Synthesis of Self-Healing Bio-Based Tannic Acid-Based Methacrylates By Thermoreversible Diels–Alder Reaction

This investigation reports the effective use of the Diels–Alder (DA) click reaction in the preparation of self-healing bio-based dendritic methacrylates having reactive furfuryl functionality. Bio-based methacrylates were synthesized by modifying tannic acid with glycidyl methacrylate and furfuryl functionality was introduced by atom transfer radical polymerization with varied amount of furfuryl methacrylate monomer. The thermoreversible network was successfully achieved by DA and retro-DA reaction between the furfuryl groups and a bifunctional maleimide crosslinker, bismaleimide. This process was studied by nuclear magnetic resonance spectroscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, and solvent exposure tests. Differential scanning calorimetry analysis was used to determine the endothermic retro-DA reaction in the DA adduct. The self-healing property of the above crosslinked material was demonstrated by monitoring the repair of a scratch in the polymer film upon heating and cooling. This was analyzed by scanning electron microscopy. POLYM. ENG. SCI., 60:140–150, 2020. © 2019 Society of Plastics Engineers     

Strategic Shuffling of Clay Layers to Imbue Them with Responsiveness

Layers of naturally occurring clay minerals are rearranged to prepare highly sensitive multiresponsive clay–clay bilayer membrane (CCBM). The CCBM introduced here responds to the minuscule changes in the surrounding environments including temperature, humidity, and presence of solvent vapors by morphing in specific manners. Strips cut from CCBM exhibit up to 588 N kg^?1 force output when exposed to temperature fluctuations. Inheriting the natural stability of clay minerals, CCBM demonstrates extreme robustness, heating up to 500 °C, cooling with liquid N₂ and exposure to corrosive chemical vapors did not deteriorate its bending performance. Mechanistic studies suggest that shape transformations of CCBM are driven by the unequal response of its components to external stimuli.     

Biodegradable and thermostable synthetic hyperbranched poly(urethane-urea)s as advanced surface coating materials

Aliphatic hyperbranched poly(urethane-urea)s with different weight percentages of branch generating moiety were synthesized by a one pot A₂ + BC₂ approach. Isophorone diisocyanate was used as the A₂ type monomer, while a tri-functional dihydroxyamine compound synthesized from ?-caprolactam and diethanol amine acted as the BC₂ monomer. Evidence supporting the hyperbranched structure of the synthesized poly(urethane-urea) was obtained from ¹H NMR spectra. FTIR study confirmed the nature and extent of hydrogen bonding present in this novel macromolecule. A Gaussian band fitting procedure of the IR band at amide-I region showed that the extent of hydrogen bonding increases with the increase of weight percentage of the tri-functional compound. The tensile strength, elongation at break, impact resistance, scratch hardness and gloss followed an increasing trend with the same. The thermal degradation of the hyperbranched poly(urethane-urea) was found to be dependent on the weight percentage of the BC₂ type moiety. The kinetics of thermal degradation studied by the Ozawa method showed that the activation energy required for thermal degradation of hyperbranched polymer is higher than its linear polyurethane analog. The synthesized polymer was found to be biodegradable by Pseudomonas aeruginosa bacteria. The study showed superiority of the hyperbranched structure over the linear one. Thus the results indicated the potential usage of the studied hyperbranched poly(urethane-urea) as an advanced surface coating material.     

Copper‐Catalyzed C–N,C–O Coupling Reaction of Arylglyoxylic Acids with Isatins

The copper(II)‐catalyzed decarboxylative coupling reactions of arylglyoxylic acids with isatins afford 4H‐benzo[d][1,3]oxazin‐4‐ones via decarbonylation and concurrent C–N, C–O bond formation.

     

Anodic dissolution of U, Zr and U–Zr alloy and convolution voltammetry of Zr|Zr couple in molten LiCl–KCl eutectic

The anodic dissolution of U and Zr metal was studied in LiCl–KCl–UCl₃ and LiCl–KCl–ZrCl₄, respectively, at 773 K by cyclic voltammetry and compared with their respective dissolution behaviour in blank LiCl–KCl eutectic. The anodic dissolution of U–Zr alloy in LiCl–KCl–UCl₃ was also studied at 773 K to compare with the dissolution of U and Zr. The transfer coefficients evaluated by Tafel analysis and the method of Allen–Hickling for U and Zr dissolution were found to be in fair agreement with each other. U dissolution in LiCl–KCl–UCl₃ and Zr dissolution LiCl–KCl–ZrCl₄ were also studied by chronoamperometry and the diffusion coefficient value of U³⁺ was calculated to be in the range of 2.9 × 10⁻⁵ to 3.3 × 10⁻⁵ cm² s⁻¹ which is in agreement with those reported in literature. Convolution voltammetric analysis of Zr⁴⁺/Zr²⁺ redox couple in LiCl–KCl–ZrCl₄ was carried out for the first time to have a comprehensive understanding of the electrode kinetics.     

Development and characterization of pseudolatex based transdermal drug delivery system of diclofenac.

A transdermal drug delivery system of diclofenac was developed for prolonged and controlled release of diclofenac. The designed system essentially based on polymeric pseudolatex dispersion. The formulation variables that could effect the formulation stability vis a vis drug release were studied. To achieve the desired release rate, different combination of hydrophilic and hydrophobic polymer were used for the preparation of pseudolatex system. The designed system exhibited linear relationship between drug release (Q) V/s square root of time (t^0.5). The product having skin permeability rate 0.188 mg/h/cm was selected for the in vitro anti-inflammatory activity and in vivo evaluation. The system could maintained a constant and effective plasma level for 24 hours. The effective drug plasma concentration was monitored periodically. The study revealed that designed pseudolatex transdermal drug delivery system of diclofenac could be used successfully with improved performance and hold promise for further studies.     

XRD and FT-IR investigations of sub-bituminous Assam coals

Two coal samples collected from Makum coal field, Assam, India were studied by XRD and FT-IR techniques. The X-ray diffractogram shows the existence of some crystalline carbons in Assam coals as proven by the appearance of peaks. The radial distribution functional (RDF) method was applied for the determination of structural aspects of the coals. The study indicates that the coals are lignite in type and there is no evidence of graphite-like structures. The maximum in the G(r) plots of function of radial distribution of atoms (FRDA) relates to different distances between carbon atoms of aliphatic chains. The first significant maximum relates to the C-C bond (type C-CH=CH-C), the second maximum relates to the distance between carbon atoms of aliphatic chains that are located across one carbon atom. The curve intensity profiles obtained from FRDA show quite regular molecular packets for this coal. The coals were found to be lignite in nature. FT-IR study shows the presence of aliphatic carbon, C=O and C-O stretching associated with -OH and -NH stretching vibrations. Kaolinite and quartz were also found to be major minerals in Assam coals by FTIR spectroscopy. The difference in intensities of carbonyl groups of the coal samples is likely to relate with the rank.