Shashank T. Mhaske

Synthesis of nano cellulose fibers and effect on thermoplastics starch based films

Starch based films limit their application due to highly hydrophilic nature and poor mechanical properties. This problem was sought to be overcome by forming a nanocomposite of Thermoplastic starch (TPS) and Nano-Cellulose fibers (NCF). NCF was successfully synthesised from short stable cotton fibres by a chemo-mechanical process. TPS/NCF composite films were prepared by solution casting method, and their characterizations were done in terms of differential scanning calorimeter (DSC), morphology (SEM), water vapor permeability (WVTR), oxygen transmission rate (OTR), X-ray diffractograms, light transmittance and tensile properties. At very low concentration of NCF filled TPS composite film showed improvement in properties. The 0.4 t% NCF loaded TPS films showed 46.10% improved tensile strength than by base polymer film, beyond that 0.5 t% concentration tensile strength starts to deteriorate. WVTR and OTR results showed improved water vapor barrier property of TPS matrix. The DSC thermograms of TPS and composite films did not show any significant effect on the melting point of composite film to the base polymer TPS.

Phase transformation of nanostructured titanium dioxide from anatase-to-rutile via combined ultrasound assisted sol-gel technique

An effort was made to synthesize nanostructured TiO(2) via sol-gel technique to obtain a 100% rutile polymorph of nanostructured TiO(2). The sol-gel synthesis technique was suitably modified by incorporating ultrasound to study the effect of cavitation on the phase transformation, crystallite size, crystallinity and morphological (scanning electron microscopy) properties of the obtained nano-TiO(2). It was observed that using ultrasound, yield of the nano-TiO(2) was improved from 86.35% to 95.078%. The phase transformation of anatase-to-rutile of TiO(2) was studied for both (ultrasound assisted and conventional) the processes. Complete phase transformation of the TiO(2) was observed as expected with and without the use of ultrasound but the marked reduction in the required calcination temperature for obtaining 100% phase transformation with ultrasound was the major achievement in the present study, leading to 70% energy savings during calcination.

Functional behaviour of polypropylene/ZnO–soluble starch nanocomposites

ZnO-polypropylene nanocomposites (nano-PP) were prepared using nanoparticles of ZnO stabilized by soluble starch (nano-ZnO) as filler in PP by the melt mixing process. X-ray diffraction (XRD) and other spectroscopic analysis—ultraviolet–visible (UV–vis), Fourier transform infrared (FTIR) and photoluminescence—revealed the presence and characteristics of nano-ZnO in the composites. The presence of ZnO imparts whiteness, while starch increased the yellowing of polymers. The nanocomposites were analyzed for changes in optical, mechanical, electrical and rheological properties, as influenced by the increasing concentration of nano-ZnO. The mechanical properties were marginally increased and the dielectric strength of the nano-PP increased to a notable level. By monitoring the evolution of the carbonyl absorption bands from FTIR analysis, the efficacy of nano-ZnO in the reduction of photo-degradation due to UV irradiation was demonstrated. The excellent antibacterial activity exhibited by nano-ZnO impregnated PP against two human pathogenic bacteria, Staphylococcus aureus and Klebsiella pneumoniae, makes it a suitable candidate for food packaging applications.

Synthesis of titanium dioxide by ultrasound assisted sol–gel technique: Effect of amplitude (power density) variation

Titanium dioxide was successfully synthesized by utilizing sol-gel technique modified by incorporation of ultrasound as a reaction aid. The effect of amplitude of irradiation (power input varied from 19.9 to 80.8 W) on % Rutile, % yield, % crystallinity, crystallite size and morphological (scanning electron microscopy) properties of the obtained nano-TiO(2) was studied. Calcination temperatures of all the samples were kept constant at 750 degrees C. With increasing ultrasonic irradiation amplitude it is observed that the values of % Rutile (after calcination) increased and reached a peak value after which further increase in amplitude resulted in a decrease in the % Rutile. A similar trend was observed in the case of % crystallinity and % yield of the reaction. On the basis of these results an optimum operating ultrasonic irradiation amplitude for the reaction has been suitably established.

Synthesis of zirconium dioxide by ultrasound assisted precipitation: Effect of calcination temperature

Nanostructured zirconium dioxide was synthesized from zirconyl nitrate using both conventional and ultrasound assisted precipitation in alkaline medium. The synthesized samples were calcinated at temperatures ranging from 400°C to 900°C in steps of 100°C. The ZrO(2) specimens were characterized using X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The thermal characteristics of the samples were studied via Differential Scanning Calorimetry-Thermo-Gravimetry Analysis (DSC-TGA). The influence of the calcination temperature on the phase transformation process from monoclinic to tetragonal to cubic zirconia and its consequent effect on the crystallite size and % crystallinity of the synthesized ZrO(2) was studied and interpreted. It was observed that the ultrasound assisted technique helped to hasten to the phase transformation and also at some point resulted in phase stabilization of the synthesized zirconia.

Preparation of nano cellulose fibers and its application in kappa-carrageenan based film

Bio-based nanocomposite films were successfully developed using nanofibrillated cellulose (NFC) as the reinforcing phase and kappa-carrageenan (KCRG) as the matrix. NFC was successfully synthesis from short stable cotton fibers by chemo-mechanical process. The bionanocomposites were prepared by incorporating 0.1, 0.2, 0.3, 0.4, 0.5, and 1wt% of the NFC into a KCRG matrix using a solution casting method there characterization was done in terms of thermal properties (DSC), morphology (SEM), water vapor transmission rate (WVTR), oxygen transmission rate (OTR), X-ray diffractograms (XRD), and tensile properties. The main conclusion arising from the analysis of the result is that the bionanocomposites containing 0.4wt% of NFC exhibited the highest enhancement in tensile strength it is almost 44% improvement. WVTR and OTR results showed improvement of all nanocomposite film compare to control KCRG film.

Synthesis of titanium dioxide by ultrasound assisted sol–gel technique: Effect of calcination and sonication time

Nanostructured titanium dioxide has been synthesized using both conventional and ultrasound assisted sol-gel technique with an objective of understanding the role of cavitational effects in the synthesis process. The experiments were conducted at a constant calcination temperature of 750 °C and the calcination time was varied from 30 min to 3 h to study the effect of calcination time on the properties of the synthesized TiO₂. The TiO₂ specimens were characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The influence of the sonication time on the phase transformation process from anatase to rutile and also on the crystallite size and percentage crystallinity of the synthesized TiO₂ has also been investigated. It was observed that 100% phase transformation occurred after 3 h of calcination for the ultrasound assisted sol-gel synthesized TiO₂. The study on the phase transformation via variation of sonication time yielded interesting results. It was observed that as the sonication time increased, an initial increase in the rutile content is obtained and beyond optimum sonication time, the rutile content decreased. In general, the ultrasound assisted process results in synthesis of TiO₂ material with higher rutile content as compared to the conventional sol-gel process.

Preparation and Characterization of K-Carrageenan/Nanosilica Biocomposite Film

The purpose of this study is to improve the performance properties of K-carrageenan (K-CRG) by utilizing nanosilica (NSI) as the reinforcing agent. The composite films were prepared by solution casting method. NSI was added up to 1.5% in the K-CRG matrix. The prepared films were characterized for mechanical (tensile strength, tensile modulus, and elongation at break), thermal (differential scanning calorimetry, thermogravimetric analysis), barrier (water vapour transmission rate), morphological (scanning electron microscopy), contact angle, and crystallinity properties. Tensile strength, tensile modulus, and crystallinity were found to have increased by 13.8, 15, and 48% whereas water vapour transmission rate was found to have decreased by 48% for 0.5% NSI loaded K-CRG composite films. NSI was found to have formed aggregates for concentrations above 0.5% as confirmed by scanning electron microscopy. Melting temperature, enthalpy of melting, and degradation temperature of K-CRG increased with increase in concentration of NSI in K-CRG. Contact angle also increased with increase in concentration of NSI in K-CRG, indicating the decrease in hydrophilicity of the films improving its water resistance properties. This knowledge of the composite film could make beneficial contributions to the food and pharmaceutical packaging applications.

Synthesis of Star-Shaped Polymers

Star-shaped polymers, consisting of a core and a number of arms radiating from the core, have attracted more and more attention because of their highly branched structures and unique rheological properties. Various synthesis methods, like reversible addition–fragmentation chain transfer polymerization (AFCTP), stable free radical polymerization (SFRP), atom transfer radical polymerization (ATRP), etc., are used to synthesize star-shaped polymers. Star-shaped polymers are formed from various different chemicals compounds, like divinyl compounds, polyisoprene, polylactides and even amphiphilic compounds. In this review various synthesis schemes and chemical compounds utilized are explained in brief to give the readers an insight in the field of star-shaped polymers.

Novel synthesis, characterization and application of dibutyrate bis(2-hydroxyethyl) terephthalamide as a plasticizer in PVC compounding

This study focuses on the synthesis and application of dibutyrate of bis(2-hydroxyethyl) terephthalamide (DB-BHETA) as a plasticizer in poly(vinyl chloride) (PVC) compounding. DB-BHETA was synthesized from poly(ethylene terephthalate) bottle waste through aminolysis followed by condensation reaction with butyric acid. Synthesized DB-BHETA was characterized by FTIR, DSC and NMR. Plasticized PVC was prepared by melt blending of PVC in different ratios with DB-BHETA and the mechanical, thermal and rheological properties were investigated. The glass transition temperature (Tg) decreased with increasing concentration of DB-BHETA, confirming its plasticizing effect. The impact properties of PVC/DB-BHETA were maximum at weight ratio of 80/20. Shore hardness continuously reduced with increase in the concentration of DB-BHETA in PVC. Also, incorporation of DB-BHETA results in a gradual decrease in the loss modulus (viscous) and an increase in the storage modulus (elastic).