scholarly journals Novel Crosslinking System for Poly-Chloroprene Rubber to Enable Recyclability and Introduce Self-Healing

Polymers ◽  
2021 ◽  
Vol 13 (19) ◽  
pp. 3347
Author(s):  
Anureet Kaur ◽  
Julien E. Gautrot ◽  
Gabriele Cavalli ◽  
Douglas Watson ◽  
Alan Bickley ◽  
...  

The introduction of dynamic bonds capable of mediating self-healing in a fully cross-linked polychloroprene network can only occur if the reversible moieties are carried by the cross-linker itself or within the main polymer backbone. Conventional cross-linking is not suitable for such a purpose. In the present work, a method to develop a self-healable and recyclable polychloroprene rubber is presented. Dynamic disulfide bonds are introduced as part of the structure of a crosslinker (liquid polysulfide polymer, Thiokol LP3) coupled to the polymer backbone via thermally initiated thiol-ene reaction. The curing and kinetic parameters were determined by isothermal differential scanning calorimetry and by moving die rheometer analysis; tensile testing was carried to compare the tensile strength of cured compound, healed compounds and recycled compounds, while chemical analysis was conducted by surface X-Ray Photoelectron Spectroscopy. Three formulations with increasing concentrations of Thiokol LP-3 were studied (2, 4, 6 phr), reaching a maximum ultimate tensile strength of 22.4 MPa and ultimate tensile strain of 16.2 with 2 phr of Thiokol LP-3, 11.7 MPa and 10.7 strain with 4 phr and 5.6 MPa and 7.3 strain with 6 phr. The best healing efficiencies were obtained after 24 h of healing at 80 °C, increasing with the concentration of Thiokol LP-3, reaching maximum values of 4.5% 4.4% 13.4% with 2 phr, 4 phr and 6 phr, respectively, while the highest recycling efficiency was obtained with 4 phr of Thiokol LP-3, reaching 11.2%.

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Shafiq Ishak ◽  
Soumen Mandal ◽  
Han-Seung Lee ◽  
Jitendra Kumar Singh

AbstractLauric acid (LA) has been recommended as economic, eco-friendly, and commercially viable materials to be used as phase change materials (PCMs). Nevertheless, there is lack of optimized parameters to produce microencapsulated PCMs with good performance. In this study, different amounts of LA have been chosen as core materials while tetraethyl orthosilicate (TEOS) as the precursor solution to form silicon dioxide (SiO2) shell. The pH of precursor solution was kept at 2.5 for all composition of microencapsulated LA. The synthesized microencapsulated LA/SiO2 has been characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), X-Ray photoelectron spectroscopy (XPS), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The SEM and TEM confirm the microencapsulation of LA with SiO2. Thermogravimetric analysis (TGA) revealed better thermal stability of microencapsulated LA/SiO2 compared to pure LA. PCM with 50% LA i.e. LAPC-6 exhibited the highest encapsulation efficiency (96.50%) and encapsulation ratio (96.15%) through Differential scanning calorimetry (DSC) as well as good thermal reliability even after 30th cycle of heating and cooling process.


2005 ◽  
Vol 13 (8) ◽  
pp. 839-846 ◽  
Author(s):  
Li-Ping Wang ◽  
Yun-Pu Wang ◽  
Fa-Ai Zhang

A new type of nano-composite film was prepared from polyvinyl alcohol, Ni2+-montmorillonite (Ni2+-MMT), defoamer, a levelling agent and a plasticizer. Its thermal characteristics were studied by Differential Scanning Calorimetry (DSC). The intermolecular interactions were measured by Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS), and the tensile strength (TS) and elongation at break (%E) were measured. The microstructures were studied by X-ray diffraction (XRD) and atomic force microscopy (AFM). FT-IR and XPS spectra indicated that cross-linking has taken place between PVA and Ni2+-MMT. XRD and AFM indicate that the PVA molecules had inserted themselves into the silicate layers of MMT, exfoliating them and dispersing them randomly into the PVA matrix. Compared to pure PVA film, the TS of the films was increased and %E decreased when the Ni2+-Montmorillonite was added and the dissolution temperature of the film was also reduced.


2018 ◽  
Vol 89 (9) ◽  
pp. 1770-1781 ◽  
Author(s):  
Huaizhong Xu ◽  
Benedict Bauer ◽  
Masaki Yamamoto ◽  
Hideki Yamane

A facile route was proposed to fabricate core–sheath microfibers, and the relationships among processing parameters, crystalline structures and the mechanical properties were investigated. The compression molded poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) (PHBH)/poly(L-lactic acid) (PLLA) strip enhanced the spinnability of PHBH and the mechanical properties of PLLA as well. The core–sheath ratio of the fibers was determined by the prefab strip, while the PLLA sheath component did not completely cover the PHBH core component due to the weak interfacial tension between the melts of PHBH and PLLA. A rotational target was applied to collect aligned fibers, which were further drawn in a water bath. The tensile strength and the modulus of as-spun and drawn fibers increased with increasing the take-up velocities. When the take-up velocity was above 500 m/min, the jet became unstable and started to break up at the tip of the Taylor cone, decreasing the mechanical properties of the fibers. The drawing process facilitated the crystallization of PLLA and PHBH, and the tensile strength and the modulus increased linearly with the increasing the draw ratio. The crystal information displayed from wide-angle X-ray diffraction patterns and differential scanning calorimetry heating curves supported the results of the tensile tests.


2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Yi Liu ◽  
Yan Chen ◽  
Junwei Zhang ◽  
Junkai Gao ◽  
Zhi Han

Abstract Copper microsphere hybrid mesoporous carbon (MPC-Cu) was synthesized by the pyrolysis of polydopamine microspheres doped with copper ions that were prepared using a novel, facile and simple one-step method of dopamine biomimetic polymerization and copper ion adsorption. The resulting MPC-Cu was then used as a supporter for polyethylene glycol (PEG) to synthesize shape-stabilized phase change materials (PEG/MPC-Cu) with enhanced thermal properties. PEG/MPC-Cu was studied by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, thermogravimetric analysis, differential scanning calorimetry and thermal constant analysis. The results demonstrated that the thermal conductivity of PEG/MPC-Cu was 0.502 W/(m K), which increased by 100% compared to pure PEG [0.251 W/(m K)]. The melting enthalpy of PEG/MPC-Cu was 95.98 J/g, indicating that PEG/MPC-Cu is a promising candidate for future thermal energy storage applications. In addition, the characterization results suggested that PEG-MPC-Cu possessed high thermal stability. Therefore, the method developed in this paper for preparing shape-stabilized phase change materials with improved thermal properties has substantial engineering application prospects.


Polymers ◽  
2020 ◽  
Vol 12 (11) ◽  
pp. 2548
Author(s):  
Vicente Espinosa-Solis ◽  
Yunia Verónica García-Tejeda ◽  
Everth Jimena Leal-Castañeda ◽  
Víctor Barrera-Figueroa

In this paper, we consider amaranth starch extracted from the seeds of Amaranthus hypochondriacus L. An amphiphilic character is conferred to the starch by a chemical modification, which involves an esterification by lauroyl chloride at three modification levels. The degree of substitution (DS) after the modification ranged from 0.06 to 1.16. X-ray photoelectron spectroscopy analysis confirmed the presence of fatty acyl chains on the surface of the esterified starches. The hydrophobicity of starches was confirmed by their adsorption isotherms, which showed a decrease in the moisture adsorption of lauroylated as DS increased. X-ray diffraction analysis revealed a higher crystallinity, which was observed in the two samples subjected to the highest levels of modification. A higher crystallinity is related to a higher gelatinization enthalpy. These results are in agreement with the thermal characterization obtained by differential scanning calorimetry (DSC). An inhibition of the retrogradation properties of lauroylated amaranth starches was also observed.


Catalysts ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 507
Author(s):  
Tomasz Jakubek ◽  
Camillo Hudy ◽  
Paweł Stelmachowski ◽  
Ewa Nowicka ◽  
Stan Golunski ◽  
...  

A series of layered birnessite (AMn4O8) catalysts containing different alkali cations (A = H+, Li+, Na+, K+, Rb+, or Cs+) was synthesized. The materials were thoroughly characterized using X-ray diffraction, X-ray fluorescence, X-ray photoelectron spectroscopy, Raman spectroscopy, specific surface area analysis, work function, thermogravimetry/differential scanning calorimetry, and transmission electron microscopy. The catalytic activity in soot combustion in different reaction modes was investigated (tight contact, loose contact, loose contact with NO addition). The activity in the oxidation of light hydrocarbons was evaluated by tests with methane and propane. The obtained results revealed that alkali-promoted manganese oxides are highly catalytically active in oxidative reactions. In soot combustion, the reaction temperature window was shifted by 195 °C, 205 °C, and 90 °C in tight, loose + NO, and loose contact conditions against uncatalyzed oxidation, respectively. The catalysts were similarly active in hydrocarbon combustion, achieving a 40% methane conversion at 600 °C and a total propane conversion at ~450 °C. It was illustrated that the difference in activity between tight and loose contacts can be successfully bridged in the presence of NO due to its facile transformation into NO2 over birnessite. The particular activity of birnessite with H+ cations paves the road for the further development of the active phase, aiming at alternative catalytic systems for efficient soot, light hydrocarbons, and volatile organic compounds removal in the conditions present in combustion engine exhaust gases.


2013 ◽  
Vol 20 (01) ◽  
pp. 1350006 ◽  
Author(s):  
PARTHASARATHI BERA ◽  
H. SEENIVASAN ◽  
K. S. RAJAM

Co–W alloy coatings were deposited with direct current (DC) and pulse current (PC) electrodeposition methods using gluconate bath at pH5 and characterized by X-ray diffraction, field emission scanning electron microscopy, atomic force microscopy, differential scanning calorimetry (DSC) and X-ray photoelectron spectroscopy (XPS). DSC studies hint at the possibility of formation of metallic glasses. Detailed XPS studies of these alloy coatings have been carried out to compare elemental states and composition of Co and W in DC and PC electrodeposited alloys. DC-plated alloy has significant amount of Co and W metal along with their respective oxidized species. In contrast, mainly oxidized metals are present in the following layers of as-deposited coatings prepared with PC plating. Concentration of Co metal is observed to increase during sputtering, whereas there is no change in W6+ concentration. Microhardness measurement of all the Co–W coatings shows higher hardness compared to Co metal and 1:1 and 1:4 PC electrodeposited coatings show little higher hardness compared to 1:2 PC electrodeposited coating.


2007 ◽  
Vol 546-549 ◽  
pp. 1571-1574
Author(s):  
L. Ji ◽  
N.L. Shi ◽  
Rui Yang

CVD (chemical vapor deposition) SiC continuous fiber is used as reinforcement of metal matrix composites because of its high strength, high stiffness and elevated temperature stability. In this work, anodic oxidation method was used to treat the surface of carbon coated SiC fiber. Then the surface of treated fiber was compared with untreated one by scan electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS). SiC was detected on the surface of untreated carbon-rich coating. It is proved by XPS that SiC was transformed into SiO2 after treatment. About 100~200nm thick oxidation layer was detected on the surface of carbon-rich coating and the structure of double coatings formed. Because the surface of fiber became smooth and the tensile stress on it was relaxed after treatment, the tensile strength of fiber was improved by 8%~20% average and the dispersing ratio of it was reduced.


2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Joo Hyung Lee ◽  
Seong Hun Kim

Abstract Incorporation of nanofillers into polyurethane (PU) is a promising technique for enhancing its thermal and mechanical properties. Silane grafting has been used as a surface treatment for the functionalization of graphene oxide (GO) with numerous reactive sites dispersed on its basal plane and edge. In this study, amine-grafted GO was prepared using silanization of GO with (3-aminopropyl)triethoxysilane. The functionalized graphene oxide (fGO) was characterized by Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy. Next, it was introduced in PU fabricated using polycaprolactone diol, castor oil, and hexamethylene diisocyanate. The fGO–PU nanocomposites were in turn characterized by FT-IR, X-ray diffraction, scanning electron microscopy, differential scanning calorimetry, thermogravimetric analysis, and a universal testing machine. The results obtained from these analyses showed changes in structural thermal properties, as well as improved thermal stability and mechanical properties because of the strong interfacial adhesion between the fGO and the PU matrix.


Pharmaceutics ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 82 ◽  
Author(s):  
Luning Dong ◽  
Yaping Mai ◽  
Qiang Liu ◽  
Wannian Zhang ◽  
Jianhong Yang

The purpose of this study was to increase the dissolution of glycyrrhetinic acid (GA) by preparing ternary solid dispersion (TSD) systems containing alkalizers, and to explore the modulating mechanism of alkalizers in solid dispersion systems. GA TSDs were prepared by hot melt extrusion (HME) with Kollidon® VA64 as the carrier and L-arginine/meglumine as the alkalizers. The in vitro release of the TSD was investigated with a dissolution test, and the dissociation constant (pKa) was used to describe the ionization degree of the drug in different pH buffers. Scanning electron microscopy (SEM), differential scanning calorimetry (DSC), X-ray powder diffraction (XRPD), Fourier Transform Infrared Spectroscopy (FTIR), Raman spectra, X-ray photoelectron spectroscopy (XPS), and a molecular model were used for solid-state characterizations and to study the dissolution mechanism of the TSDs. It was evident that the dissolution of GA significantly increased as a result of the TSD compared to the pure drug and binary solid dispersion. SEM, DSC, and XPRD data showed that GA transformed into an amorphous form in TSD. As illustrated by FTIR, Raman, XPS, and molecular docking, high binding energy ion-pair complexes formed between GA and the alkalizers during the process of HME. These can destroy the H-bond between GA molecules. Further, intermolecular H-bonds formed between the alkalizers and Kollidon® VA64, which can increase the wettability of the drug. Our results will significantly improve the solubility and dissolution of GA. In addition, the lower pKa value of TSD indicates that higher ionization is beneficial to the dissolution of the drug. This study should facilitate further developments of TSDs containing alkalizers to improve the dissolution of weakly acidic drugs and gain a richer understanding of the mechanism of dissolution.


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