Synthesis and properties of phthalonitrile-based resins containing spirocycle acetal

2020 ◽  
pp. 095400832097759
Author(s):  
Ke Li ◽  
Hua Yin ◽  
Kun Yang ◽  
Pei Dai ◽  
Ling Han ◽  
...  

Designing novel low-melting, high-rigidity phthalonitrile resin is of great significance in the current context of development. In this study, rigid spirocycle acetal structure was introduced into phthalonitrile to reduce the melting point and maintain their thermal stability. The chemical structure of resins was confirmed by nuclear magnetic resonance (NMR) spectrometry, matrix-assisted laser desorption/ionization time of flight (MALDI-TOF) mass spectrometry and Fourier-transform infrared (FTIR) spectroscopy. The curing behaviors were studied by differential scanning calorimetry (DSC). Thermal stability and mechanical properties of the cured resins were investigated by dynamic mechanical thermal analysis (DMTA) and thermogravimetric analysis (TGA). The processability was studied by rheological analysis. The results indicated the three monomers had a low melting temperature, wide processing windows and low viscosities. These polymers did not exhibit Tg from room temperature to 400°C, exhibited superb dynamic mechanical property and thermal stability.

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
M. Soccio ◽  
N. Lotti ◽  
L. Finelli ◽  
A. Munari

AbstractSeveral novel ether or thioether linkage containing aliphatic polyesters and poly(alkylene dicarboxylate)s were synthesized for comparison and characterized in terms of chemical structure and molecular weight. The thermal behavior was examined by thermogravimetric analysis and differential scanning calorimetry. All the polymers showed a good thermal stability, even though lower for the ether or thioether linkage-containing polyesters. The decrement of the thermal stability appears to be more relevant in the case of the presence of sulphur atoms. At room temperature the samples appeared semicrystalline, except PTTDG and PDEDG, which were viscous oils; the effect of the introduction of ether or thioether group was an increment of the Tgvalue, a decrement of the melting temperature and a significant decrease of the crystallization rate. The entity of the variations was found to be affected by the kind of group introduced, and the trend observed can be explained on the basis of atom electronegativity and dimensions


e-Polymers ◽  
2011 ◽  
Vol 11 (1) ◽  
Author(s):  
M. Soccio ◽  
N. Lotti ◽  
L. Finelli ◽  
A. Munari

AbstractSeveral novel ether or thioether linkage containing aliphatic polyesters and poly(alkylene dicarboxylate)s for comparison were synthesized and characterized in terms of chemical structure and molecular weight. The thermal behavior was examined by thermogravimetric analysis and differential scanning calorimetry. All the polymers showed a good thermal stability, even though lower for the ether or thioether linkage-containing polyesters. The decrement of the thermal stability appears to be more relevant in the case of presence of sulphur atoms. At room temperature the samples appeared semicrystalline, except PTTDG and PDEDG, which were viscous oils; the effect of the introduction of ether or thioether group was an increment of the Tg value, a decrement of the melting temperature and a significant decrease of the crystallization rate. The entity of the variations was found to be affected by the kind of group introduced, and the trend observed can be explained on the basis of atom electronegativity and dimensions.


2012 ◽  
Vol 727-728 ◽  
pp. 1552-1556
Author(s):  
Renata Barbosa ◽  
Dayanne Diniz Souza ◽  
Edcleide Maria Araújo ◽  
Tomás Jefférson Alves de Mélo

Studies of degradation have verified that the decomposition of some quaternary ammonium salts can begin to be significant at the temperature of about 180 ° C and like most thermoplastics are processed at least around this temperature, the thermal stability of the salt in clay should always be considered. Some salts are more stable than others, being necessary to study the degradation mechanisms of each case. In this work, four quaternary ammonium salts were characterized by differential scanning calorimetry (DSC) and thermogravimetry (TG). The results of DSC and TG showed that the salts based chloride (Cl-) anion begin to degrade at similar temperatures, while the salt based bromide (Br-) anion degrades at higher temperature. Subsequently, a quaternary ammonium salt was chosen to be used in organoclays, depending on its chemical structure and its thermal behavior.


2020 ◽  
Vol 1010 ◽  
pp. 274-279
Author(s):  
Syifa' Muhamad Sharifuddin ◽  
Mohd Shukri Mat Nor ◽  
Fathin Asila Mohd Pabli ◽  
Piyawadee Luangchuang ◽  
Wannarat Chueangchayaphan ◽  
...  

A study on polymer-ceramic composite, CaCu3Ti4O12 (CCTO) embedded in epoxidised natural rubber (ENR-25) were successfully fabricated through mixing method using an internal mixer and two-roll mill followed by hot-pressed via compression moulding for a potential electronic device such as a flexible capacitor. CCTO powders were successfully synthesised through a solid-state reaction and calcined at 900 °C for 12 hours. The ENR-25 was blended with 0, 20, 40, 60, 80, 100, and 120 phr (part per hundreds of rubber) of CCTO powders. Thermal stability and degradation are crucial properties for the composite based polymer. Therefore, thermogravimetric and differential scanning calorimetry (TGA/DSC) used to find out the thermal reaction and degradation mechanism of CCTO/ENR-25 composites. Besides, dynamic mechanical analysis (DMA) also used to investigate glass transition temperature (Tg) and storage modulus. TGA/DSC showed a two-step degradation mechanism with increasing thermal stability over increasing filler content of CCTO and only showed a major endothermic reaction. However, for DMA there is no significant difference in Tg value between each composite but showed high storage modulus up to 4398 MPa for 120 phr. High storage modulus indicates the high stiffness of the composite. In conclusion, the addition of filler content will show high thermal stability, storage modulus, and stiffness of CCTO/ENR-25 composites.


2019 ◽  
Vol 27 (9) ◽  
pp. 567-581 ◽  
Author(s):  
RDS Zwane ◽  
ER Sadiku ◽  
SS Ray ◽  
NE Luruli

Thermal and rheological properties of polyamide 6/layered double hydroxide (PA6/LDH) composites were studied. Pristine (U-LDH) and organically modified (M-LDH) clays were used in this study. Some evidence of intercalation was observed on the microstructure of PA6/M-LDH samples, while PA6/U-LDH was characterised by microcomposite morphology as shown by the transmission electron microscopy results. The scanning electron microscopy results showed a complete delamination of the M-LDH in the PA6 matrix while U-LDH was evenly dispersed as immiscible tactoids. In the melt state, the M-LDH had a significant influence on the melt microstructure of PA6 matrix when compared to U-LDH. Differential scanning calorimetry results, both dynamic and isothermal experiments, showed that LDH had a heterogeneous nucleating effect on the PA6 matrix, with the U-LDH showing better nucleating effect when compared to M-LDH. The thermogravimetric analysis results showed that M-LDH had a negative influence on the thermal stability of the composites, while U-LDH improved their thermal stability. The X-ray diffraction and dynamic mechanical analysis results showed that the presence of M-LDH promoted the formation of γ-crystallites in the PA6 matrix, while U-LDH composites were dominated by the α-crystallites. This phenomenon had a positive correlation with increasing content of both LDH clays. An overall improved dynamic mechanical properties were observed for PA6/U-LDH when compared to PA6/M-LDH composites.


2011 ◽  
Vol 23 (7) ◽  
pp. 513-517 ◽  
Author(s):  
Mohsen Ghorbani ◽  
Mohammad Soleimani Lashkenari ◽  
Hossein Eisazadeh

This study investigated the preparation and properties of polyaniline/silver (PAn/Ag2O) nanocomposite in aqueous media by chemical polymerization of aniline in the presence of ammonium peroxydisulphate as an oxidant. The products were investigated in terms of morphology, chemical structure, thermal stability and thermal degradation using scanning electron microscopy, Fourier transform infrared, thermal gravimetric analysis and differential scanning calorimetry, respectively. The results indicated that the properties of products were dependent on the nanocomposite structure.


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.


Molecules ◽  
2020 ◽  
Vol 25 (21) ◽  
pp. 5212
Author(s):  
Jaroslav Charvot ◽  
Daniel Pokorný ◽  
Milan Klikar ◽  
Veronika Jelínková ◽  
Filip Bureš

The current portfolio of organoselenium compounds applicable as volatile precursors for atomic layer deposition can be denoted as very limited. Hence, we report herein facile and cost-effective preparation of two bis(trialkylstannyl)selenides as well as one selenole and three bis(trialkylsilyl)selenides. Their syntheses have been optimized to: (i) use readily available and inexpensive starting materials, (ii) involve operationally simple methodology (heating in a pressure vessel), (iii) use a minimum amount of additives and catalysts, and (iv) either exclude additional purification or involve only simple distillation. The chemical structure of prepared Se derivatives was confirmed by multinuclear NMR and GC/MS. Their fundamental thermal properties were investigated by differential scanning calorimetry (DSC) and TGA methods that revealed thermal stability within the range of 160–300 °C.


2019 ◽  
Vol 70 (2) ◽  
pp. 149-155
Author(s):  
Mohammad Ahmadi ◽  
Bita Moezzipour ◽  
Aida Moezzipour

In this study, thermal stability of fibers obtained from recycled MDF was investigated and compared with virgin fibers by using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Two different methods, including electrical heating and hydrothermal treatment, were used for recycling the MDF wastes. Electrical heating method was performed at two different times (2 and 4 min) and hydrothermal method was done at three different temperatures (105, 125 and 150 °C). Chemical structure of wood fibers was also studied. TGA and DSC analysis showed higher weight loss of recycled fibers as compared to virgin fibers in a similar degradation region, which means that thermal stability of recycled fibers is lower than virgin fibers. In fact, thermal behavior of recycled fibers was medium between wood and UF resin. DSC analysis showed two exotherms at around 340 and 475 °C. The transition at around 340 °C in fibers thermogram was considered to be due to polysaccharides thermal deterioration and the exotherm at 475 °C was related to lignin carbohydrate complex deterioration. The results of chemical structure analysis showed that lignin and hemicellulose content of recycled fibers was significantly lower than that of virgin fibers, which resulted in decreased thermal stability.


e-Polymers ◽  
2020 ◽  
Vol 20 (1) ◽  
pp. 500-509
Author(s):  
Dayong Zhang ◽  
Xiaohui Liu ◽  
Xuefeng Bai ◽  
Yinyin Zhang ◽  
Gang Wang ◽  
...  

AbstractA new type of phthalonitrile-etherified resole resin (PNR) was synthesized from resole resin and 4-nitrophthalonitrile. The differential scanning calorimetry results showed that the curing temperature of PNR is lower than that of phthalonitrile resin. Excellent thermal stability and bonding properties were obtained after curing at 220°C. TGA showed that in air, the temperature of 5% weight loss (T5%) of the cured PNR was 446°C, approximately 41°C higher than that of resole resin (RS), and the char yield at 800°C increased from 4% for RS to 33% for PNR. The shear strengths of PNR at room temperature and high temperature were increased by 8% and 133%, respectively, over those of RS, and after aging at 350°C for 2 h, these values were increased by 262% and 198%, respectively, over those of RS. Its excellent curing behavior, heat resistance and high bonding strength show that PNR can be used as a high temperature-resistant adhesive.


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