Isolation and characterization of cellulose nanowhiskers from Acacia caesia plant

Acacia caesia (L.) Willd (soap bark) fiber is an abundant natural resource, that is rich in cellulose. The study reports the effective utilization of underutilized Acacia caesia fiber for the isolation of nanocellulose whiskers. The nanocellulose whiskers were isolated successfully from Acacia caesia fibers by following alkali, bleaching, and sulfuric acid treatment. The obtained nanocellulose whiskers were carefully investigated for its chemical composition, structure, morphology, crystallinity, and thermal stability. The chemical composition and Fourier transform infrared spectra of nanocellulose whiskers showed the elimination of the non-cellulosic parts present in the raw Acacia caesia fibers. The X-ray diffraction analysis showed an upsurge in the crystallinity of the cellulose fibers after the chemical treatments. The isolation of nanocellulose whiskers from Acacia caesia raw fiber was confirmed by electron microscopy analysis. The thermogravimetric analysis showed remarkably high char residue for the nanocellulose whiskers compared to raw fibers. Based on the properties of nanocellulose whiskers, it can be concluded that the nanocellulose whiskers produced from Acacia caesia raw fibers are potential reinforcing material for developing high-performance green composites.     

Antibacterial and thermomechanical properties of composites of polylactic acid modified with capsicum oleoresin-impregnated nanoporous silica

Biodegradable composite films of poly(lactic acid) (PLA) modified with varying amounts of capsicum oleoresin (CO)-impregnated nanoporous silica (SiCO) were prepared. The antimicrobial and thermomechanical properties of the PLA composites were carefully investigated. The Gram-positive pathogenic bacteria (Staphylococcus aureus and Bacillus) and the Gram-negative pathogenic bacteria (Escherichia coli and Salmonella enterica) tests established excellent antimicrobial properties of the composites even at small concentrations of SiCO. The microscopic (scanning electron micrograph) and spectroscopic (energy-dispersive X-ray) investigations manifested the uniformity of particle distribution. Although the addition of CO slightly decreased the thermal stability of the composite films, it marginally enhanced the mechanical properties and crystallinity. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47825.     

High performance HTLNR/epoxy blend—Phase morphology and thermo-mechanical properties

An attempt was made to toughen diglycidyl ether of bisphenol A (DGEBA) type epoxy resin with liquid natural rubber possessing hydroxyl functionality (HTLNR). Epon 250 epoxy monomer is cured using nadic methyl anhydride as hardener in presence of N, N dimethyl benzyl amine as accelerator. HTLNR of different concentrations up to 20 wt % is used as modifier for epoxy resin. The addition HTLNR to an anhydride hardener/epoxy monomer mixture has given rise to the formation of phase-separated structure, consisting of small spherical liquid natural rubber particles bonded to the surrounding epoxy matrix. The particle size increased with increase in rubber content. The viscoelastic properties of the blends were analyzed using dynamic mechanical thermal analysis. The T_g corresponding to epoxy rich phase was evident from the dynamic mechanical spectrum, while the T_g of the rubber phase was overlapped by the β relaxation of epoxy phase. Glass transition of the epoxy phase decreased linearly as a function of the amount of rubber. The mechanical properties such as impact and fracture toughness were also carefully examined. The impact and fracture toughness increase with HTLNR content. A threefold increase in impact strength was observed with 15 wt % HTLNR/epoxy blend. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Reaction‐induced phase separation and resulting thermomechanical and surface properties of epoxy resin/poly(ethylene oxide)–poly(propylene oxide)–poly(ethylene oxide) blends cured with 4,4′‐diaminodiphenylsulfone

We investigated the phase separation, cure kinetics and thermomechanical properties of diglycidyl ether of bisphenol‐A/4,4′‐diaminodiphenylsulfone/poly(ethylene oxide)–poly(propylene oxide)–poly(ethylene oxide) (PEO–PPO–PEO) triblock copolymer (TBCP) blends. Fourier transform infrared spectroscopy, differential scanning calorimetry, and atomic force microscopy revealed that the blends exhibited heterogeneous phase morphology in which the TBCP formed dispersed domains in epoxy matrix, due to reaction induced phase separation. A fraction of phase‐separated PEO phase underwent partial crystallization whereas another fraction formed interphases between the dispersed domains and epoxy matrix. Moreover, the dispersed PEO chains improved the compatibility and interfacial adhesion between the matrix and domains and, consequently, significantly improved the mechanical properties of epoxy resin. Furthermore, the thermal degradation studies and contact angle measurements disclosed that the dispersed domains were well protected by the epoxy matrix. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44406.     

Epoxidized natural rubber/epoxy blends: Phase morphology and thermomechanical properties

Epoxidized natural rubbers (ENRs) were prepared. ENRs with different concentrations of up to 20 wt % were used as modifiers for epoxy resin. The epoxy monomer was cured with nadic methyl anhydride as a hardener in the presence of N,N‐dimethyl benzyl amine as an accelerator. The addition of ENR to an anhydride hardener/epoxy monomer mixture gave rise to the formation of a phase‐separated structure consisting of rubber domains dispersed in the epoxy‐rich phase. The particle size increased with increasing ENR content. The phase separation was investigated by scanning electron microscopy and dynamic mechanical analysis. The viscoelastic behavior of the liquid‐rubber‐modified epoxy resin was also evaluated with dynamic mechanical analysis. The storage moduli, loss moduli, and tan δ values were determined for the blends of the epoxy resin with ENR. The effect of the addition of rubber on the glass‐transition temperature of the epoxy matrix was followed. The thermal stability of the ENR‐modified epoxy resin was studied with thermogravimetric analysis. Parameters such as the onset of degradation, maximum degradation temperature, and final degradation were not affected by the addition of ENR. The mechanical properties of the liquid‐natural‐rubber‐modified epoxy resin were measured in terms of the fracture toughness and impact strength. The maximum impact strength and fracture toughness were observed with 10 wt % ENR modified epoxy blends. Various toughening mechanisms responsible for the enhancement in toughness of the diglycidyl ether of the bisphenol A/ENR blends were investigated. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 39906.     

Effect of nanoclay and carboxyl-terminated (butadiene-co-acrylonitrile) (CTBN) rubber on the reaction induced phase separation and cure kinetics of an epoxy/cyclic anhydride system

The effects of nano clay, carboxyl-terminated (butadiene-co-acrylonitrile) (CTBN) liquid rubber and the combination of both on the cure kinetics of diglycidyl ether of bisphenol-A (DGEBA)-based epoxy resin/nadic methyl anhydride were studied. Cure kinetics studies were carried out by performing dynamic and isothermal differential scanning calorimetric (DSC) experiments. The dynamic DSC experiments were carried out at four different heating rates. Dynamic kinetic modeling was performed using Kissinger and Ozawa approaches. Since these methods are based exclusively on the maximum rate of cure, which occurs approximately at the beginning of the cure reaction, the activation energy calculated using these methods is valid only for the initial stage of the cure. The clay (3 phr) filled epoxy system has an activation energy 24 % lower than the unfilled system. The role of the surfactant chemistry on the initial stage of the cure reaction was also studied. A plausible reaction mechanism which involves the effect of the nanoclay surfactant as an accelerator of the cure reaction was proposed. The phase separated CTBN rubber hindered the cure reaction and has 3 % higher activation energy for epoxy/CTBN system than the unfilled system. In the ternary epoxy/3 phr clay/15 phr CTBN system, the accelerating effect of clay on cure was highlighted. The cure activation observed in the presence of clay overshadows the hindrance created by the phase separated CTBN. Isothermal DSC scans were carried out at five different temperatures. The experimental datas showed an autocatalytic behavior of the reaction, and the isothermal modeling was carried out by Kamal autocatalytic model. The results showed a very good agreement within the whole conversion range for the unfilled and all the filled systems. The evolution of the morphology and phase separation was also studied using optical and scanning electron microscope. Faster cure reaction resulted in smaller phase-separated CTBN particles in epoxy/clay/CTBN ternary system as compared with those observed in epoxy/CTBN binary blend.     

Preparation and properties of MWCNTs/poly(acrylonitrile‐ styrene‐butadiene)/epoxy hybrid composites

Poly(acrylonitrile‐styrene‐butadiene) (ABS) was used to modify diglycidyl ether of bisphenol‐A (DGEBA) type epoxy resin, and the modified epoxy resin was used as the matrix for making multiwaled carbon tubes (MWCNTs) reinforced composites and were cured with diamino diphenyl sulfone (DDS) for better mechanical and thermal properties. The samples were characterized by using infrared spectroscopy, pressure volume temperature analyzer (PVT), thermogravimetric analyzer (TGA), dynamic mechanical analyzer (DMA), thermo mechanical analyzer (TMA), universal testing machine (UTM), and scanning electron microscopy (SEM). Infrared spectroscopy was employed to follow the curing progress in epoxy blend and hybrid composites by determining the decrease of the band intensity due to the epoxide groups. Thermal and dimensional stability was not much affected by the addition of MWCNTs. The hybrid composite induces a significant increase in both impact strength (45%) and fracture toughness (56%) of the epoxy matrix. Field emission scanning electron micrographs (FESEM) of fractured surfaces were examined to understand the toughening mechanism. FESEM micrographs reveal a synergetic effect of both ABS and MWCNTs on the toughness of brittle epoxy matrix. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Mechanical,thermal, and viscoelastic response of novel in situ CTBN/POSS/epoxy hybrid composite system

The present study focuses on the preparation of a novel hybrid epoxy nanocomposite with glycidyl polyhedral oligomeric silsesquioxane (POSS) as nanofiller, carboxyl terminated poly(acrylonitrile‐co‐butadiene) (CTBN) as modifying agent and diglycidyl ether of bisphenol A (DGEBA) as matrix polymer. The reaction between DGEBA, CTBN, and glycidyl POSS was carefully monitored and interpreted by using Fourier transform infrared (FTIR) and differential scanning calorimetry (DSC). An exclusive mechanism of the reaction between the modifier, nanofiller, and the matrix is proposed herein, which attempts to explains the chemistry behind the formation of an intricate network between POSS, CTBN, and DGEBA. The mechanical properties, such as tensile strength, and fracture toughness, were also carefully examined. The fracture toughness increases for epoxy/CTBN, epoxy/POSS, and epoxy/CTBN/POSS hybrid systems with respect to neat epoxy, but for hybrid composites toughening capability of soft rubber particles is lost by the presence of POSS. Field emission scanning electron micrographs (FESEM) of fractured surfaces were examined to understand the toughening mechanism. The viscoelastic properties of epoxy/CTBN, epoxy/POSS, and epoxy/CTBN/POSS hybrid systems were analyzed using dynamic mechanical thermal analysis (DMTA). The storage modulus shows a complex behavior for the epoxy/POSS composites due to the existence of lower and higher crosslink density sites. However, the storage modulus of the epoxy phase decreases with the addition of soft CTBN phase. The T_g corresponding to epoxy‐rich phase was evident from the dynamic mechanical spectrum. For hybrid systems, the T_g is intermediate between the epoxy/rubber and epoxy/POSS systems. Finally, TGA (thermo gravimetric analysis) studies were employed to evaluate the thermal stability of prepared blends and composites. POLYM. COMPOS., 37:2109–2120, 2016. © 2015 Society of Plastics Engineers     

Mechanical properties of poly(styrene‐co‐acrylonitrile)‐modified epoxy resin/glass fiber composites

Poly(styrene‐co‐acylonitrile) was used to modify diglycedyl ether of bisphenol‐A type epoxy resin cured with diamino diphenyl sulfone and the modified epoxy resin was used as the matrix for fiber‐reinforced composites (FRPs) to get improved mechanical properties. E‐glass fiber was used as fiber reinforcement. The tensile, flexural, and impact properties of the blends and composites were investigated. The blends exhibited considerable improvement in mechanical properties. The scanning electron micrographs of the fractured surfaces of the blends and tensile fractured surfaces of the composites were also analyzed. The micrographs showed the influence of morphology on the properties of blends. Results showed that the mechanical properties of glass FRPs increased gradually upon fiber loading. Predictive models were applied using various equations to compare the mechanical data obtained theoretically and experimentally. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Cure kinetics and thermal stability of micro and nanostructured thermosetting blends of epoxy resin and epoxidized styrene‐block‐butadiene‐block‐styrene triblock copolymer systems

The compatibility of styrene‐block‐butadiene‐block‐styrene (SBS) triblockcopolymer in epoxy resin is increased by the epoxidation of butadiene segment, using hydrogen peroxide in the presence of an in situ prepared catalyst in water/dichloroethane biphasic system. Highly epoxidized SBS (epoxy content SBS >26 mol%) give rise to nanostructured blends with epoxy resin. The cure kinetics of micro and nanostructured blends of epoxy resin [diglycidyl ether of bisphenol A; (DGEBA)]/amine curing agent [4,4′‐diaminodiphenylmethane (DDM)] with epoxidized styrene‐block‐butadiene‐block‐styrene (eSBS 47 mol%) triblock copolymer has been studied for the first time using differential scanning calorimetry under isothermal conditions to determine the reaction kinetic parameters such as kinetic constants and activation energy. The cure reaction rate is decreased with increasing the concentration of eSBS in the blends and also with the lowering of cure temperature. The compatibility of eSBS in epoxy resin is investigated in detailed by Fourier transform infrared spectroscopy, optical and transmition electron microscopic analysis. The experimental data of the cure behavior for the systems, epoxy/DDM and epoxy/eSBS(47 mol%)/DDM show an autocatalytic behavior regardless of the presence of eSBS in agreement with Kamal's model. The thermal stability of cured resins is also evaluated using thermogravimetry in nitrogen atmosphere. POLYM. ENG. SCI., 2012. © 2012 Society of Plastics Engineers