Synthesis and thermal properties of high temperature phthalonitrile resins cured with self-catalytic amino-contanining phthalonitrle compounds

2016 ◽  
Vol 29 (10) ◽  
pp. 1209-1221 ◽  
Author(s):  
Xinggang Chen ◽  
Jiayu Liu ◽  
Zhenjie Xi ◽  
Shuyan Shan ◽  
Huili Ding ◽  
...  

A series of self-catalytic phthalonitrile compounds with o-, m-, and p- amino groups, namely, 4-(2-aminophenoxy)phthalonitrile (2-NH2-CN), 4-(3-aminophenoxy)phthalonitrile (3-NH2-CN), and 4-(4-aminophenoxy)phthalonitrile (4-NH2-CN), were synthesized via a facile nucleophilic displacement of a nitro-substituent with 4-nitrophthalonitrile. The phthalonitrile resins were prepared by curing 2-NH2-CN, 3-NH2-CN, and 4-NH2-CN with 1,3-bis(3,4-dicyanophenoxy) benzene ( m-BDB). The structures of these compounds were characterized by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance, and wide-angle X-ray diffraction. Curing behaviors of 2-NH2-CN, 3-NH2-CN, and 4-NH2-CN with m-BDB were recorded by differential scanning calorimetry. The results show that the processabilities of m-BDB with 4-NH2-CN are superior to those with 2-NH2-CN and 3-NH2-CN due to higher self-catalytic efficiency and broader processing windows. Thermal stabilities were evaluated by thermogravimetric analysis, and the polymers with all these self-catalytic compounds exhibit excellent thermal and thermal-oxidative stabilities. Dynamic mechanical analysis reveals that these polymers have high storage modulus and high glass transition temperatures. The polymers of 4-NH2-CN show more outstanding processability, thermal stability, and dynamic mechanical properties than those of 2-NH2-CN and 3-NH2-CN and can be considered as a good candidate as a self-catalytic curing agent for high-temperature phthalonitrile polymers.

Polymers ◽  
2019 ◽  
Vol 11 (11) ◽  
pp. 1855 ◽  
Author(s):  
Li-wu Zu ◽  
Bao-chang Gao ◽  
Zhong-cheng Pan ◽  
Jun Wang ◽  
Abdul Qadeer Dayo ◽  
...  

Phenol-diaminodiphenylmethane-based benzoxazine (P-ddm)/phthalocyanine copolymer was prepared by using P-ddm resin as matrix and 3,10,17,24-tetra-aminoethoxy lead phthalocyanine (APbPc) as additive. Fourier-transform infrared (FTIR), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and thermogravimetric analysis (TGA) were used to investigate the curing behavior, curing kinetics, dynamic mechanical properties, thermal stability, and impact strength of the prepared copolymers. The kinetic parameters for the P-ddm/APbPc blend curing processes were examined by utilizing the iso-conversional, Flynn–Wall–Ozawa, and Málek methods. The P-ddm/APbPc blends exhibit two typical curing processes, and DSC results confirmed that the blending of APbPc monomer can effectively reduce the curing temperature of P-ddm resin. The autocatalytic models also described the non-isothermal curing reaction rate well, and the appropriate kinetic parameters of the curing process were obtained. The DMA and impact strength experiments proved that the blending of APbPc monomer can significantly improve the toughness and stiffness of P-ddm resin, the highest enhancements were observed on 25 wt.% addition of APbPc, the recorded values for the storage modulus and impact strength were 1003 MPa and 3.60 kJ/m2 higher, respectively, while a decline of 24.6 °C was observed in the glass transition temperature values. TGA curves indicated that the cured copolymers also exhibit excellent thermal stabilities.


2000 ◽  
Vol 73 (5) ◽  
pp. 864-874 ◽  
Author(s):  
T. Murakami ◽  
S. Kohjiya ◽  
Y. Ikeda ◽  
H. Urakawa ◽  
K. Kajiwara

Abstract Three viologen-type poly(tetramethylene oxide) (PTMO) ionenes with chloride anions (PTVs) were synthesized by living cationic polymerization, whose molecular masses of PTMO segments between the viologen units were 6100, 9800 and 12000 g/mol. The PTV films were elastomers and possessed the microphase-separated structure consisting of three phases, i.e., PTMO amorphous phase, PTMO crystalline phase and ionic aggregated phase. The effect of ionic content, i.e., the effect of molecular mass between the ionic segments on the higher-order structure and properties of the PTV films were investigated by differential scanning calorimetry, dynamic mechanical analysis, wide-angle X-ray diffraction and small-angle X-ray scattering (SAXS) measurements. The lower the ionic content was, the smaller the amorphous PTMO phase became and the more the long range-ordered structure of PTMO crystals of lamellae was regularly formed. This crystalline part significantly influenced the dynamic mechanical properties. The distance between the ionic domains became larger with the increase of the PTMO segments. The scattering peaks attributed to the crystalline phases and ionic domains were detected by SAXS for the PTV films whose molecular masses of PTMO segments were 9800 and 12000 g/mol. The distance between the ionic domains was changed little before and after the melting of PTMO crystals of PTV films.


2017 ◽  
Vol 24 (5) ◽  
pp. 691-697
Author(s):  
Behzad Shirkavand Hadavand ◽  
Hossein Hosseini

AbstractIn this study, the dynamic-mechanical properties and thermal behavior of the nanocomposites of a photocurable epoxy-acrylate resin and CuO nanohybrid were determined. In order to improve the dispersion of CuO nanoparticles and prevention of nanoparticle migration to the surface coating, the surface of commercial nanoparticles was modified by triethoxymethylsilane (TEMS) and vinyltrimethoxysilane (VTMS) as silane-coupling agents. Dynamic mechanical analysis (DMA), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC) tests were then performed on CuO-filled epoxy-acrylate resins to identify the loading effect on the properties of material. The thermal stability of nanocomposites was affected slightly after incorporation of CuO nanoparticles. DMA studies revealed that filling the CuO nanoparticles into epoxy-acrylate resin can produce a significant enhancement in storage modulus, as well as a shift in the glass transition temperature. The films reinforced with the modified CuO exhibit the most significant enhancements in properties.


2019 ◽  
Vol 39 (6) ◽  
pp. 508-514
Author(s):  
Yannan He ◽  
Zhiqiang Yu

Abstract The thermal and dynamic mechanical properties of epoxy composites filled with zirconium diboride/nano-alumina (ZrB2/Al2O3) multiphase particles were investigated by means of differential scanning calorimetry, dynamic thermo-mechanical analysis, and numerical simulation. ZrB2/Al2O3 particles were surface organic functional modified by γ-glycidoxypropyltrimethoxysilane for the improvement of their dispersity in epoxy matrix. The results indicated that the curing exotherm of epoxy resin decreased significantly due to the addition of ZrB2/Al2O3 multiphase particles. In comparison to the composites filled with unmodified particles, the modified multiphase particles made the corresponding filling composites exhibit lower curing reaction heat, lower loss modulus, and higher storage modulus. Generally speaking, the composites filled with 5 wt% modified multiphase particles presented the best thermal stability and thermo-mechanical properties due to the better filler-matrix interfacial compatibility and the uniform dispersity of modified particles. Finite element analysis also suggested that the introduction of modified ZrB2/Al2O3 multiphase particles increased the stiffness of the corresponding composites.


2011 ◽  
Vol 335-336 ◽  
pp. 120-123 ◽  
Author(s):  
Chang Su ◽  
Pan He ◽  
Li Huan Xu ◽  
Cheng Zhang

In this article, the damping mechanism of organic hybrids consisting of Nitrile Butadiene Rubber (NBR) and phenolic oligomer 4-methyl-pheno reaction products of both dicyclopentadiene and isobutylene (MPDI) were investigated by dynamic mechanical analysis (DMA). It was shown that NBR/MPDI blends exhibit only one damping peak, which shifted to higher temperature with the increase of MPDI content, and the maximum of tan δ peak decreased slightly when the ratio of NBR/MPDI was no more than 100/20, and then increased when the ratio rised from 100/20 to 100/80. Fourier transform infrared spectrum (FT-IR) showed that the hydrogen bond were formed between -OH of MPDI and a-H of NBR. X-ray diffraction (XRD) and differential scanning calorimetry (DSC) measurements indicated that MPDI exhibit amorphous features, which was compatible with the blends. These may imply that much more stable damping material with both higher tan δ peak and controllable damping peak position can be achieved.


Polymers ◽  
2020 ◽  
Vol 12 (2) ◽  
pp. 490
Author(s):  
Xing Huang ◽  
Songbo Chen ◽  
Songhan Wan ◽  
Ben Niu ◽  
Xianru He ◽  
...  

Poly (butyl methacrylate) (PBMA) was blended with a series of phenolic resins (PR) to study the effect of PR molecular weight on dynamic mechanical properties of PBMA/PR composites. Differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) found a similar variation of glass transition temperature (Tg). The maximum loss peak (tanδmax) improved in all PBMA/PR blends compared with the pure PBMA. However, tanδmax reduced as the molecular weight increased. This is because PR with higher molecular weight is more rigid in the glass transition zone of blends. The hydrogen bonding between PBMA and PR was characterized by Fourier transform infrared spectroscopy (FTIR). Lower molecular weight PR formed more hydrogen bonds with the matrix and it had weaker temperature dependence. Combined with the results from DMA, we studied how molecular weight affected hydrogen bonding and thus further affected tanδmax.


2018 ◽  
Vol 19 (7) ◽  
pp. 2032 ◽  
Author(s):  
Dongmei Han ◽  
Guiji Chen ◽  
Min Xiao ◽  
Shuanjin Wang ◽  
Shou Chen ◽  
...  

The blends of Poly(propylene carbonate) (PPC) and polyester-based thermoplastic polyurethane (TPU) were melt compounded in an internal mixer. The compatibility, thermal behaviors, mechanical properties and toughening mechanism of the blends were investigated using Fourier transform infrared spectra (FTIR), tensile tests, impact tests, differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and dynamic mechanical analysis technologies. FTIR and SEM examination reveal strong interfacial adhesion between PPC matrix and suspended TPU particles. Dynamic mechanical analyzer (DMA) characterize the glass transition temperature, secondary motion and low temperature properties. By the incorporation of TPU, the thermal stabilities are greatly enhanced and the mechanical properties are obviously improved for the PPC/TPU blends. Moreover, PPC/TPU blends exhibit a brittle-ductile transition with the addition of 20 wt % TPU. It is considered that the enhanced toughness results in the shear yielding occurred in both PPC matrix and TPU particles of the blends.


Author(s):  
Kristin L. Schaaf ◽  
Sia Nemat-Nasser

The essence of this research is to mitigate shock through material design. Here we seek to develop a thorough understanding of the material through experimental characterization methods that lend themselves to creating verifiable constitutive relations, all while working towards the development of a new blast resistant elastomeric composite material. The host elastomer, polyurea, is created by reacting Versalink P-1000 with Isonate 143L. This study evaluates the impact of both chemistry modifications and the integration of micro-scale additives on the polyurea material system properties and performance. The properties of the resultant elastomers and elastomeric composite materials are mechanically and thermally characterized using durometer testing, dynamic mechanical analysis (DMA) testing, and differential scanning calorimetry (DSC) testing in order to determine the hardness, storage and loss moduli, and glass transition temperature of the composites, respectively. Preliminary results indicate that the durometer and dynamic mechanical properties of the material can be significantly altered through such modifications. The work described here is part of an ongoing effort to develop and verify rules and tools for creating elastomer-based composite materials with optimally designed compositions and characteristics.


Materials ◽  
2021 ◽  
Vol 14 (19) ◽  
pp. 5538
Author(s):  
Yanbo Zhang ◽  
Yaqi Wu ◽  
Ming Yang ◽  
Gang Zhang ◽  
Haiyan Ju

Poly (ε-caprolactone) (PCL) and chitosan (CS) are widely used as biodegradable and biocompatible polymers with desirable properties for tissue engineering applications. Composite membranes (CS–PCL) with various blend ratios (CS:PCL, w/w) of 0:100, 5:95, 10:90, 15:85, 20:80, and 100:0 were successfully prepared by lyophilization. The thermal stabilities of the CS–PCL membranes were systematically characterized by thermogravimetric analysis (TG), dynamic thermogravimetry (DTG), and differential scanning calorimetry (DSC). It was shown that the blend ratio of PCL and CS had a significant effect on the thermal stability, hydrophilicity, and dynamic mechanical viscoelasticity of the CS–PCL membranes. All the samples in the experimental range exhibited high elasticity at low temperature and high viscosity at high temperatures by dynamic mechanical thermal analysis (DMTA). The performances of the CS–PCL membranes were at optimum levels when the blend ratio (w/w) was 10:90. The glass transition temperature of the CS–PCL membranes increased from 64.8 °C to 76.6 °C compared to that of the pure PCL, and the initial thermal decomposition temperature reached 86.7 °C. The crystallinity and porosity went up to 29.97% and 85.61%, respectively, while the tensile strength and elongation at the breakage were 20.036 MPa and 198.72%, respectively. Therefore, the 10:90 (w/w) blend ratio of CS/PCL is recommended to prepare CS–PCL membranes for tissue engineering applications.


2019 ◽  
Vol 19 (3) ◽  
pp. 545
Author(s):  
Siti Hasnah Kamarudin ◽  
Emiliana Rose Jusoh ◽  
Luqman Chuah Abdullah ◽  
Mohd Halim Shah Ismail ◽  
Min Min Aung ◽  
...  

This research aims to investigate the effect of crude palm oil (CPO) as a plasticizer in polypropylene blown film on thermal and dynamic mechanical properties. Polypropylene (PP) was blended with 1, 3, and 5% of CPO using a twin screw extruder. The extruded samples were blown using the blown thin film technique. The samples were analyzed using dynamic mechanical analysis (DMA), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). From the dynamic mechanical analysis, the storage modulus and loss modulus for PP presented decreasing pattern about 3–5% due to the action of CPO as plasticizer which introduced free volume and enabled the polyolefins chains to deform more easily. The glass transition temperatures (Tg) of PP were found being shifted to lower temperature from 10 to 1 °C with the increasing CPO content. The fraction of crystallization was determined using DSC. The thermogravimetric analysis (TGA) results showed that the incorporation of CPO as plasticizer showed a small increased effect in the thermal stability for PP. These findings have contributed new knowledge to the additives area and give important implications for designing and manufacturing polymer packaging materials.


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