Department of Chemical Engineering

Indian Institute of Technology Hyderabad (IITH) is a premier institute of science and technology established in 2008. IITH has been consistently ranked in the&nbsp;<a href="https://iith.ac.in/reports/" rel="noopener noreferrer">top 10 institutes</a>&nbsp;in India for Engineering&nbsp;<a href="https://www.nirfindia.org/2021/EngineeringRanking.html" rel="noopener noreferrer" target="_blank">according to NIRF</a>&nbsp;making it one of the most coveted schools for science and technology in the country.

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IIT Hyderabad

Poly(ester amide)s (PEAs) are polymers with both ester and amide bonds in the polymer backbone offering a combination of desirable properties such as degradability of esters and physio-chemical properties of amides that are attractive for biomedical applications. Olive oil (OO) is known to possess anti-inflammatory properties and offers beneficial health effects. Thus, the aim of this work was to develop a novel class of resorbable PEAs from OO for biomedical applications. Cross-linked PEAs were synthesized by melt condensation followed by curing. The chain length of the diacid, molar ratio of the reactants, and curing conditions were systematically varied to yield a library of polymers with tunable properties. FTIR and 1H-NMR revealed the presence of ester and amide bonds in the polymers. Properties such as the water contact angle and storage modulus (which is directly related to the cross-linking density) increased with the increase in the chain length of the diacid as well as the curing time and with the decrease in the molar ratio of diacid to the functionalized precursor. Hydrolytic degradation studies showed that polymers had a wide range of degradation that spanned ≈ 12 to 50% in 1 week. The dye release followed the Korsmeyer-Peppas semi-empirical equation. In vitro cell studies showed that the polymers were cytocompatible. Thus, this work presents PEAs from OO that are promising resorbable biomaterials for biomedical applications. © 2019, Qatar University and Springer Nature Switzerland AG.

World University root node

Emergent Materials

Degradable poly(ester amide)s from olive oil for biomedical applications

The present work demonstrates the use of mesoporous nanofibers for the enhanced analytical performance of electrochemical biosensor. By exploiting the phase separation property of the block copolymers, a simple three-step process was used to generate the porosity in the nanofibers. Here we present the effect of the porosity on the sensing ability of the electrospun PS-b-PMMA nanofibers. The functional groups present on the nanofiber surface were characterized using DPV. The nanofibers modified electrode showed a large decrease in the oxidation current with the increase in the pH from 4.2 to 6.8 for the anionic redox couple whereas the change in the current is negligible for a neutral redox couple, this suggested the presence of -COOH groups. A one-step process was used for the immobilization of biotin. There were about 35.5 % and 66.6 % decrease in the redox current for the as-spun and porous nanofibers after functionalization respectively which indicate the presence of a high amount of active sites in the porous nanofibers. Finally, the sensor response was studied using streptavidin (1μg/ml–1fg/ml) as a model analyte. CV studies showed a 2.7-fold increase whereas DPV showed a 6-fold increase in the sensitivity for the porous nanofibers as compared to the as-spun nanofibers. © 2019 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

Electroanalysis

Electrospun Mesoporous Poly(Styrene-Block-Methyl- Methacrylate) Nanofibers as Biosensing Platform: Effect of Fibers Porosity on Sensitivity

In this study, we synthesized amine functionalized cellulose nanofiber based adsorbent for effective removal of dissolved fluoride ions from groundwater samples. Cellulose acetate was electrospun into nanofibers followed by deacetylation to yield cellulose nanofibers which were then treated with ethylenediamine to prepare amine functionalized cellulose fabric to be used as an adsorbent. As- synthesized adsorbent was first characterized by scanning electron microscopy and Fourier transform infrared spectroscopy for physiochemical characteristics. Fluoride adsorption studies were then carried out under batch mode to study the influence of various parameters on adsorption process. Amine functionalized cellulose nanofibrous mat was found to be effective with high adsorption efficiency for removal of fluoride ions from aqueous solution, even at low fluoride concentrations (&lt; 5 mg L −1 ). Adsorption mechanism of fluoride onto prepared cellulose nanofibers based adsorbent was explained from the studies of isotherms, kinetic and thermodynamic parameters. Field studies conducted using this amine functionalized cellulose nanofibrous mat revealed the suitability and effectiveness of adsorbent for fluoride removal from contaminated groundwater. © 2019, Springer Science+Business Media, LLC, part of Springer Nature.

Journal of Polymers and the Environment

Amine Functionalized Electrospun Cellulose Nanofibers for Fluoride Adsorption from Drinking Water

The thermochemical conversion of lignocellulosic biomass including lignin leads to the generation of a complex mixture of oxygenated aromatic monomers. Further processing of this mixture is essential for the production of value-added chemicals. The present investigation is therefore dedicated to the hydrodeoxygenation (HDO) of guaiacol as model compound over molybdenum (Mo), tungsten (W) and tantalum (Ta) modified nickel catalysts supported on Al2O3, ZrO2, TiO2 and SiO2 in a batch reactor. All the catalysts were prepared by co-impregnation method and characterized by several techniques such as BET, powder-XRD, H2-TPR, UV–vis, FTIR and pyridine-FTIR to understand the interaction of nickel and modifier and their role in activity and product selectivity. Among the various catalysts studied, molybdenum modified nickel catalyst (Ni-Mo) supported on zirconia exhibits superior activity and selectivity. Detail characterization results revealed that various reducible surface species were formed depending on nickel to molybdenum mole ratio, total metal loading, reduction temperature and supports. The Ni-Mo/Zr catalysts are associated with metallic nickel and partially reduced Mo4+ species which acts as Lewis acid sites. The proportion of Ni/Mo4+ varies with the nickel to molybdenum mole ratio and reduction temperature. The Ni-Mo/Zr catalyst of equimolar Ni-Mo composition showed higher HDO activity of guaiacol and selectivity of phenol due to the presence of optimum proportion of Ni and Mo4+ species. During HDO of guaiacol, phenol, catechol, anisole, cresols, cyclohexanol, cyclohexanone, cyclohexene and cyclohexane were identified as products and phenol was the primary product with higher selectivity. A possible reaction pathway is proposed based on the product distribution obtained under wide range of process parameters and using different catalysts. The structural informations of catalysts obtained from various characterization studies are co-related with the HDO activity and selectivity of products. © 2018 Elsevier B.V.

Catalysis Today

Hydrodeoxygenation of guaiacol over Mo, W and Ta modified supported nickel catalysts

Lignin is recognized as a renewable and rich source of aromatics, which could be an alternative to fossil fuel-based petrochemicals. However, the development of an efficient catalyst and industrially scalable process for lignin depolymerization remains a challenge. The present work is therefore dedicated towards a one-pot approach for depolymerization of commercial kraft lignin in a batch reactor with higher loading using the water-THF solvent mixture over the HZSM-5 and NaOH catalytic system. Process parameters such as time, temperature, lignin-to-solvent (w/v), water-to-THF (v/v), NaOH-to-lignin (w/w), catalyst-to-lignin (w/w), and Si/Al mole ratios of HZSM5 were chosen carefully and optimized using statistical analysis-response surface methodology (RSM). A significant yield of 61% for a particular single ring aromatic compound (i.e. guaiacols) was obtained under the optimized reaction conditions: reaction time = 2 h, temperature = 533 K, lignin-to-solvent ratio = 0.060 (1:16.6), water-to-THF ratio = 0.86:1, catalyst-to-lignin ratio = 1:6 (0.16), NaOH-to-lignin ratio = 0.1 and Si/Al ratio = 280. Around 77% of lignin was selectively converted to guaiacols (79%) with minimal char formation (7.7%). The Hansen solubility parameter and RSM studies indicate that the obtained results were significantly related to the solubility of lignin and guaiacol at different water-THF ratios. FT-IR and 1H-NMR studies were also performed to correlate the process outcome with the presence of functional groups in identified EtOAc soluble products. A plausible mechanism for catalytic depolymerization of lignin has been proposed considering the product distribution obtained under varying process parameters. © 2019 The Royal Society of Chemistry.

Green Chemistry

Thermocatalytic depolymerization of kraft lignin to guaiacols using HZSM-5 in alkaline water-THF co-solvent: A realistic approach

Research on self-healing materials has been a topic of interest for almost one decade now and it represents a wide interdisciplinary area, exhibiting a large variety of different approaches. Although different types of polymers have been researched upon for this application, synthesizing them and using them for large-scale applications still remain a challenge. Polyurethanes (PU) have emerged as a promising class of polymeric materials in this context due to their ease of synthesis, shape memory properties and the ability to be fabricated on the basis of desired end properties. In this critical review, we have enlisted a comprehensive summary of different approaches that have been used over the past decade to synthesize self-healing PUs. In addition, we have also discussed in detail the "close then heal" and "shape memory assisted self-healing" concept whereby the shape memory properties of PUs can be utilised to bring the damaged parts together to achieve autonomous healing. Such a review will help guide researchers working in this field both from academia and industry. © The Royal Society of Chemistry 2019.

Polymer Chemistry

The journey of self-healing and shape memory polyurethanes from bench to translational research

Polyols are multifunctional alcohols, with branched structures, where each arm terminates with an –OH group. These free –OH groups have been utilised to make a variety of polymer structures ranging from cross-linked to linear to starshaped. This review presents a comprehensive account of polyol-based polymers in biomedical applications. The advantages afforded by polyolbased biodegradable polymers are detailed in this review, alongside a general historical perspective on the development of biodegradable polymers. The major advantage of these polyols is that they are endogenous to the human body. Synthesis strategies and fabrication techniques to mould these materials into three-dimensional (3D) scaffolds are discussed. Modifications to the conventionally used polyol-based polyesters have been achieved by chemically incorporating drugs/ bioactives or by preparing nanocomposites. This review discusses the physicochemical properties and biological responses of these polymers relevant in biomedical applications and further outlines the need for improving their processability and performance. © 2018, © 2018 Institute of Materials, Minerals and Mining and ASM International Published by Taylor & Francis on behalf of the Institute and ASM International.

International Materials Reviews

Biodegradable polyol-based polymers for biomedical applications

Hypothesis: Spray drying is a facile technique to transform colloidal dispersion into micro-granules of controlled size, shape, and morphology. There is significant interest to understand the structural integrity, different morphology of the granules obtained post spray drying which find potential application in many technological fields. The shape of the constituent particles in the colloidal dispersion that is spray dried is expected to influence the micro-structural features of the micro-granules. Experiments: We investigate the formation of micro-granules consisting of nano-ellipsoids through controlled spray drying. The morphological features and the packing of ellipsoids in the granules are quantitatively analyzed by using small angle neutron scattering, small angle X-ray scattering and high-resolution field emission scanning electron microscopy. The time evolution of the micro-structure and the structural integrity of the granules are investigated by re-dispersing the powder granules in water. Findings: The morphology of the granules are found to be strongly correlated with the aspect ratio of the ellipsoid. While the drying of droplets containing lower aspect ratio ellipsoids give rise to mostly spherical granules, in stark contrast, for higher aspect ratio ellipsoids, micro-granules of different morphologies are formed including doughnut shaped granules. A plausible mechanism explaining such an aspect ratio dependent shape transformation is proposed. © 2019 Elsevier Inc.

Journal of Colloid and Interface Science

Spray drying of colloidal dispersions containing ellipsoids

In this article, we outline a procedure used to isolate individual intracellular bacterial communities from a mouse that has been experimentally infected in the urinary tract. The protocol can be broadly divided into three sections: the infection, bladder epithelial cell harvesting, and mouth micropipetting to isolate individual infected epithelial cells. The isolated epithelial cell contains viable bacterial cells and is nearly free of contaminating extracellular bacteria, making it ideal for downstream single-cell analysis. The time taken from the start of infection to obtaining a single intracellular bacterial community is about 8 h. This protocol is inexpensive to deploy and uses widely available materials, and we anticipate that it can also be utilized in other infection models to isolate single infected cells from cell mixtures even if those infected cells are rare. However, due to a potential risk in mouth micropipetting, this procedure is not recommended for highly infectious agents. © 2019 Creative Commons Attribution-NonCommercial-NoDerivs 3.0 Unported License.

Journal of Visualized Experiments

Isolation of single intracellular bacterial communities generated from a murine model of urinary tract infection for downstream single-cell analysis

The recent surge in the usage of electronics has led to a new kind of problem; electromagnetic interference which necessitates finding alternate materials that offer ease of processing, design flexibility, light weight, and ease of embedding and integrating with the existing systems in place as shields to protect the precise electronic circuitry. Herein, lightweight polycarbonate (PC)-based nanocomposites using doped graphene derivatives and multiwalled carbon nanotubes (MWCNT) has been explored for effective shielding of EM radiation in X- and Ku-band. To get a mechanistic insight as to how the dopant in graphene derivatives influences the EM shielding properties, two dopants have been explored here: ferrimagnetic (ferrite, Fe 3 O 4 ) and the other one as paramagnetic (gadolinium oxide, Gd 2 O 3 ). The doped graphene derivatives when composited with PC and MWCNTs resulted in materials that can shield the incoming EM radiation through magnetic and dielectric losses. This strategy of doping improves the state of dispersion of these dopants in the nanocomposites, besides enhancing the shielding effectiveness. The PC-based nanocomposites illustrated a total shielding effectiveness (SE T ) of -28 and -33 dB at 18 GHz for a given concentration of Gd 2 O 3 and Fe 3 O 4 hybrid, respectively. A closer look into the mechanism of shielding reveals that irrespective of the dopant, various losses (magnetic and dielectric) decide the shielding effectiveness in polymeric nanocomposites facilitated by multiple internal reflections. Taken together, this study brings in new insight as to how the losses contribute toward effective shielding rather than the choice of the dopant and will help guide researchers working in this area from both industrial as well as academic perspective. Copyright © 2019 American Chemical Society.

Journal of Physical Chemistry C

Mechanistic Insight into the Nature of Dopants in Graphene Derivatives Influencing Electromagnetic Interference Shielding Properties in Hybrid Polymer Nanocomposites