Synthesis and properties of soluble polyimides containing tert-butyl, ether linkages, and triphenylmethane units

2020 ◽  
Vol 32 (8) ◽  
pp. 924-932
Author(s):  
Zhuwei Qin ◽  
Suyun Lv ◽  
Yixuan Wu ◽  
Cong Wang ◽  
Siyu Zhang ◽  
...  

A molecular theory design was carried out to synthesize a diamine monomer 1-(4-tert-butylphenyl)-1,1-bis[4-(4-aminophenoxy)] phenylethane containing tert-butyl, ether linkage, and triphenylmethane units. Then it was polymerized with several commercial aromatic dianhydrides, including diphenyl hexafluoroisopropylidene tetraic acid dianhydride (6FDA), diphenyl ether tetracarboxylic dianhydride (ODPA), biphenyltetracarboxylic dianhydride (BPDA), and benzophenone tetraacid dianhydride (BTDA), via the conventional two-step method to afford a series of aromatic polyimides (PIs). The structure and properties of the polymer were characterized by Fourier transform infrared (FTIR) spectroscopy, solubility test, thermogravimetric analysis, differential scanning calorimetry, ultraviolet–visible spectroscopy, and tensile tests. The results showed that there were characteristic peaks of PI around 1776, 1720, and 1378 cm−1 in the FTIR spectra; 6FDA-, ODPA-, and BPDA-based PI are easily soluble in N-methylpyrrolidone (NMP), concentrated sulfuric acid, N,N-dimethylacetamide (DMAc), pyridine, Tetrahydrofuran (THF), Trichloromethane (CHCl3), and other common organic solvents showing excellent solubility. In a nitrogen atmosphere, the glass transition temperature of the PI films are between 246°C and 275°C, the temperature of 5% weight loss is above 501°C, and the residual mass fraction at 750°C is 53–61%. The mechanical properties range from 67.2 MPa to 88.6 MPa. In addition to the BTDA-based PI film, the other three types of PI have good transparency. The simultaneous introduction of tert-butyl, ether linkages, and triphenylmethane units has a synergistic effect, which greatly improves the solubility of PI and maintains good thermal stability, mechanical properties, and optical properties of PI at the same time.

Materials ◽  
2021 ◽  
Vol 14 (15) ◽  
pp. 4205
Author(s):  
Marta Przybysz-Romatowska ◽  
Mateusz Barczewski ◽  
Szymon Mania ◽  
Agnieszka Tercjak ◽  
Józef Haponiuk ◽  
...  

Reactive blending is a promising approach for the sustainable development of bio-based polymer blends and composites, which currently is gaining more and more attention. In this paper, biodegradable blends based on poly(ε-caprolactone) (PCL) and poly(lactic acid) (PLA) were prepared via reactive blending performed in an internal mixer. The PCL and PLA content varied in a ratio of 70/30 and 55/45. Reactive modification of PCL/PLA via liquid organic peroxides (OP) including 0.5 wt.% of tert-butyl cumyl peroxide (BU), 2,5-dimethyl-2,5-di-(tert-butylperoxy)-hexane (HX), and tert-butyl peroxybenzoate (PB) is reported. The materials were characterized by rotational rheometer, atomic force microscopy (AFM), thermogravimetry (TGA), differential scanning calorimetry (DSC), tensile tests and biodegradability tests. It was found that the application of peroxides improves the miscibility between PCL and PLA resulted in enhanced mechanical properties and more uniform morphology. Moreover, it was observed that the biodegradation rate of PCL/PLA blends reactively compatibilized was lower comparing to unmodified samples and strongly dependent on the blend ratio and peroxide structure. The presented results confirmed that reactive blending supported by organic peroxide is a promising approach for tailoring novel biodegradable polymeric systems with controllable biodegradation rates.


Materials ◽  
2020 ◽  
Vol 13 (5) ◽  
pp. 1242
Author(s):  
Olga Mysiukiewicz ◽  
Paulina Kosmela ◽  
Mateusz Barczewski ◽  
Aleksander Hejna

Investigations related to polymer/metal composites are often limited to the analysis of the electrical and thermal conductivity of the materials. The presented study aims to analyze the impact of aluminum (Al) filler content (from 1 to 20 wt%) on the rarely investigated properties of composites based on the high-density polyethylene (HDPE) matrix. The crystalline structure, rheological (melt flow index and oscillatory rheometry), thermal (differential scanning calorimetry), as well as static (tensile tests, hardness, rebound resilience) and dynamic (dynamical mechanical analysis) mechanical properties of composites were investigated. The incorporation of 1 and 2 wt% of aluminum filler resulted in small enhancements of mechanical properties, while loadings of 5 and 10 wt% provided materials with a similar performance to neat HDPE. Such results were supported by the lack of disturbances in the rheological behavior of composites. The presented results indicate that a significant content of aluminum filler may be introduced into the HDPE matrix without additional pre-treatment and does not cause the deterioration of composites’ performance, which should be considered beneficial when engineering PE/metal composites.


2021 ◽  
Vol 36 (2) ◽  
pp. 137-143
Author(s):  
S. A. Awad

Abstract This paper aims to describe the thermal, mechanical, and surface properties of a PVA/HPP blend whereby the film was prepared using a solution casting method. The improvements in thermal and mechanical properties of HPP-based PVA composites were investigated. The characterization of pure PVA and PVA composite films included tensile tests, thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). The results of TGA and DSC indicated that the addition of HPP increased the thermal decomposition temperature of the composites. Mechanical properties are significantly improved in PVA/HPP composites. The thermal stability of the PVA composite increased with the increase of HPP filler content. The tensile strength increased from 15.74 ± 0.72 MPa to 27.54 ± 0.45 MPa and the Young’s modulus increased from 282.51 ± 20.56 MPa to 988.69 ± 42.64 MPa for the 12 wt% HPP doped sample. Dynamic mechanical analysis (DMA) revealed that at elevated temperatures, enhanced mechanical properties because of the presence of HPP was even more noticeable. Morphological observations displayed no signs of agglomeration of HPP fillers even in composites with high HPP loading.


2016 ◽  
Vol 30 (2) ◽  
pp. 174-195 ◽  
Author(s):  
Rungsima Chollakup ◽  
Haroutioun Askanian ◽  
Florence Delor-Jestin

In the furniture, automotive and contruction industries, there is increased demand for cost-effective and lightweight biocomposites. The objective of this work was to develop new natural fibre-based composites with specific properties. Palm and pineapple leaf fibres were chosen in association with polypropylene (PP). The first step was to investigate the effect of these natural fibres as reinforcement for PP. The evolution of chemical structure and crystallinity was proposed with infrared spectroscopy measurements and differential scanning calorimetry thermograms, respectively. The assessments of mechanical properties with tensile tests and melt viscoelastic behaviour were also investigated. The study enabled to distinguish the influence of fibre content. The second step in our work was to assess the composite durability after ultraviolet exposure or thermal ageing. The oxidation level was calculated. The long-term evolution of thermal and mechanical properties was also proposed. As a result, the PP/pineapple leaf composite revealed a promising biocomposite.


2002 ◽  
Vol 753 ◽  
Author(s):  
Masahiro Tsuji ◽  
Hideki Hosoda ◽  
Kenji Wakashima ◽  
Yoko Yamabe-Mitarai

ABSTRACTEffects of ruthenium (Ru) substitution on constituent phases, phase transformation temperatures and mechanical properties were investigated for Ti-Ni shape memory alloys. Ti50Ni50-XRuX alloys with Ru contents (X) from 0mol% (binary TiNi) to 50mol% (binary TiRu) were systematically prepared by Ar arc-melting followed by hot-forging at temperatures from 1173K to 1673K depending on chemical composition. Phase stability was assessed by DSC (differential scanning calorimetry), XRD (X-ray diffractometry) and TEM (transmission electron microscopy). Mechanical properties were investigated using hardness and tensile tests at room temperature. With increasing Ru content, it was found that the lattice parameter of B2 phase increases, the martensitic transformation temperature slightly decreases, and the melting temperature increases monotonously. Besides, R-phase appears for Ti-Ni alloys containing 3mol% and 20mol%Ru but no diffusionless phase transformation is seen in Ti-Ni alloy containing 5mol%Ru. Vickers hardness shows the maximum at an intermediate composition (HV1030 at 30mol%Ru); this suggests that large solid solution hardening is caused by Ru substitution for the Ni-sites in TiNi.


2016 ◽  
Vol 682 ◽  
pp. 245-251 ◽  
Author(s):  
Grzegorz Włoch ◽  
Tomasz Skrzekut ◽  
Jakub Sobota ◽  
Antoni Woźnicki ◽  
Justyna Cisoń

Mixed and preliminarily consolidated powders of aluminium and nickel (90 mass % Al and 10 mass % Ni) were hot extruded. As results the rod, 8 mm in diameter, was obtained. As-extruded material was subjected to the microstructural investigations using scanning electron microscopy (SEM/EDS) and X-ray analysis (XRD). The differential scanning calorimetry (DSC) and thermo-mechanical analysis (TMA) were also performed. The mechanical properties of as extruded material were determined by the tensile test and Vickers hardness measurements. In order to evaluate the thermal stability of PM alloy, samples were annealed at the temperature of 475 and 550 °C. After annealing Vickers hardness measurements and tensile tests were carried out. The plastic consolidation of powders during extrusion was found to be very effective, because no pores or voids were observed in the examined material. The detailed microstructural investigations and XRD analyses did not reveal the presence of the intermetallic phases in the as-extruded material. During annealing, the Al3Ni intermetallic compound was formed as the result of chemical reaction between the alloy components. The hardness of the alloy after annealing at the temperature of 475°C was found to be comparable to the hardness in as-extruded state. Annealing of the material at the temperature of 550°C results in hardness decreasing by about 50%, as the consequence of porosity formation and Al3Ni cracking.


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.


2018 ◽  
Vol 31 (2) ◽  
pp. 154-167 ◽  
Author(s):  
Yu Qing Cui ◽  
Zhong Wei Yin

Although the extensive research has expanded on the modification of cyanate ester (CE) resins and the mechanical properties of CE composites, very few studies have been conducted on carbon fibre (CF)/modified CE winding composites and the thermomechanical properties of the composites. In this research, epoxy (EP)-modified novolac cyanate ester (NCE) and bismaleimide (BMI)-modified NCE resins were prepared. The CF/modified CE winding composites were manufactured, and their thermomechanical properties were tested. The optimal winding process was determined, and a preheating technique was implemented. Then, the EP/CE resin (10:90) and the BMI–DBA/CE resin (10:90) were selected as the resin matrix of the winding composite based on the viscosity properties, mechanical properties and thermal analysis (using thermogravimetric analysis and differential scanning calorimetry) of the modified CE resin. The selected resin exhibited good manufacturability at 70°C, good thermal stability and high Tg (above 370°C). The thermomechanical property tests indicate that the modified CE resin composite exhibits an outstanding mechanical strength at room temperature and at high temperatures (130°C, 150°C and 180°C) compared with that of the pure CE resin composite. The reasons for this enhancement can be attributed to a toughening mechanism and the effect of sizing agents on the CFs.


Polymers ◽  
2019 ◽  
Vol 11 (6) ◽  
pp. 1069 ◽  
Author(s):  
Gabriele Nanni ◽  
José A. Heredia-Guerrero ◽  
Uttam C. Paul ◽  
Silvia Dante ◽  
Gianvito Caputo ◽  
...  

Poly(furfuryl alcohol) (PFA) is a bioresin synthesized from furfuryl alcohol (FA) that is derived from renewable saccharide-rich biomass. In this study, we compounded this bioresin with polycaprolactone (PCL) for the first time, introducing new functional polymer blends. Although PCL is biodegradable, its production relies on petroleum precursors such as cyclohexanone oils. With the method proposed herein, this dependence on petroleum-derived precursors/monomers is reduced by using PFA without significantly modifying some important properties of the PCL. Polymer blend films were produced by simple solvent casting. The blends were characterized in terms of surface topography by atomic force microscopy (AFM), chemical interactions between PCL and PFA by attenuated total reflection-Fourier transform infrared (ATR-FTIR), crystallinity by XRD, thermal properties by differential scanning calorimetry (DSC), and mechanical properties by tensile tests and biocompatibility by direct and indirect toxicity tests. PFA was found to improve the gas barrier properties of PCL without compromising its mechanical properties, and it demonstrated sustained antioxidant effect with excellent biocompatibility. Our results indicate that these new blends can be potentially used in diverse applications ranging from food packing to biomedical devices.


2008 ◽  
Vol 37 (1) ◽  
pp. 21-27
Author(s):  
H. Satapathy ◽  
A.K. Banthia

PurposeThe purpose of this paper is to synthesise, characterise and study polymerisation kinetics of novel 4‐nonylphenylmethacrylate (NPMA) polymer.Design/methodology/approachNew methacrylic monomer, 4‐NPMA with a pendant nonylphenyl group was synthesised and characterised using various characterisation techniques. The free radical polymerisation kinetics study was done with the help of differential scanning calorimetry data.FindingsThe average heat of polymerisation (ΔHp) was found to be 685.43 J/g. Activation energy (Ea) of 95.86 kJ mol−1 and frequency factor of (A) 3.4 × 104 min−1 was obtained using Kissinger method. The thermogravimetric analysis of the polymer in nitrogen reveals that it possesses very good thermal stability in comparison to alkyl methacrylates due to presence of pendant nonylphenyl group.Research limitations/implicationsNew methacrylic monomer, 4‐NPMA was synthesised by reacting nonylphenol dissolved in methyl ethyl ketone (MEK) with methacryloyl chloride in the presence of triethylamine as a base. Polymerisation of 4‐NPMA was carried out in MEK using benzoyl peroxide (BPO) as initiator under nitrogen atmosphere. The kinetics study of NPMA monomer with 1.1 wt% BPO was reported for evaluation of kinetic parameters by employing the Kissinger equation.Practical implicationsThis is a simple and easy method of modification of methacrylate ester with phenyl groups to obtain a polymer of enhanced properties.Originality/valueThis is a novel method for enhancing the thermal as well as surface adhesion properties of methacrylate polymers which finds several applications in surface coatings and adhesives.


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