scholarly journals Thermal Analysis and Crystal Structure of Poly(Acrylonitrile-Co-Itaconic Acid) Copolymers Synthesized in Water

Polymers ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 221
Author(s):  
Hailong Zhang ◽  
Ling Quan ◽  
Aijun Gao ◽  
Yuping Tong ◽  
Fengjun Shi ◽  
...  

The composition and structure of polyacrylonitrile (PAN) precursors play an important role during thermal stabilization, which influences the properties of the resulting carbon fibers. In this paper, PAN homopolymer and PAN-itaconic (IA) copolymers with different IA contents were synthesized by aqueous phase precipitation polymerization. The effects of IA content on the structure and thermal properties were studied using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). The morphology of PAN polymers showed that the average size of the PAN particles increased with the increase of IA content in the feed. The content of the IA comonomer on the copolymers was quantitatively characterized by the relative absorbance intensity (A1735/A2243) in FTIR spectrum. With the increase of IA content in the feed, PAN-IA copolymers exhibited lower degree of crystallinity and crystal size than the control PAN homopolymer. The results from DSC curves indicated that PAN-IA1.0 copolymers had lower initial exothermic temperature (192.4 °C) and velocity of evolving heat (6.33 J g−1 °C−1) in comparison with PAN homopolymer (Ti = 238.1 °C and ΔH/ΔT = 34.6 J g−1 °C−1) in an air atmosphere. TGA results suggested that PAN-IA1.0 copolymers had higher thermal stability than PAN homopolymer, which can form a ladder structure easier during thermal processing. Therefore, PAN-IA1.0 copolymers would be a suitable candidate for preparing high performance PAN based carbon fibers.

2019 ◽  
Vol 89 (23-24) ◽  
pp. 4959-4966 ◽  
Author(s):  
AM Ali ◽  
HM El-Dessouky

Polylactic acid (PLA) fibers are receiving growing interest as one of the recent innovative materials being developed for various applications. The inherent biodegradability of PLA makes it highly attractive for the biomedical and health care sectors. PLA fibers need to be partially and/or highly oriented to allow high performance and readiness for a wide range of manufacturability. In this study, the structure and properties of PLA fibers, manufactured at different spinning speeds, were studied. Laser diffractometry, polarized light microscopy, differential scanning calorimetry (DSC) and X-ray diffraction (XRD) were used to determine the diameter, birefringence, molecular orientation, enthalpy and degree of crystallinity of as-spun and drawn PLA fibers. The results of DSC and XRD showed that the degree of crystallinity of the PLA fibers is significantly improved for the drawn PLA fibers compared to the as-spun fibers and leveled off in the case of changing the take-up speeds of drawn fibers.


Polymers ◽  
2019 ◽  
Vol 11 (7) ◽  
pp. 1150 ◽  
Author(s):  
Huichao Liu ◽  
Shuo Zhang ◽  
Jinglong Yang ◽  
Muwei Ji ◽  
Jiali Yu ◽  
...  

The quality of polyacrylonitrile (PAN) precursor has a great influence on the properties of the resultant carbon fibers. In this paper, a novel comonomer containing the sulfonic group, 2-acrtlamido-2-methylpropane acid (AMPS), was introduced to prepare P(AN-co-AMPS) copolymers using itaconic acid (IA) as the control. The nanofibers of PAN, P(AN-co-IA), and P(AN-co-AMPS) were prepared using the electrospinning method. The effect of AMPS comonomer on the carbon nanofibers was studied using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA) and Raman spectrum. The structural evolutions of PAN-based nanofibers were quantitatively tracked by FTIR and XRD during the thermal oxidative stabilization (TOS) process. The results suggested that P(AN-co-AMPS) nanofibers had the lower heat release rate (ΔH/ΔT = 26.9 J g−1 °C−1), the less activation energy of cyclization (Ea1 = 26.6 kcal/mol and Ea2 = 27.5 kcal/mol), and the higher extent of stabilization (Es and SI) during TOS process, which demonstrated that the AMPS comonomer improved the efficiency of the TOS process. The P(AN-co-AMPS) nanofibers had the better thermal stable structures. Moreover, the carbon nanofibers derived from P(AN-co-AMPS) precursor nanofibers had the better graphite-like structures (XG = 46.889). Therefore, the AMPS is a promising candidate comonomer to produce high performance carbon fibers.


2021 ◽  
Vol 5 (3) ◽  
pp. 48-55
Author(s):  
Mahbubor Rahman ◽  
TUBA DEMIREL ◽  
İsmail Karacan

The thermal oxidative stabilization and carbonization processes of poly(hexamethylene adipamide) or (polyamide 66) fibers were accomplished to transform into carbon fibers. Polyamide 66 fibers were pretreated with a ethanol solution of cupric chloride followed by a stabilization process in the air atmosphere. Carbonization experiments were executed at temperatures of 500, 700, 900, and 1100°C utilizing heating rate of 2.5 °C/min. Carbonization experiments were performed at temperatures between 500 and 1100°C employing the rises of 100°C. X-ray diffraction analysis of the carbon fibers shown a highly disordered carbon structure developed during the carbonization process. The values of fiber diameter, linear density, volume density, carbon fiber yield, elemental analysis, and electrical properties revealed a strong dependence on the carbonization temperature. As an insulating material, the polyamide 66 or PA66 precursor was transformed to a semiconducting stage after the thermal stabilization and carbonization processes. The current study demonstrated how processing parameters influence the structure and characteristics of carbon fibers produced from poly(hexamethylene adipamide) fibers.


Pharmaceutics ◽  
2020 ◽  
Vol 12 (11) ◽  
pp. 1008 ◽  
Author(s):  
Qilei Yang ◽  
Chang Zu ◽  
Wengang Li ◽  
Weiwei Wu ◽  
Yunlong Ge ◽  
...  

Paclitaxel (PTX) is a poor water-soluble antineoplastic drug with significant antitumor activity. However, its low bioavailability is a major obstacle for its biomedical applications. Thus, this experiment is designed to prepare PTX crystal powders through an antisolvent precipitation process using 1-hexyl-3-methylimidazolium bromide (HMImBr) as solvent and water as an antisolvent. The factors influencing saturation solubility of PTX crystal powders in water in water were optimized using a single-factor design. The optimum conditions for the antisolvent precipitation process were as follows: 50 mg/mL concentration of the PTX solution, 25 °C temperature, and 1:7 solvent-to-antisolvent ratio. The PTX crystal powders were characterized via scanning electron microscopy, Fourier transform infrared spectroscopy, high-performance liquid chromatography–mass spectrometry, X-ray diffraction, differential scanning calorimetry, thermogravimetric analysis, Raman spectroscopy, solid-state nuclear magnetic resonance, and dissolution and oral bioavailability studies. Results showed that the chemical structure of PTX crystal powders were unchanged; however, precipitation of the crystalline structure changed. The dissolution test showed that the dissolution rate and solubility of PTX crystal powders were nearly 3.21-folds higher compared to raw PTX in water, and 1.27 times higher in artificial gastric juice. Meanwhile, the bioavailability of PTX crystal increased 10.88 times than raw PTX. These results suggested that PTX crystal powders might have potential value to become a new oral PTX formulation with high bioavailability.


2021 ◽  
Vol 21 (11) ◽  
pp. 5592-5602
Author(s):  
Samira Almasi ◽  
Ali Mohammad Rashidi

The effect of the yttria-stabilized zirconia (YSZ) nanoparticle loading in an electro-less bath was considered as one of the vital synthesis variables for control Ni content and microstructure of prepared nanocomposite particles, which are two crucial factors to achieving high-performance SOFC anode. Nanocomposite particles were prepared using a simple electroless method without any expensive pretreatment of sensitizing by Sn2+ ions as well as activating by Pd2+ ions that are usually used to apply nickel coating on the surface of a non-conductive substrate. The process was performed by adding YSZ nanoparticles into NaOH solution, separating them from the solution by the centrifugal method, then providing several water-based nanofluids with different concentrations of activated YSZ nanoparticles, mixing them with NiCI2 solution, followed by adding the hydrazine and then NaOH solution. X-ray diffraction and scanning electron microscopy coupled with energy dispersive X-ray analysis were used to analyze the prepared nanocomposite particles. It is observed that after adding YSZ nanoparticles into the NaOH solution, the pH of the solution varied gradually from a starting pH of 10.2 to 9. Also, by increasing the YSZ nanoparticles loading in the electroless bath from 76 mg/l to 126 mg/l, the grain size of Ni deposits, the Ni content and the average size of the prepared nanocomposite particles decreased. The electrochemical mechanism previously proposed for the nickel ion reduction was modified, and a novel analytical model was proposed for variation of the efficiency of Ni deposition with YSZ nanoparticles loading.


Chemija ◽  
2020 ◽  
Vol 31 (3) ◽  
Author(s):  
Ehab AlShamaileh ◽  
Muayad Esaifan ◽  
Qusay Abu-Afifeh

The formation of metal oxide-based hydroxysodalite by alkali-activation of kaolinite is studied using X-ray diffraction (XRD) study and differential scanning calorimetry (DSC) analysis. Different metal oxides (CoO, MgO, FeO and SiO2) were used to form the metal oxide-based hydroxysodalite. The transformation from kaolinite into hydroxysodalite is confirmed by XRD. In the thermodynamic study, the maximum peak temperatures for DSC curves at various heating rates were used to determine the activation energy (Ea) of the hydroxysodalite formation. With magnesium oxide and cobalt oxide, the formation process was found to be exothermic while it was endothermic with iron oxide.


Polymers ◽  
2019 ◽  
Vol 11 (6) ◽  
pp. 937 ◽  
Author(s):  
Niki Poulopoulou ◽  
George Kantoutsis ◽  
Dimitrios N. Bikiaris ◽  
Dimitris S. Achilias ◽  
Maria Kapnisti ◽  
...  

Poly(butylene 2,5-furandicarboxylate) (PBF) constitutes a new engineering polyester produced from renewable resources, as it is synthesized from 2,5-furandicarboxylic acid (2,5-FDCA) and 1,4-butanediol (1,4-BD), both formed from sugars coming from biomass. In this research, initially high-molecular-weight PBF was synthesized by applying the melt polycondensation method and using the dimethylester of FDCA as the monomer. Furthermore, five different series of PBF blends were prepared, namely poly(l-lactic acid)–poly(butylene 2,5-furandicarboxylate) (PLA–PBF), poly(ethylene terephthalate)–poly(butylene 2,5-furandicarboxylate) (PET–PBF), poly(propylene terephthalate)–poly(butylene 2,5-furandicarboxylate) (PPT–PBF), poly(butylene 2,6-naphthalenedicarboxylate)-poly(butylene 2,5-furandicarboxylate) (PBN–PBF), and polycarbonate–poly(butylene 2,5-furandicarboxylate) (PC–PBF), by dissolving the polyesters in a trifluoroacetic acid/chloroform mixture (1/4 v/v) followed by coprecipitation as a result of adding the solutions into excess of cold methanol. The wide-angle X-ray diffraction (WAXD) patterns of the as-prepared blends showed that mixtures of crystals of the blend components were formed, except for PC which did not crystallize. In general, a lower degree of crystallinity was observed at intermediate compositions. The differential scanning calorimetry (DSC) heating scans for the melt-quenched samples proved homogeneity in the case of PET–PBF blends. In the remaining cases, the blend components showed distinct Tgs. In PPT–PBF blends, there was a shift of the Tgs to intermediate values, showing some partial miscibility. Reactive blending proved to improve compatibility of the PBN–PBF blends.


2007 ◽  
Vol 29-30 ◽  
pp. 337-340 ◽  
Author(s):  
M.A. Sawpan ◽  
K.L. Pickering ◽  
Alan Fernyhough

The potential of hemp fibre as a reinforcing material for Poly(lactic acid) (PLA) was investigated. Good interaction between hemp fibre and PLA resulted in increases of 100% for Young’s modulus and 30% for tensile strength of composites containing 30 wt% fibre. Different predictive ‘rule of mixtures’ models (e.g. Parallel, Series and Hirsch) were assessed regarding the dependence of tensile properties on fibre loading. Limited agreement with models was observed. Differential scanning calorimetry (DSC) and x-ray diffraction (XRD) studies showed that hemp fibre increased the degree of crystallinity in PLA composites.


2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Di Li ◽  
Guo-Qing Zhong

The antimony(III) complex [Sb(Hedta)]·2H2O was synthesized with ethylenediaminetetraacetic acid (H4edta) and antimonous oxide as main raw materials in aqueous solution. The composition and structure of the complex were characterized by elemental analysis, infrared spectra, single crystal X-ray diffraction, X-ray powder diffraction, thermogravimetry, and differential scanning calorimetry. The crystal structure of the antimony(III) complex belongs to orthorhombic system, space group Pna2(1), with cell parameters ofa=18.4823(18) Å,b=10.9408(12) Å,c=7.3671(5) Å,V=1489.7(2) Å3,Z=4, andDc=1.993 g cm−3. The Sb(III) ion is five-coordinated by two amido N atoms and three carboxyl O atoms from a single Hedta3−ligand, forming a distorted trigonal bipyramid geometry. The thermal decomposition processes of the complex include dehydration, oxidation, and pyrolysis of the ligand, and the last residue is Sb2O3at the temperature of 570°C.


2018 ◽  
Vol 251 ◽  
pp. 01045 ◽  
Author(s):  
Vyacheslav Semenov

Modern requirements in the field of energy and resource saving determines the need to apply effective fencing structures. To ensure the thermal homogeneity of the structures erected with small-piece masonry elements (ceramic and light-weight concrete units etc.), it is necessary to use lightweight mortars. One of the most effective methods to obtain such mortars is the introduction of hollow ceramic microspheres as a filler into their composition. The purpose of this work is studying of the composition and structure of a cement masonry mortar with hollow ceramic microspheres and modifying additives in correlation with its properties. The methods of thermogravimetric analysis, scanning electron microscopy, X-ray diffraction and standard test methods for the masonry mortars were used. The effect of the structural characteristics of the composite on the properties of final product was analyzed. It is established that the microstructure of the modified mortar samples is more compact in compare with basic composition, and the surface of the microspheres is covered by the products of the chemical interaction of its walls with the cement matrix. The aforesaid research allowed to obtain the high-performance lightweight mortars with hollow ceramic microspheres.


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