Studies on ionic salt of polyamic acid and related compounds

Amic acid compound namely bisphthalamic acid of 2, 2-dimethyl-4, 4-diaminobiphenyl (amic acid) and its ionic salt with 3-(dimethylamino)propyl methacrylate (amic acid salt) were synthesized and characterized by FT-IR, mass spectroscopy, NMR and DSC. Effect of temperature and water content on these compounds was studied by ¹H-NMR and potentiometric titration. In the absence of added water, both amic acid and its ionic salt had undergone imidization followed by hydrolysis, which was attributed to the water formed as a result of an initial imidization reaction. Polyamic acid (PAA) was synthesized by reacting 4, 4-oxydiphthalic anhydride and 2, 2-dimethyl 4, 4-diaminobiphenyl (m-tolidine) in N-methyl-2-pyrrolidone, which was then reacted with 3-(dimethylamino)propyl methacrylate to obtain PAS. Their storage stabilities were studied by monitoring their bulk viscosities and acid numbers as a function of time and temperature. PAS was found to be less stable than PAA. Similar observations were made for amic acid compounds. PAA and PAS showed two-step thermal degradation in air and nitrogen.     

Metal hollow sphere electrocatalysts

Metal micro-/nano hollow spheres have been widely applied in numerous fields during the last decade. This review will only focus on the synthetic strategies to synthesize hollow spherical structures in the enhancement of their electrocatalytic activity, especially the metal hollow spherical materials. We present a comprehensive overview of synthetic strategies for metal hollow spherical structures which have been approached specifically in electrochemical reactions. These synthetic methods are mainly categorized as hard templates, soft templates, sacrificial templates and without templates. The review further includes electrocatalytic approaches of hollow spherical metals in different electrochemical processes, especially the methanol electro-oxidation reaction for methanol fuel cell application and hydrogen and oxygen evolution reactions in water electrolyzer, as metal hollow spherical materials are especially applied in these specific reactions.     

Energy efficient control of a BTX dividing-wall column

Dividing-wall column (DWC) is considered nowadays the new champion in distillation, as it can bring substantial reduction in the capital invested as well as savings in the operating costs. This work presents the simulation results of energy efficient control and dynamics of a dividing-wall column (DWC). In order to allow a fair comparison of the results with previously published references, the case-study considered here is the industrially relevant ternary separation of the mixture benzene-toluene-xylene (BTX) in a DWC. Rigorous simulations were carried out in Aspen Plus and Aspen Dynamics. Several conventional control structures based on PID control loops (DB/LSV, DV/LSB, LB/DSV, LV/DSB) were used as a control basis. These control structures were enhanced by adding an extra loop controlling the heavy component composition in the top of the prefractionator, by using the liquid split as an additional manipulated variable, thus implicitly achieving minimization of energy requirements. The results of the dynamic simulations show relatively short settling times and low overshooting especially for the DB/LSV and LB/DSV control structures. Moreover, the energy efficient control proposed in this work allows the operation of DWC with minimum energy requirements or maximum purity of products.     

Isocyanurate based fluorinated polyurethane dispersion for anti-graffiti coatings

Fluorinated polyurethane dispersions (FPUDs) were synthesized using HDI isocyanurate, polyester polyol and DMPA with varying concentrations of trifluoro ethanol (TFE) in the range of 0–9 wt%. Further FPUDs were characterized by FT-IR and ¹H NMR for structural elucidation. Effects of trifluoro ethanol on the dispersion were evaluated by particle size analyzer. It was observed that with increase in TFE, particle size increases. Topography and contact angle were studied by atomic force microscopy (AFM) and goniometer, respectively. To gain more insight into the formation of roughness, power spectral density (PSD) analysis was carried out. It was found that with increase in TFE content, surface roughness increases due to migration of fluorinating agent on the coating substrate and consequently water repellency increases. Nano indentation of coating revealed that fluorinated coating possesses less stiffness and elastic modulus, due to the presence of fluorine on the coating. Further, coatings were analyzed for thermal properties by thermogravimetry analysis (TGA) and differential scanning calorimetry (DSC) which shows the enhancement in thermal stability and glass transition temperature with increase in TFE content. Anti-graffiti test was carried out which showed improved resistance with increasing fluorine content.     

Computational Approaches for Studying the Granular Dynamics of Continuous Blending Processes, 2 – Population Balance and Data‐Based Methods

The application of computationally inexpensive modeling methods for a predictive study of powder mixing is discussed. A multidimensional population balance model is formulated to track the evolution of the distribution of a mixture of particle populations with respect to position and time. Integrating knowledge derived from a discrete element model, this method can be used to predict residence time distribution, mean and relative standard deviation of the API concentration in a continuous mixer. Low‐order statistical models, including response surface methods, kriging, and high‐dimensional model representations are also presented. Their efficiency for design optimization and process design space identification with respect to operating and design variables is illustrated.

     

Synthesis of magnetic nanocomposite microparticles for binding of chlorinated organics in contaminated water sources

In this work, the development of novel magnetic nanocomposite microparticles (MNMs) via free radical polymerization for their application in the remediation of contaminated water is presented. Acrylated plant-based polyphenols, curcumin multiacrylate (CMA) and quercetin multiacrylate (QMA), were incorporated as functional monomers to create high affinity binding sites for the capture of polychlorinated biphenyls (PCBs), as a model pollutant. The MNMs were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, dynamic light scattering, and UV–visible spectroscopy. The affinity of these novel materials for PCB 126 was evaluated and fitted to the nonlinear Langmuir model to determine binding affinities (K_D). The results suggest the presence of the polyphenolic moieties enhances the binding affinity for PCB 126, with K_D values comparable to that of antibodies. This demonstrates that these nanocomposite materials have promising potential as environmental remediation adsorbents for harmful contaminants.     

Influence of normal contact force model on simulations of spherocylindrical particles

How the choice of elastic normal contact force model affects predictions from discrete element method simulations of spherocylindrical particles is investigated in this article. Three force models were investigated: (1) a Hertzian force model (HFM) which assumes a circular contact area; (2) a linear force model (LFM) with a constant stiffness; and (3) a modified HFM (MFM) that accounts for various contact areas and contact transitions. With the MFM, transitions between contact area types must be accounted for otherwise discontinuities in the contact force can occur. It is found that simple force models (HFM, LFM) can be substituted for more accurate force models if only force data and bulk properties are of interest. However, if more detailed contact information, such as contact area, contact overlap, contact duration, or collision frequency, are needed, for example, in population balance models and transient liquid bridge modeling, then a more accurate force model should be used. © 2018 American Institute of Chemical Engineers AIChE J, 64: 1986–2001, 2018     

Application of inline imaging for monitoring crystallization process in a continuous oscillatory baffled crystallizer

In this study, an in situ imaging system has been analysed to characterize the crystal size, the shape and the number of particles during a continuous crystallization process in a Continuous Oscillatory Baffled Crystallizer (COBC). Two image analysis approaches were examined for particle characterization in the suspension containing both small nuclei and larger grown crystals (nonspherical and irregular in shape). The pattern matching approach, in which the particles are approximated to be spherical, did result in an overestimation of the size. Alternatively, a segmentation‐based algorithm resulted in reliable crystal size and shape characteristics. The laser diffraction analysis in comparison to the image analysis overestimated the particle sizes due to the agglomeration of particles upon filtration and drying. The trend in the particle counts during the start of crystallization process, including nucleation, determined by the image analysis probe was comparable with the one measured by FBRM, highlighting the potential of in situ imaging for process monitoring. © 2018 American Institute of Chemical Engineers AIChE J, 64: 2450–2461, 2018     

Enhanced fracture toughness in carbon-nanotube-reinforced amorphous silicon nitride nanocomposite coatings

Multiwalled-carbon-nanotube (MWCNT)-reinforced silicon nitride coatings were grown to evaluate the toughness contribution of nanotubes in a ceramic coating. An MWCNT array was first grown using catalytic chemical vapor deposition of acetylene on a silicon substrate. This aligned MWCNT preform was then infiltrated with an amorphous silicon nitride matrix by low-pressure chemical vapor deposition of dichlorosilane (DCS) and ammonia (NH₃). The fracture toughness of this material was determined by generating cracks using nanoindentation and then employing finite-element analysis to estimate the bridging toughness contribution of the MWCNTs. The MWCNT bridging toughness of the composites is determined to be ～5.6 MPa m^1/2, which is seven times higher than that of the matrix. The interfacial frictional stress is also estimated and ranges from 7 to 20 MPa.     

Methyl acrylate/1‐octene copolymers: Lewis acid‐mediated polymerization

Copolymerization of methyl acrylate (MA) with 1‐octene (1‐Oct) was conducted in the presence of free radical initiator, 2,2′‐azobis(2‐methylpropionitrile) (AIBN) using heterogeneous Lewis acid, acidic alumina. The polymers obtained were transparent and highly viscous liquids. The copolymer composition calculated from ¹H NMR showed alkene incorporation in the range of 10–61%. The monomodal nature of chromatographic curves corresponding to the molecular weight distribution in gel permeation chromatography (GPC) further confirmed that the polymers obtained are true copolymers. The number–average molecular weights (M_n) of the copolymers were in the range of 1.1 × 10⁴–1.6 × 10⁴ with polydispersity index of 1.75–2.29. The effects of varying the acidic alumina amount, time of polymerization, and monomer infeed on the incorporation of 1‐Oct in the polymer chain were studied. Increased 1‐Oct infeed led to its higher inclusion in the copolymer chain as elucidated by NMR. DEPT‐135 NMR spectral analysis was used to explicate the nature of arrangement of monomer sequences in the copolymer chain. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009