Char Yield Research Articles

Structure and Properties of Thermally Stabilized and Ecologically Friendly Organic Cotton Fibers as a New Activated Carbon Fiber Precursor

Organic cotton precursor yarn was impregnated in an aqueous solution consisting of diammonium hydrogen phosphate (DAP), boric acid (BA), and urea (U) mixtures before the thermal stabilization stage and then subjected to heat treatments in an air environment at 245 °C. The effect of chemical pretreatment on organic cotton yarn was examined using methods such as X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and infrared (IR) spectroscopy. The XRD analysis revealed a gradual decrease in the crystalline structure, attributed to the disruption of intermolecular hydrogen bonds. DSC and TGA measurements showed an improved thermal stability due to the formation of pre-graphitic structures with aromatic entities at higher temperatures. For samples chemically impregnated and then stabilized, the char yield values increased from 25% to 68% at 500 °C and 23% to 53% at 1000 °C. Analysis of IR spectra indicated a gradual reduction in both intermolecular and intramolecular hydrogen bonds associated with dehydration and dehydrogenation reactions. The IR spectra also confirmed a decrease in crystallinity with increasing oxidation time, which is consistent with the findings from X-ray diffraction. In addition, the IR spectra showed the presence of C = C bonds, indicating the formation of a crosslinked ladder-like structure. The results showed that DAP-BA-U integration increased the thermal stability of organic cotton fibers and the obtained samples were ready for the next stage, carbonization.Graphical

Controllable construction of mesoporous hollow carbon spheres rich in micropores from waterborne benzoxazine and their application in supercapacitors

Mesoporous hollow carbon spheres (MHCSs) with mesoporous channels and nanocages structure have unique advantages in energy storage. However, this structure alone does not significantly enhance the electrochemical double layer capacitance (EDLC). Additionally, the current hydrophobic nature of polymer precursors with high char yield impedes effective binding with templates due to polarity differences. Moreover, the use of toxic organic solvents presents obstacles to further development. So, it remains a challenge to prepare MHCSs rich in micropores using polar polymers with high char yield in green solvent. In this work, we prepared MHCSs rich in micropores (MMHCSs) using waterborne benzoxazine as a carbon sources and dendritic/fibrous nano-silica as a sacrificial hard template using water as the solvent and combined with freeze-drying, curing, carbonization and an activation step. The optimal MMHCSs (MMHCSs306–1–7000.5h) has a large specific surface area (1057 m2 g−1), and has a maximum specific capacitance value near 221.45 F g−1 at 0.5 A g−1 in a three-electrode system, the specific capacitance still reaches 156.66 F g−1 at a high current density (20 A g−1) due to the full utilization of micropores in the presence of mesoporous-shell and hollow-core. When assembled into a symmetrical supercapacitor, the energy density reaches 5.91 Wh kg−1 when the power density is 137.5 W kg−1. The study provides an eco-friendly method for preparing MMHCSs, and the unique structure has potential application in supercapacitors.

Highly stable mesoporous Co/Ni mixed metal-organic framework [Co/Ni(μ3-tp)2(μ2-pyz)2] for Co (II) heavy metal ions (HMIs) remediation

A bimetallic cobalt/nickel-based metal-organic framework (MOF), [Co/Ni(μ3-tp)2(μ2-pyz)2], denoted as Co/Ni-MOF, has been successfully prepared by a hydrothermal method. The MOF was prepared by incorporating mixed O− and N− donor ligands, specifically terephthalic acid (tp) and pyrazine (pyz). The Mesoporous Co/Ni-MOF was comprehensively characterized using various analytical methods such as XRD, BET, FT-IR, TGA (23 % char yields), SEM, and EDS analyses. The synthesized mesoporous Co/Ni-MOF was then used to absorb Co (II) from aquatic areas efficiently. Several critical parameters, such as the beginning Co (II) concentration (25–150 mg/L), the effect of pH (2–10), the duration of time (5–30 min), and the amount of adsorbent (0.003–0.02 g), were systematically investigated. Remarkably, the Mesoporous Co/Ni MOF displayed a significant adsorption capacity of 372.66 mg g−1 in the optimum conditions, including pH = 6, amount of adsorbent = 0.003 g, duration of time = 25 min, and beginning Co (II) concentration = 150 mg/L. Adsorption data from the experimental studies of the mesoporous Co/Ni MOF are matched based on the non-linear pseudo-first-order (PSO) kinetic model (R2 = 0.9999), and a chemical process is suggested for chemisorption. Furthermore, the adsorption isotherms of Co (II) heavy metal ions (HMIs) are an excellent fit with the non-linear Temkin, indicating that they explain the sorbent/sorbate interactions concerning the heat of adsorption. It is evident from the thermodynamic parameters that adsorption is a spontaneous and favorable exothermic process. These results highlight the promising adsorption performance and potential applications of the mesoporous Co/Ni-MOF as an effective adsorbent for Co (II) elimination from aquatic areas. Four-cycle regeneration studies were the most effective for the Co (II) under study.

Conversion of municipal garden waste to activated carbon: Laboratory production and characterization comparing production parameters

This research aims to investigate the potential of the municipal garden waste as a new precursor to generate activated carbon by CO2 activation. TGA analysis shows the distinctive thermal degradation nature of garden waste. The activation of the garden waste enhanced its surface area where well-developed internal micro-mesoporous structure is also noticed. The results suggest that most of the volatiles decomposed at temperatures beyond 450 °C. A decrease in char yield, increase in surface area and pore volume and weakening of oxygen and hydrogen-containing groups were observed at higher pyrolysis temperatures. Raman and XRD support the amorphous and porous graphitic structure of carbon. Carbonization temperature of 500 °C and activation temperature of 800 °C were shown to produce the better-quality AC where highest surface area of 363.32 m2/g and highest pore volume of 0.095 cm3/g was achieved. Compared to the pyrolysis temperature, pyrolysis steps did not have notable contribution to the AC characteristics.

Synthesis and Polymerization of the Bio‐Benzoxazine Derived from Resveratrol and Thiophenemethylamine and Properties of its Polymer

AbstractResveratrol and 2‐thiophenemethylamine have been employed in the synthesis of a novel tri‐functional benzoxazine (RES‐th) to develop the bio‐benzoxazine monomer. The chemical structure of the synthesized monomer is confirmed by various characterization technics. The polymerization behavior is monitored by in situ Fourier transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). The in situ FTIR results reveal distinct reaction mechanisms for the three oxazine rings presented in RES‐th, with both ether and phenolic Mannich bridge structures observed in the products. The activation energy values of RES‐th are calculated to be 119.05, 120.97, and 119.44 kJ mol−1 by Kissinger, Ozawa, and Starink methods, respectively, which are all based on the heat flow curves at various heating temperatures. The thermal stability and flame retardancy of the resulting polybenzoxazine (poly(RES‐th)) are investigated by thermogravimetric analysis (TGA) and microscale combustion calorimeter (MCC). The values of Td5 and Td10 of polybenzoxazine are found to be 356 °C and 399 °C, respectively, with a char yield of 66.3% at 800 °C. The prepared polybenzoxazine also demonstrates nonflammability characteristics with the values of heat release capacity (HRC) and total heat release rate (THR) of 18.65 J (g K)−1 and 2.69 kJ g−1, respectively. These findings suggest that the thermoset, poly(RES‐th), is a promising candidate for fire‐resistant applications.

Phenyl propyl polysiloxane modified epoxy resin I: The content, phase structures and macroproperties

Polysiloxanes are known to significantly enhance the toughness and thermal stability of epoxy resins. However, the study of phase transitions and their effects on the properties of modified resins, synthesized through copolymerization or blending, was quite limited. In this work, a phenyl propyl polysiloxane (PPPS) modified epoxy resin (P/E) was prepared using a solvent method to scrutinize the influence of varying PPPS concentrations and phase transitions on the macroscopic properties of the resin. The molecular structure of P/E composite was confirmed through Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (1H and 29Si NMR) analysis. Based on atomic force microscopy (AFM) results, the progression of phase transitions was deduced: from a homogeneous phase to a co-continuous phase, and subsequently to a sea-island phase. This progression of phase transitions is attributed to the varying solubility of the copolymer with different PPPS content in the resin. At a PPPS content of 20 wt%, a significant improvement in tensile strength (σ) and critical strain energy release rate (GIc) was observed, increasing by 45 % and 400 %, respectively, upon the formation of a co-continuous phase. The presence of a silicone-rich spherical domain within sea-island phase can significantly improve the GIc of the resins, while this also results in a rapid reduction in tensile strength (σ). Furthermore, the thermal stability of P/E composite is also affected by its phase structures. The silicone-rich spherical domains are more effective in forming a protective layer compared to the co-continuous phase, which leads to a decreased pyrolysis rate and an increased yield of residual char. This work elucidates the influence of PPPS content and phase structure on the macroscopic properties, highlighting the significant potential for developing composite materials with superior comprehensive performance.

Multi‐objective optimization of hybrid polypropylene composites for enhanced mechanical, thermal, and flame‐retardant properties

AbstractOptimizing composite materials is crucial for engineering advancements because it allows for the creation of materials tailored to specific functional requirements, thereby enhancing efficiency, safety, and sustainability. This study examines both the combined and individual effects of long flax fiber (LFF) bundles, short basalt fibers (BF), and rice husk powder (RHP) on the properties of polypropylene (PP) hybrid composites. LFF primarily provides mechanical strength, BF enhances mechanical, thermal, and flame‐retardant properties by filling gaps, and RHP reinforces and improves the overall composite. Contrary to previous studies that relied on random combinations, this research employs a systematic Box–Behnken design (BBD) for three variables: LFF plies, BF, and RHP by weight percentage. This approach facilitated the development of a new second‐order regression equation via response surface methodology (RSM), clarifying the contribution of each component, with R2 values exceeding 0.85, indicating high predictability. Optimization, conducted using a non‐dominated sorting genetic algorithm (NSGA‐II), demonstrated that the optimal composites significantly outperformed the non‐optimized ones in mechanical strength, thermal stability, and flame retardancy. Compared to the average values before optimization, improvements post‐optimization included increases of 49.86% in tensile strength (TS), 38.82% in TS modulus, 73.93% in char yield (YC), and 29.81% in peak heat release rate (pHRR). Specifically, the fire performance index improved by 237.5% and the fire growth index by 101.33%, compared to pure PP, highlighting significant advancements in fire safety. This study shows that mathematical equations can predict composite properties, helping to select balanced compositions without sacrificing flammability.Highlights Multi‐filler approach technique used for manufacturing of PP composites. LFF, BF & RHP optimize mechanics & flammability. Box–Behnken design predicts optimal composition for superior properties. NSGA‐II optimization improves tensile, thermal & flame retardant properties.

Supersonic hot jet ablative testing and analysis of boron nitride nanotube hybrid composites

Boron nitride nanotubes (BNNTs) are high-strength, high-modulus nanotubes with high thermal and oxidative stabilities. Two hybrid composites were prepared with satin weave carbon fiber (CF) and resole-type phenolic resin: one with surface layers of BNNTs and one with alternating interlayers of BNNTs. The samples were subjected to hot jet tests that simulate realistic high-pressure-temperature conditions to understand the behavior of BNNTs under high-pressure erosion. Adding BNNTs to CF/phenolic laminates enhanced the ablation resistance by reinforcing the char material and mitigated localized thermal damage. Hybrid laminates exhibited up to 14 % lower weight loss, 55 % increase in flexural modulus, higher thermal diffusivity, and improved char yield and microstructure compared to CF/phenolic samples. The surface layer hybrid had many surviving nanotubes reinforcing the char and crystalline oxide structures that could mitigate further oxygen diffusion. Various characterization methods were used to deduce possible mechanisms and their products, indicating that BNNTs could serve as growth templates for direct crystalline boron oxide formation. Overall, hybrid BNNT/CF/phenolic laminates displayed better ablation resistance and favorable microstructure evolution under high-pressure conditions.

Bio-oil production from the catalytic pyrolysis of raw and torrefied corn waste by using MgO and CaO catalysts

Abstract This research investigates the influence of torrefaction and catalytic pyrolysis of raw corn waste (RCW) to upgrade the quality of bio-oil. RCW was torrefied at 280°C for 16 mins to produce torrefied corn waste (TCW). Natural basic oxides (CaO and MgO) catalysts were selected because of inexpensive and high catalytic performance. Pyrolysis experiments were conducted in a bench-scaled bubbling fluidized bed reactor at 500°C. The effects of torrefaction and the presence of a catalyst on the pyrolysis product both yield and composition were investigated. The results from non-catalytic pyrolysis revealed that TCW pyrolysis gave 15 wt.% lower in oil yield, and about 6.8 wt.% lower in gas yield but the char yield was approximately 22 wt.% higher compared to the pyrolysis of RCW. Considering the effect of catalyst, the yield of bio-oil reduced slightly, while the yield of char and gas increased compared to non-catalytic pyrolysis for both RCW and TCW. The bio-oil composition derived from TCW pyrolysis contained more phenolic and aromatic compounds and significantly lower oxygenated compounds when compared to that of RCW pyrolysis. Moreover, with the presence of the catalysts, the bio-oil composition and HHVs of bio-oil was also improved.

Five-Axis Additive Manufacturing of a Thermoset Composite Formulation for Thermal Protection Systems

Thermal protection systems (TPS) are employed on space vehicles to protect against the heat fluxes faced upon re-entry to the Earth’s atmosphere. This work reports a method of 3D printing composite materials for TPS to reduce the time and cost associated with hand layup production methods. A phenolic resin system was tested to determine char yield, viscosity, cure behavior and cure evolutions. A commercial 3D printer was modified to move along two additional axes to accommodate the complex curves of typical heat shields on space vehicles. This technique can be scaled to produce full-sized TPS for industrial applications.

Analysis of Performance of Additively Manufactured Reinforced Ablatives

This study investigates reentry conditions for Mars missions, focusing on extreme anaerobic heating. This work studies poly(ether ketone ketone) (PEKK), a high-performance thermoplastics polymer, in both small-scale laboratory and simulated oxyacetylene test bed conditions to eliminate low-performing polymeric materials. Previous research demonstrated PEKK’s superior ablation performance compared to poly(ether ether ketone) (PEEK) and polyetherimide. The aerothermal performance of neat PEKK can be further enhanced with reinforcement materials. This work explores PEKK composite materials reinforced with additives such as carbon nanotubes (CNTs), carbon fibers (CFs), and glass fibers (GFs). The CNT-reinforced (10%wt) PEKK exhibited the highest char yield (69%wt) during thermogravimetric analysis (TGA) in nitrogen, superior to the short CF-reinforced PEKK. Various CF and GF loadings (10% and 20%wt) were tested for their thermophysical and aerothermal performance. Oxyacetylene tests (OTBs) under fuel-rich conditions further validated the results. Except for 10% CF PEEK, the mass loss in OTB tests correlated with TGA and thermal diffusivity measurements. The addition of CF/GF in PEKK enhanced thermal effusivity, but it also led to significant swelling due to increased conductive flux and reduced ablated heat flux. Among the tested materials, CNT-reinforced PEKK displayed the highest char yield, lowest mass loss, and minimal swelling. The unique porous structure of CNTs minimized char expansion and erosion during the OTB tests, making a promising material for reentry flights.

An analytical characterization study on biofuel obtained from pyrolysis of Madhuca longifolia residues

The current study focuses on examining the characteristics of biofuel obtained from the pyrolysis of Madhuca longifolia residues, since the selected forest residue was primarily motivated by its greater volatile matter content. The study used several analytical techniques to describe pyrolysis oil, char, and gas obtained from slow pyrolysis process conducted between 350 and 600 °C in a fixed-bed reactor. Initially, the effect of process temperature on product distribution was assessed to motivate maximum pyrolysis oil yield and found to be 44.2 wt% at pyrolysis temperature of 475 °C, while the yields of char and gas were 22.1 wt% and 33.7 wt%, respectively. In order to determine the suitability of the feedstock, the Madhuca longifolia residues were analyzed by TGA and FT-IR, which revealed that the feedstock could be a feasible option as an energy source. The characterization of pyrolysis oil, char, and gas has been done through various analytical methods like FT-IR, GC-MS, and gas chromatography. The physicochemical characteristics of the pyrolysis oil sample were examined, and the results showed that the oil is a viscous liquid with a lower heating value than conventional diesel. The FT-IR and GC-MS analysis of pyrolysis oil revealed the presence of increased levels of oxygenated chemicals, acids, and phenol derivatives. The findings of the FT-IR analysis of char indicated the existence of aromatic and aliphatic hydrocarbons. The increased carbon content in the char indicated the possibility of using solid fuel. Gas chromatography was used to examine the chemical structure of the pyrolysis gas, and the results showed the existence of combustible elements.

Producing ablative thermal protection systems by additive manufacturing

Aerospace vehicles that undergo atmospheric re-entry require thermal protection systems (TPS) to protect them from the extreme environment. Currently, TPS production relies on hand layup techniques which are time-, cost-, and energy-intensive. A method to produce composite TPS via additive manufacturing (AM) is demonstrated, which uses a custom-designed formulation. Thermal characterization of the composite system showed that char yield values were comparable to ablative systems presently used in TPS. Printability was demonstrated by in situ deposition onto a rotating/tilting aluminum substrate. A five-axis printer system was developed/adapted to accommodate the contours of TPS substrates and to enable the extrudate to completely cover leading edges of vehicle control surfaces.

Study on pyrolysis of ultra-high-quality oil shale: product characterization and a utilization process

ABSTRACT Nantun (NT) oil shale of ultra-high oil yield (>30%) is rare in the world, while the characteristics of this kind of oil shale are not widely reported. An oil shale pyrolysis experiment has been conducted in a tube furnace. The products of gas, oil and char are collected and analyzed on their yield and properties in the range of 450 to 650°C. The oil yield remained above 30% in the range of 450 to 550°C and decreased rapidly from 30.84% to 9.35% at 550 to 650°C. The char yield drops from 66.14% to 57.94% as the pyrolysis temperature increases, and aliphatic hydrocarbon components in char have been cracked completely at 450°C. The yield of pyrolysis gas rises as the pyrolysis temperature increases. CO accounts for the largest proportion of pyrolysis gas, with a volume fraction of over 70%. Based on the characteristics of pyrolysis products, an ultra-high-quality oil shale pyrolysis and utilization process and an Aspen Plus simulation model have been developed that provides estimated material and energy equilibriums for an industrial self-sustaining pyrolysis process to produce char and shale oil. This process can produce 0.61 kg oil and 0.29 kg char per kilogram of oil shale under self-sustaining conditions at 500°C. In practical applications, the pyrolysis temperature is recommended to be 500°C.

A comprehensive enhancement of the optical, mechanical, low dielectric, and flame-retardant characteristics of epoxy resin by the incorporation of multifunctional additive

Epoxy resin is widely utilized but faces the drawback of flammability. However, adding flame retardants often results in the compromise of other properties, such as mechanical and optical characteristics. In this study, a phosphorus-nitrogen multifunctional flame retardant named DPVPI was successfully synthesized. The resulting epoxy resin containing DPVPI demonstrated good transparency and low dielectric constant. Furthermore, the unique structure of DPVPI led to additional enhancements in the mechanical properties of EP composite. The tensile strength of EP composite was increased by 33 %, and the impact strength was improved from 13.61 kJ/m² to 25.74 kJ/m². Remarkably, the composites with Only 4wt% DPVPI can achieve a V-0 rating in the UL-94 test and the maximum limiting oxygen index (LOI) of it reached 32.6 %. The cone calorimeter test showed that the peak heat release of the composites with a 5 wt% addition decreased by 35 %, the total smoke release decreased by 37 %, and the char yield doubled. This research presents a novel strategy for subsequent synthesis endeavors about multifunctional flame retardants.

Selective Capturing of the CO2 Emissions Utilizing Ecological (3-Mercaptopropyl)trimethoxysilane-Coated Porous Organic Polymers in Composite Materials.

Capturing carbon dioxide (CO2) is still a major obstacle in the fight against climate change and the reduction of greenhouse gas emissions. To address this problem, we employed a simple Friedel-Crafts alkylation to investigate the effectiveness of porous organic polymers (POPs) based on triphenylamine (TPA) and trihydroxy aryl terms derived from chloranil (CH), designated as TPA-CH POP. We then treated the TPA-CH POP with (3-mercaptopropyl)trimethoxysilane (3-MPTS), forming a TPA-CH POP-SH nanocomposite to enhance CO2 capture. Utilizing FTIR, solid-state NMR, SEM, TEM, along with XPS techniques, the molecular makeup, morphological characteristics, as well as physical features of TPA-CH POP and the TPA-CH POP-SH nanocomposite were thoroughly explored. Upon scorching to 800 °C, the TPA-CH POP-SH nanocomposite demonstrated more thermal durability over TPA-CH POP, achieving a char yield of up to 71.5 wt.%. The TPA-CH POP-SH nanocomposite displayed a 2.5-times better CO2 capture, as well as a comparable adsorption capacity of 48.07 cm3 g-1 at 273 K. Additionally, we found that the TPA-CH POP-SH nanocomposite exhibited an improved CO2/nitrogen (N2) selectivity versus the original TPA-CH POP. Typical enthalpy changes for CO2 capture were somewhat increased by the 3-MPTS coating, indicating greater binding energies between CO2 molecules and the adsorbent surface. Our outcomes demonstrate that a TPA-CH POP composite coated with MPTS is a viable candidate for effective CO2 capture uses. Our findings encourage the investigation of different functional groups and optimization strategies.

Mechanical and thermal properties of fumed silica‐incorporated silane‐terminated urethane/epoxy‐interpenetrating polymer network nanocomposites

AbstractIn this study, it was aimed to improve the mechanical and thermal properties of epoxy materials based on diglycidyl ether of bisphenol‐A‐based. For this purpose, three different nanocomposite materials were prepared at various ratios including a fumed silica nanoparticle‐reinforced epoxy nanocomposite (FSN), an epoxy/silane‐terminated urethane (STU) hybrid interpenetrating polymer network (IPN) nanocomposite (SHIN), and a fumed silica‐reinforced epoxy/STU hybrid IPN nanocomposite (FSHIN). While synthesizing SHIN, 3‐isocyanato propyl trimethoxy silane (ICPTMS) and poly (hexamethylene carbonate) diol were used. The synthesized STU polymer chains were crosslinked by reacting them with TEOS via the sol–gel process. Therefore, hybrid networks were obtained. Moreover, fumed silica nanoparticles were incorporated into the hybrid networks via the sol–gel process for FSHINs. The three different nanocomposite materials exhibited much more improved properties than the neat epoxy. The most prominent nanocomposite was FSHIN. In comparison with the neat epoxy, Young's modulus, ultimate tensile strength, and Izod impact resistance values increased at ratios of 53%, 50%, and 223%, respectively. Glass transition temperature values and char yield values increased substantially in all nanocomposites. However, thermal decomposition temperatures increased only for FSNs. Moreover, these values for FSHINs that were very close to those of the neat epoxy were considerably higher than those of SHINs.Highlights Fumed silica‐incorporated silane‐terminated urethane/epoxy IPN nanocomposites. Substantially improved mechanical properties and impact resistance. Improved thermal stability.

In-situ catalytic upgrading of lignin pyrolysis volatiles over red mud

Red mud (RM) is a solid waste of Bayer's alumina industry production process, which comprises a mixture of diverse minerals. After calcination, the minerals in RM are present in the form of oxides, exhibiting remarkable catalytic performance for biomass pyrolysis. It is thought that pyrolysis of lignin generates renewable aromatic chemicals. In this paper, the effect of in-situ catalysis of calcinated RM on the distribution of lignin pyrolysis volatile products is investigated. In addition, upgrading of tar by components in RM, including SiO2, Al2O3, Fe2O3, and Na2O is also discussed. The results show that the addition of RM in lignin pyrolysis leads to lower char yield and higher gas yield. RM catalyzes the breaking and rearrangement of methoxy groups and induces the generation of hydroxyl groups, which leads to an increase from 1.96 to 3.96 wt% in monophenol content of the tar. Furthermore, the activation of C-O bonds by Fe2O3 and the redox properties of Fe2O3 (FeSi) combine to stimulate the production of monophenols and aldehydes by 30.8 % and 148.2 %, while Al2O3 (AlSi) boosts the production of guaiacols by 32.0 % comparing with SiO2 (Si). It is found that synergistic effect between multiple species improves the catalytic performance, the yield of tar reaches 24.5 wt% and the selectivity of oxygenated compounds achieves 94.4 % (FeAlSiNa). The catalytic performances of RM for product yield and tar component distribution are similar to that of FeSi, indicating that Fe2O3 and SiO2 play a main catalytic role in RM.

Study on the curing characteristics and properties of phthalonitrile resin cured with organic guanidine

Bisphenol A-based phthalonitrile resin was synthesized by nucleophilic substitution reaction from bisphenol A and 4-nitrophthalonitrile, and then the obtained resin was cured with sulfaguanidine as a novel curing agent. The curing characteristics, kinetics, thermal stability and dynamic mechanical property were studied by standard thermal analysis techniques including DSC, TGA, and DMA. The peak temperature of exothermic peak ( Tp) and apparent activation energy ( Ea) of sulfaguanidine cured phthalonitrile resin were 263.20°C and 76.6 kJ·mol−1 respectively, much lower than those of traditional aromatic diamine cured resin. Moreover, the resin cured by sulfaguanidine showed excellent thermomechanical properties and thermal stability. The glass transition temperature ( Tg) was 284.8°C, the initial thermal decomposition temperature ( Td,5%) was 439.6°C, and the char yield at 800°C was 62.1% in nitrogen atmosphere. To sum up, organic guanidine cured phthalonitrile resin exhibits excellent curing characteristics (low Tp and Ea) and high thermal properties, which provides a promising approach to preparing phthalonitrile resin with high comprehensive performance.

Preparation and characterization of a novel allyl ether naphthalene phenolic modified bismaleimide resin and its composites

AbstractAllyl ether naphthol resin (ANPF) was synthesized by introducing 1,5‐dihydroxynaphthalene and 2,7‐dihydroxynaphthalene into phenolic resin and was copolymerized with 4,4′‐bismaleimidodiphenylmethane resin (BDM) to obtain allyl ether naphthol‐modified bismaleimide resins (15‐ANPF‐BDM and 27‐ANPF‐BDM). The resulting thermal stability and glass transition temperature (Tg) were explored by thermogravimetric and dynamic mechanical analyses. The char yield of 15‐ANPF‐BDM at a temperature of 800°C was 46.0%. Additionally, the Tg of 15‐ANPF‐BDM was measured as 311°C, which is an increase of 44°C compared to that of c. The mechanical properties of the ANPF‐BDM/quartz fiber (Qf) composites were also investigated. The results reveal that ANPF‐BDM/Qf composites exhibit similar mechanical strength to APF‐BDM/Qf composites at room temperature. In addition, the mechanical properties of the ANPF‐BDM/ Qf composites demonstrated significant improvement in mechanical properties retained significantly improved at 200°C, with a 68% flexural strength retention and a 96% interlaminar shear retention of 15‐ANPF‐BDM/Qf composites. Thus, ANPF‐BDM/Qf composites exhibit outstanding mechanical properties at 200°C.