Kissinger methods. The photo-stability of the copolymers was investigated. Furthermore, the photo-stability of the copolymers and the biological activity of polymers against different types of bacteria and fungi were investigated.

scholarly journals Poly(lactic acid) polymer stars built from early generation dendritic polyols

2013 ◽  
Vol 91 (6) ◽  
pp. 392-397 ◽  
Author(s):  
Genny E. Keefe ◽  
Jean-d'Amour K. Twibanire ◽  
T. Bruce Grindley ◽  
Michael P. Shaver
Keyword(s):  
Molecular Weight ◽  
Ring Opening ◽  
Gel Permeation Chromatography ◽  
Poly Lactic Acid ◽  
Reactive Site ◽  
Scanning Calorimetry ◽  
Early Generation ◽  
Sequential Reaction ◽  
Cyclic Esters ◽  
Total Molecular Weight

A family of polymer stars has been prepared from early generation dendritic cores with four, six, and eight arms. Four dendritic cores were prepared from the sequential reaction of a multifunctional alcohol with a protected anhydride, followed by deprotection to afford two or three new alcohol functionalities per reactive site. These cores were used as initiators for the tin-catalyzed ring-opening polymerization of l-lactide and rac-lactide to afford isotactic and atactic degradable stars, respectively. Two series of stars were prepared for each monomer, either maintaining total molecular weight or number of monomer units per arm. The polymers were characterized by NMR spectroscopy, light-scattering gel-permeation chromatography, differential scanning calorimetry, and thermogravimetric analysis. Our results support previous work that suggests that the length of the arms dictates thermal properties rather than the total molecular weight of the star. Little effect was noted between aromatic and aliphatic cores, presumably due to the flexibility of the rest of the core molecule. We have shown that early generation dendrimers can serve as excellent core structures for building core-first polymer stars via the ring-opening of cyclic esters.

scholarly journals Methylene-Bridged Tridentate Salicylaldiminato Binuclear Titanium Complexes as Copolymerization Catalysts for the Preparation of LLDPE through [Fe]/[Ti] Tandem Catalysis

Polymers ◽  
2019 ◽  
Vol 11 (7) ◽  
pp. 1114 ◽  
Author(s):  
Yani Luo ◽  
Jian Li ◽  
Derong Luo ◽  
Qingliang You ◽  
Zifeng Yang ◽  
...  
Keyword(s):  
Molecular Weight ◽  
High Temperature ◽  
Gel Permeation Chromatography ◽  
13C Nmr Spectroscopy ◽  
Molar Ratio ◽  
Tandem Catalysis ◽  
Titanium Complexes ◽  
Scanning Calorimetry ◽  
Molecular Weights ◽  
Branching Degree

A novel tandem catalysis system consisted of salicylaldiminato binuclear/mononuclear titanium and 2,6-bis(imino)pyridyl iron complexes was developed to catalyze ethylene in-situ copolymerization. Linear low-density polyethylene (LLDPE) with varying molecular weight and branching degree was successfully prepared with ethylene as the sole monomer feed. The polymerization conditions, including the reaction temperature, the Fi/Ti molar ratio, and the structures of bi- or mononuclear Ti complexes were found to greatly influence the catalytic performances and the properties of obtained polymers. The polymers were characterized by differential scanning calorimetry (DSC), high temperature gel permeation chromatography (GPC) and high temperature 13C NMR spectroscopy, and found to contain ethyl, butyl, as well as some longer branches. The binuclear titanium complexes demonstrated excellent catalytic activity (up to 8.95 × 106 g/molTi·h·atm) and showed a strong positive comonomer effect when combined with the bisiminopyridyl Fe complex. The branching degree can be tuned from 2.53 to 22.89/1000C by changing the reaction conditions or using different copolymerization pre-catalysts. The melting points, crystallinity and molecular weights of the products can also be modified accordingly. The binuclear complex Ti2L1 with methylthio sidearm showed higher capability for comonomer incorporation and produced polymers with higher branching degree and much higher molecular weight compared with the mononuclear analogue.

scholarly journals Analysis of the Degradation During Melt Processing of PLA/Biosilicate® Composites

2019 ◽  
Vol 3 (2) ◽  
pp. 52 ◽  
Author(s):  
Eduardo H. Backes ◽  
Laís de N. Pires ◽  
Lidiane C. Costa ◽  
Fabio R. Passador ◽  
Luiz A. Pessan
Keyword(s):  
Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Melt Processing ◽  
Poly Lactic Acid ◽  
Processing Route ◽  
Mechanical Resistance ◽  
Scanning Calorimetry ◽  
Oxidative Reactions ◽  
Bioactive Composites ◽  
Internal Mixer

Poly (lactic acid) (PLA)/bioactive composites are emerging as new biomaterials since it is possible to combine stiffness, mechanical resistance, and bioactive character of the bioglasses with conformability and bioabsorption of the PLA. In this study, PLA/Biosilicate® composites were prepared using a melt-processing route. The processability and properties were evaluated aiming to produce composites with bioactive properties. Two different PLA (PLA 2003D and PLA 4043D) were tested with the addition of 1 wt. % of Biosilicate®. Both materials presented a huge reduction in melt viscosity after internal mixer processing. The degradation effects of the addition of Biosilicate® in the PLAs matrices were evaluated using zeta potential tests that showed a very high liberation of ions, which catalyzes PLA thermo-oxidative reactions. To understand the extension of degradation effects during the processing, the composites were characterized using thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), gel permeation chromatography (GPC), and rheological tests. GPC results showed that PLA with the lowest residual acid content (RAC), PLA 2003D, presented higher thermal stability, higher molecular weight, and viscosity baseline compared to PLA 4043D. The composites showed a significant decrease in molecular weight for both PLA with the addition of Biosilicate®. TGA results showed that Biosilicate® might have reduced the activation energy to initiate thermodegradation reactions in PLAs and it occasioned a reduction in the Tonset by almost 40 °C. The DSC results showed that severe matrix degradation and the presence of bioglass did not significantly affect glass transition temperature (Tg), melting temperature (Tm) and crystallinity of PLAs, but it influenced cold crystallization peak (Tcc). In this way, the type of PLA used influences the processability of this material, which can make the production of filaments of this material for 3D printing unfeasible.

scholarly journals Fractionation of lignosulphonates released during the early stages of delignification

1983 ◽  
Vol 61 (2) ◽  
pp. 416-420 ◽  
Author(s):  
Norman G. Lewis ◽  
David A. I. Goring ◽  
Alfred Wong
Keyword(s):  
Molecular Weight ◽  
High Performance ◽  
Black Spruce ◽  
Gel Permeation Chromatography ◽  
Bimodal Distribution ◽  
High Yield ◽  
Low Molecular Weight ◽  
Lower Yield ◽  
Spruce Wood ◽  
Gel Permeation

High-yield spent bisulphite liquor (HY-SBL) from sulphonated black spruce wood (Piceamariana) was fractionated by gel permeation chromatography (GPC) and by high-performance liquid chromatography (HPLC). The GPC fractionation gave a wide bimodal distribution, whereas with HPLC, a more detailed resolution was seen with the bulk of the fraction giving several clearly defined peaks. The paucidisperse material was further concentrated by a bulk fractionation of the crude SBL which included complexing the lignosulphonates with dicyclohexylamine. The isolated paucidisperse material was found to be dialyzable and to constitute 90% of the lignosulphonate in the sample of SBL. If the bisulphite pulp obtained was recooked in fresh acid sulphite liquor to a lower yield, most of the lignosulphonate dissolved was widely polydisperse with no indication of the discrete components resolvable by HPLC. However, 25% of the lignin made soluble was in the form of the paucidisperse fractions. In all, we were able to obtain about 50% of the lignin in spruce wood as a relatively low molecular weight lignosulphonate resolvable into discrete fractions by HPLC.

Purification and characterization of kraft lignin

Holzforschung ◽  
2015 ◽  
Vol 69 (8) ◽  
pp. 943-950 ◽  
Author(s):  
Wenwen Fang ◽  
Marina Alekhina ◽  
Olga Ershova ◽  
Sami Heikkinen ◽  
Herbert Sixta
Keyword(s):  
Thermal Properties ◽  
High Performance ◽  
Inorganic Compounds ◽  
Gel Permeation Chromatography ◽  
Kraft Lignin ◽  
Hot Water ◽  
Scanning Calorimetry ◽  
Target Values ◽  
Lower Glass Transition Temperature

Abstract To upgrade the utilization of kraft lignin (KL) for high-performance lignin-based materials (e.g., carbon fiber), the purity, molecular mass distribution (MMD), and thermal properties need to be improved and adjusted to target values. Therefore, different methods, such as ultrasonic extraction (UE), solvent extraction, dialysis, and hot water treatment (HWT), were applied for the purification of KL. The chemical and thermal properties of purified lignin have been characterized by nuclear magnetic resonance, Fourier transform infrared, gel permeation chromatography, elemental analysis, differential scanning calorimetry, and thermogravimetric analysis. The lignin fractions obtained by UE with ethanol/acetone (E/A) mixture (9:1) revealed a very narrow MMD and were nearly free of inorganic compounds and carbohydrates. Further, the E/A-extracted lignin showed a lower glass transition temperature (Tg) and a clearly detectable melting temperature (Tm). Dialysis followed by HWT at 220°C is an efficient method for the removal of inorganics and carbohydrates; however, lignin was partly forming condensed structures during the treatment.

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