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  • Articles  (671)
  • Wiley  (671)
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  • 4519
  • 1
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    A Short Multi-step Flow Synthesis of a Potential Spirocyclic Fragrance Component (2015)
    Wiley
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    Publication Date: 2015-08-04
    Description: The search for novel chemical architectures displaying improved biological properties is a never-ending synthetic challenge. In this context many new test structures are often conceived by selecting and replicating specific design elements from naturally occurring molecules and displaying them in an alternative format by way of a new chemical assembly. Constructing these newly designed compounds can be a timely and expensive process especially when a large quantity of the target material is required for physiochemical and property testing. To permit easier scale up and safer working practice many chemical researchers are employing flow chemistry approaches to aid in their synthesis challenges. Herein we report on the preparation of a key spirocyclic lactone using flow based reaction processing techniques.
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  • 2
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    Mass Transfer from Single Taylor Bubbles in Mini Channels (2015)
    Wiley
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    Publication Date: 2015-08-08
    Description: Mass transfer from single CO 2 Taylor bubbles in vertical mini channels was measured for channel hydraulic diameters, D h , from 5.5 to 8.0 mm. The effects of channel geometries on the mass transfer were also investigated by using square ducts and circular pipes. Bubble rising velocities, v B , in the ducts were much faster than those in the pipes due to large liquid flow areas in the corners of the ducts. The values of mass transfer coefficients, k L , in the pipes were almost the same as those in the ducts, in spite of a large difference in v B . Sherwood numbers, Sh D , using D h as a characteristic length are well correlated in terms of the Eötvös number. The proposed Sh D correlation can well predict a long-term dissolution process of a Taylor bubble.
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  • 3
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    Numerical Simulation of Wetting Phenomena with a Phase-Field Method Using OpenFOAM® (2015)
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    Publication Date: 2015-08-19
    Description: The phase-field method coupled with the Navier-Stokes equations is a rather new approach for scale-resolving numerical simulation of interfacial two-phase flows. The intention is to implement it as finite-volume method in the open source library for computational continuum mechanics OpenFOAM® and make it freely available. An overview on the governing equations is given and the numerical method is shortly discussed. The focus is on application and validation of the code for some fundamental wetting phenomena, namely the capillary rise in a narrow channel and the spreading of a droplet on a flat surface, which is chemically homogeneous or regularly patterned. The numerical results on static meshes agree well with analytical solutions and experimental/numerical results from literature. Also, first 3D finite-volume simulations with adaptive mesh refinement near the interface are presented as a key element to achieve CPU-time efficient simulations. A phase-field method for interface resolving numerical simulations of two-phase flows is presented and implemented in OpenFOAM®. The method is validated for several capillary flows with moving contact lines and is used to study dynamic droplet spreading on a flat surface by three-dimensional simulations with adaptive mesh refinement near the interface.
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  • 4
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    Palladium theory of aqueous-phase Heck alkynylations for intensification of discovery and manufacture (2015)
    Wiley
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    Publication Date: 2015-08-04
    Description: The influence of water on the catalysis of biphasic Heck alkynylation, a family of palladium-catalyzed carbon-carbon bond formations, was investigated. Kinetic theory derived from Hatta moduli and pseudo-stationary-state approximations discovered that water, in coordination, reductive elimination, and product dissociation reaction steps of the deprotonation catalytic cycle, increases Gibbs energy barriers compared to values previously estimated by density functional theory calculations of purely organic syntheses involving an aryl iodide. On the contrary, water reduces the energy barrier of reductive elimination in the carbopalladation catalytic cycle. Quantum tunneling in proton transfer mechanism might account for the change. Water also influenced the rate-determining steps of the catalytic cycles, and its existence potentially switches the cross-coupling’s mechanism from deprotonation, previously thought to govern the reaction, to carbopalladation. Carbopalladation theory identified the ~35% of the Pd wasted during synthesis was ~10% greater than the amount predicted by deprotonation. Our discoveries enabled E-factor predictions that could someday help reduce chemical wastes generated during materials, natural products, and pharmaceutical manufactures. Theoretical groundwork is laid that enables data-driven research in the academic laboratory and data-driven development by the process chemist.
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  • 5
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    Continuous fuel cell catalyst preparation in a directly electrically heated tubular reactor (2015)
    Wiley
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    Publication Date: 2015-08-04
    Description: A continuous process to produce carbon supported platinum catalysts by polyol reduction was examined. The reactant dispersion was rapidly heated up to reaction temperature while flowing through a directly electrically heated tube followed by a downstream isothermic tubular reactor. Appropriate inner diameters corresponding to desired short heating-up times were calculated. A certain lower limit for the inner diameter is caused by temporary pluggings of particle agglomerates circumventing steady-state operation. Tube diameters were evaluated with respect to heating-up times and plugging. It was proved that with a tubular reactor a continuous preparation of carbon nanotube supported platinum catalysts with a low particle size and evenly distributed particles is possible.
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  • 6
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    Modeling separation processes in decanter centrifuges by considering the sediment build-up (2015)
    Wiley
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    Publication Date: 2015-08-08
    Description: This work focussed on the mathematical modeling of the separation process in counter-current decanter centrifuges, taking the influence of the sediment build-up and the flow pattern into account. Thus far, separation processes in centrifuges are calculated by means of simplified empirical models based on the so-called sigma-theory. To reduce experimental effort, we have developed a new model, which describes the separation process by considering material functions for sedimentation and the gel point. In addition to that, an arising sediment build-up and a change in the flow conditions are taken into account. The conducted numerical simulations are validated by experiments. Simplified models such as the sigma theory usually depend on experimental data of industrial machines. Our approach shows an enhanced accuracy while not depending on such information. The proposed simulation procedure is adaptable to other types of decanter centrifuges such as co-current machines.
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  • 7
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    Kinetics of catalytic oxidation of sulphite in diluted aqueous solutions (2015)
    Wiley
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    Publication Date: 2015-08-08
    Description: Catalyzed reaction of sulfite with oxygen is often used by industry for corrosion protection by chemical deoxygenation. The same reaction system is considered very important as a part of atmospheric chemistry due to SO2 immission modeling. In these applications, reaction kinetic data are of crucial importance. In deoxygenation, low concentrations of sulfite close to the stoichiometric ratio to oxygen are being used. Unfortunately, the values of kinetic constants for the reaction are sparse.The reaction kinetics was investigated in a rapid-mixing apparatus, where air or pure oxygen saturated solution containing the catalyst was mixed with aqueous sulfite solution. Mixing ratios with stoichiometric excess of dissolved oxygen were tested.Analysis of literature data suggests that the reaction is of 1.5 order in sulfite, 0 order in oxygen and 0.5 order in cobalt(II) catalyst. These reaction orders had been confirmed in the concentration range tested. The apparent kinetic constant and activation energy are also presented. Crucial importance of proper mixing of the two reacting solutions is reported, which was revealed during the development of the precise experimental technique providing reliable kinetic data.
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  • 8
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    Modeling of high concentration ethanol production by Mucor hiemalis (2015)
    Wiley
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    Publication Date: 2015-08-04
    Description: Inhibitory effects of high glucose and ethanol concentrations on ethanol production from wheat enzymatic hydrolysate by zygomycetes fungus Mucor hiemalis were investigated and modeled. Ethanol yield was decreased by increasing glucose concentration from 70 to 120 g.l -1 . Among different kinetic models, i.e., linear, Emerson, and modified Williams, modified Williams model was successfully described the fungal growth kinetics. Considering the inhibitory effect of glucose, a new model was developed for describing the rate of ethanol production. Moreover, the inhibitory effect of ethanol on ethanol yield, Y p/x , was modeled. The model prediction was successfully covered the experimental data.
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  • 9
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    Correlation for kLa-prediction of airlift loop reactors including the gas-phase residence time effect (2015)
    Wiley
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    Publication Date: 2015-08-08
    Description: In this study experimental mass transfer data and literature data of airlift loop reactors are analyzed concerning an effect of gas-phase residence time on the volumetric mass transfer coefficient k L a. It becomes evident that a neglect of the oxygen depletion can be regarded as a diminishment of the mass transfer driving force. The latter is found to be an important cause of the mass transfer dependency on the actual apparatus height of airlift loop reactors. Therefore a new correlation is presented which describes the volumetric mass transfer coefficients of airlift loop reactors by including the effect of gas-phase transient component concentration depletion. In this work two geometrically similar experimental apparatuses of different absolute size are utilized. Both of them are driven as airlift loop reactors with aerated concentric draft tube. The operating method is schematically illustrated in Fig. 3. The essential geometric data of the reactors is listed in Tab. 1.
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  • 10
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    Monolithic Honeycombs in Loop Reactor Configuration for Intensification of Multiphase Processes (2015)
    Wiley
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    Publication Date: 2015-08-08
    Description: Monolithic honeycomb reactors are characterized by small parallel channels, which make them an interesting approach to be applied as microstructured reactors. Besides the established manufacturing of ceramic honeycombs, these structures exhibit excellent mass transfer characteristics for multiphase reactions combined with degrees of freedom in the structural design. In this contribution the potential of monolithic honeycomb reactors operated in the beneficial slug flow regime is evaluated for heterogeneously catalyzed gas-liquid reactions. Therefore, results of the Fischer-Tropsch synthesis and hydrogenation of glucose to sorbitol were analyzed in order to obtain a more generalized picture of the interaction between mass transfer and reaction in small channels operated in multiphase flow.
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  • 11
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    Reforming of Methane in a Multi-Stage Microstructured Reactor (2015)
    Wiley
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    Publication Date: 2015-08-08
    Description: The concept of a multi-stage microstructured (MM) reactor has been tested in the bench-scale rig for combined steam and CO 2 reforming of methane (RM). In this reactor type the RM reaction is carried out in a series of adiabatic catalytic reaction steps with heat supply through fin-plate heat exchangers placed between the stages. RM reaction has been performed over a rhodium based catalyst in form of pellets. The experimental results have been described with a reaction engineering model that can be used as basis for model-supported scale-up. This paper describes an intermediate step in the development of the integrated reactor for thermal integration of oxidative coupling and reforming of methane. Conversion and yield near thermodynamical equilibrium have been achieved. Experiments confirmed advantages of the MM reactor against wall-coated micro reactors.
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  • 12
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    Gas-phase photo-oxidation: reactors and materials (2015)
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    Publication Date: 2015-09-11
    Description: This short review describes photocatalytic vs photosensitizing materials to be used respectively for gas-phase photooxidation and photo-oxygenation. The reactive oxygen species specific to photocatalysis and to photosensitization are summarized. Various kinds of gas-phase reactors and of photocatalytic materials are described in order to illustrate the great number of possible configurations and conditions of use. Some efforts towards standardization of gas-phase photocatalytic reactors devoted to indoor- or outdoor-air treatment are mentioned. Some examples of use of singlet oxygen in solvent-free photooxygenation reaction of volatile sulfides are given together with the properties of silica-based photosensitizing materials.
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  • 13
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    Photochemical Fluorination Reactions - A Promising Research Field for Continuous-Flow Synthesis (2015)
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    Publication Date: 2015-09-11
    Description: Fluorine and fluorine-containing groups are omnipresent in pharmaceuticals, agrochemicals and many other high-value chemical products like liquid crystals and organic electronics. The unique properties of fluorine resulting from its tremendously high electronegativity make this element a key player in the quest of enabling new and advanced qualities for chemical compounds and materials. With the advent of fluorinating reagents a great diversity of synthetic methodologies has been developed to incorporate fluorine or fluorine-containing groups into small molecules with high conversion and selectivity. Especially photochemically catalyzed fluorination reactions proved their potential for the synthesis of fluorine-containing fine chemicals due to their mild reaction conditions. This tutorial review gives an overview of recently published synthesis strategies that use (visible-) light-absorbing catalysts for the activation of fluorinating reagents. A special focus is made on the use of continuous-flow microreactors for photochemically catalyzed fluorination reactions due to the excellent utilization of this reactor equipment for photochemistry.
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  • 14
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    EFFICIENCY FACTORS IN PHOTOCATALYTIC REACTORS. QUANTUM YIELD and PHOTOCHEMICAL THERMODYNAMIC EFFICIENCY FACTOR. A REVIEW (2015)
    Wiley
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    Publication Date: 2015-09-11
    Description: This manuscript addresses the evaluation of photocatalytic efficiency using Quantum Yields (QY) and the “Photochemical Thermodynamic Efficiency Factor” (PTEF). While the QY can be considered as an early photocatalytic reactor efficiency factor, developed in the 80’s, the PTEF was first introduced by Serrano and de Lasa in 1997 [29]. The PTEF allows establishing reactor efficiency as the ratio of utilized enthalpy for the formation of consumed OH • free radicals over the absorbed photon energy. In all cases, a key consideration for the evaluation of efficiency factors is the establishment of macroscopic energy balances together with an accurate assessment of evolved and absorbed photons. Of considerable help, as well, are the experimental devices developed at the Chemical Reactor Engineering Centre (CREC)-University of Western Ontario laboratories. Furthermore, photoconversion kinetics is a required information for the calculation of the OH • consumption rates and the establishment of the related kinetic parameters. In this respect, de Lasa et al (2005) [6] postulated a unified “in series-parallel” model for the kinetics in photocatalytic conversion. Until today, both PTEFs and QYs have been used by CREC-UWO researchers for efficiency calculations in photocatalytic reactors for the decontamination of air, water and hydrogen production. This methodology is very relevant, in particular, for the assessment of the effects of reactor scale, reactor configuration, irradiation source, type of photocatalyst and model pollutant compounds.
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  • 15
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    Digital Imaging of Lithographic Materials by Radical Photopolymerization and Photonic Baking with NIR Diode Lasers (2015)
    Wiley
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    Publication Date: 2015-09-23
    Description: Photoinitiated crosslinking of multifunctional acrylic esters in polymeric binders was investigated based on digital imaging using the Computer to Plate (CtP) technology applying laser exposure at 830 nm in the near infrared (NIR). All coating components were applied as thin double layer film on Al-plates with an anodized surface. Materials exposed exhibit a sensitivity between 30-100 mJ/cm 2 . Processing of the exposed materials occurred in a weak aqueous alkaline bath. Generation of initiating radicals occurs by electron transfer from the excited state of the NIR-sensitizer to the radical generator – an onium salt. Several onium salts with distinct cation and anion pattern were synthesized. Iodonium salts derived from several borates and those with the bis(trifluoromethylsulfonyl)imide anion resulted in lithographic materials with high sensitivity. Photoinduced electron transfer plays a major function to generate initiating radicals by a sensitized mechanism but thermal events also influence sensitivity of the coating. Particular the radiationless deactivation of the NIR-sensitizer possesses a major function for selective release of heat. Internal conversion (〉85%) was the major deactivation pathway while a certain fraction of NIR-dye fluorescence (〈15%) was also available. Moreover, a line shape focused laser system with emission in the NIR (808 nm) was successfully used to bake the materials. This was initiated by the absorption of the NIR-dye embedded in the coating.
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  • 16
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    Overview Contents: Chem. Eng. Technol. 10/2015 (2015)
    Wiley
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    Publication Date: 2015-09-29
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  • 17
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    Cover Chem. Eng. Technol. 10/2015 (2015)
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    Publication Date: 2015-09-29
    Description: The cover represents on opening window which represents the Novel Process Windows concept. Inside the window, a photomicroreactor can be seen. In photochemistry, photons are used to activate organic substrates for reactions. More information on the photomicroreactor design and its application can be found in the paper by Su et al. Yuanhai Su, Ali Talla, Volker Hessel, and Timothy Noël Controlled Photocatalytic Aerobic Oxidation of Thiols to Disulfides in an Energy-Efficient Photomicroreactor Chem. Eng. Technol. 2015 , 38 (10) , 1733–1742 DOI: 10.1002/ceat.201500376
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  • 18
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    Overview Contents: Chemie Ingenieur Technik 10/2015 (2015)
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    Publication Date: 2015-09-29
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  • 19
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    Chemical Intensification in Flow – Novel Process Windows (2015)
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    Publication Date: 2015-09-29
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  • 20
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    Numerical simulation of the arrangement of baffles on radiation distribution and disinfection in UV reactor (2015)
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    Publication Date: 2015-11-25
    Description: The optimization of installation of baffles in UV rector is investigated. The flow field is obtained by solving continuity equation and momentum equation. The radiation intensity is solved by use of radiative transfer equation. The UV dosage is obtained by coupling Lagrangian particle tracking approach with the solved radiation intensity. One unbaffled reactor and two baffled reactors are simulated. The baffled UV reactor A has the biggest residence time and the smallest UV dosage while the baffled UV reactor B has the relatively bigger residence time and the biggest UV dosage. The unbaffled reactor performs between two baffled reactors in residence time and UV dosage. The baffled UV reactor B can get the best disinfection of microorganisms. The present study shows that the optimization must be coupled the flow field and the radiation intensity to attain a harmony between them.
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  • 21
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    A Review: Contaminant Degrading Microorganisms Identified Using Stable Isotope Probing (2015)
    Wiley
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    Publication Date: 2015-11-25
    Description: Stable isotope proving (SIP) enables function to be linked with identity without isolating the microorganisms responsible. This culture-independent approach has been adapted to identify the microorganisms involved in the degradation of numerous environmental contaminants. SIP studies have been performed in situ or in laboratory microcosms inoculated with soil, sediment, groundwater or bioreactor samples. This review focuses on the microorganisms that have been identified in those projects. SIP studies involving the degradation of polycyclic aromatic hydrocarbons, polychlorinated biphenyls, gasoline associated contaminants, chlorinated solvents, RDX, phenol, uranium and pentachlorophenol are discussed. This review brings to light the significant diversity of contaminant degrading microorganisms.
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  • 22
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    Segmented Flow-Based Multistep Synthesis of Cadmium Selenide Quantum Dots with Narrow Particle Size Distribution (2015)
    Wiley
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    Publication Date: 2015-05-30
    Description: A continuous-flow microreactor was used to synthetize II–VI semiconductor quantum dots (CdSe). In order to improve the size distribution of the nanoparticles, the synthesis was carried out in a two-step procedure. A seed solution was obtained in a separate nucleation step, followed by a controllable growth step. Quantum dots that are synthesized with the two-step method show a much narrower size distribution in comparison to those obtained in a conventional batch synthesis. Quantum dots are nanocrystalline semiconductors that differ greatly from their bulk counterparts. To obtain CdSe quantum dots with a narrow size distribution, a two-step procedure was applied, in which CdSe seeds were synthesized in a separate process prior to the nanoparticle growing procedure. The seeds were mixed into the growing solution-containing droplet by coaxial injection.
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    Process Intensification Tools in the Small-Scale Pharmaceutical Manufacturing of Small Molecules (2015)
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    Publication Date: 2015-05-30
    Description: The chemical process industry is paying significant attention to the intensification of processes with the main aim of achieving increased productivity, improved economic status, and enhanced sustainability. The pharmaceutical industry is moving in the same direction and, therefore, dozens of processes are in a state of change. However, it is important to note that not all processes can be intensified easily, such as slow chemical reactions, processes with solids, slurries, and on the like. This review summarizes applications of promising tools for achieving process intensification in the small-scale pharmaceutical manufacturing of so-called small molecules. The focus is on microwave radiation, microreactors, ultrasounds, and meso-scale tubular reactors. Promising tools for accelerating slow chemical reactions in organic synthesis in order to achieve process intensification are reviewed with the focus on microwave radiation, meso-scale tubular reactors, microreactors, and ultrasounds. Applications of such tools for producing small molecules in the pharmaceutical industry are discussed and illustrated with examples.
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    Integration of Fire and Explosion Index in 3D Process Plant Design Software (2015)
    Wiley
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    Publication Date: 2015-06-02
    Description: Process design management system is the essential computer-aided design type of software used in design and 3D modeling of process plants. Actually, it is a management center of process plant projects which allows designers and engineers from various disciplines to concurrently create, control, and manage changes to the plant design and other related engineering data. Some methods for achieving the inherently safer designs guide the location of process equipment and utilities. Therefore, there is room for close interactions between 3D modeling and methods to assess the inherent safety. The feasibility of integration of the Fire and Explosion Index into 3D modeling of industrial chemical processes is evaluated and supported by a case study. The importance of the presented concept as key part of such management philosophies like the lean design and the building information modeling is highlighted. In conventional process plant design, safety analysis is performed at the stage when the main design decisions were already made. The presented perspective allows placing the safety considerations using the Fire and Explosion Index (F&EI) in a 3D modeling environment. Results of the F&EI assessment can be visualized and shared between all disciplines involved in plant design.
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    Energy Optimization for a Multistage Crude Oil Distillation Process (2015)
    Wiley
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    Publication Date: 2015-06-02
    Description: Energy optimization is a hot research topic for design and operation of crude oil distillation plants. Optimum energy utilization in a multistage crude oil distillation process is achieved by optimizing the distillation load of each distillation column as well as the yield of the sidestreams of distillation columns. A generalized multistage distillation energy consumption model is proposed, and the optimal distillation load distribution is accomplished by minimizing the total energy consumption. Based on the optimal distillation loads, a nonlinear programming model is then formulated to determine the yields of sidestreams by maximizing the thermal exergy recovery for the crude oil plant. Finally, a four-stage crude oil distillation plant is investigated to demonstrate the performance of the proposed approach. The results show a decrease in energy consumption and an increase in heat recovery. The distillation load distribution of the distillation columns in a multistage crude oil distillation process is directly related to the energy consumption, and the yields of the sidestreams of these columns affect the thermal exergy recovery for the crude oil plant. These problems are formulated by an energy optimization approach combining mathematical programming and exergy analysis.
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  • 26
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    Particle Motion in Two- and Three-Phase Fluidized-Bed Reactors Determined by Pulsed Field Gradient Nuclear Magnetic Resonance (2015)
    Wiley
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    Publication Date: 2015-06-02
    Description: Pulsed-field gradient nuclear magnetic resonance (PFG-NMR) was employed to investigate the velocity distribution (propagator) and dispersion coefficient of a model fluidized-bed reactor of low aspect ratio containing mustard seeds. Both propagator and dispersion were found to be strongly anisotropic due to slug-flow conditions, with the vertical/axial dispersion ratio becoming smaller with increasing air flow rate. The influence of air humidity and flow rate was discussed in the gas-solid system, and the concurrent effect of electrostatic charging of particles close to the reactor wall was shown. Dispersion was generally found to increase with growing humidity and superficial gas velocity. For comparison, results are presented for a gas-liquid-solid system with a water-to-particle mass ratio of 2:1 as a function of bed height. The results indicated that the addition of water enhanced the particle motion in the bed. Velocity distribution and dispersion coefficient of a model fluidized-bed reactor of low aspect ratio was investigated by pulsed-field gradient nuclear magnetic resonance. For the first time, the feasibility is demonstrated to describe statistically the behavior in three-phase reactors with a dominating water component. Addition of water enhanced the particle motion in the bed.
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    Metathesis of 1-Hexene over Heterogeneous Tungsten-Based Catalysts (2015)
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    Publication Date: 2015-06-02
    Description: 1-Hexene metathesis was performed over standard and potassium-doped WO 3 /SiO 2 catalysts. The samples were tested at various reaction temperatures, molar feed compositions, and space times. Under the applied reaction conditions, doping with potassium reduced the isomerization and cracking activity of the catalyst by at least half and improved the yield of detergent-range alkenes twofold. However, increasing the potassium loading to a higher amount resulted in a significant reduction in the metathesis activity as both Brønsted and Lewis acid sites were affected. Optimum operating conditions for the yield of detergent-range alkenes were identified using response surface methodology. The metathesis of terminal linear alkenes can be applied for the valorization of secondary Fischer-Tropsch product streams. The performance of silica-supported tungsten trioxide catalysts was investigated for the gas-phase metathesis of 1-hexene in a fixed-bed reactor. Metathesis of 1-hexene yielded valuable detergent-range alkenes. Doping WO 3 /SiO 2 with potassium was found to reduce isomerization and cracking of 1-hexene.
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    Preliminary Design of a Vacuum Pressure Swing Adsorption Process for Natural Gas Upgrading Based on Amino-Functionalized MIL-53 (2015)
    Wiley
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    Publication Date: 2015-06-03
    Description: A preliminary study based on a conceptual process design methodology that includes a technical evaluation and an economic study has been carried out for the use of the metal-organic framework NH 2 -MIL-53(Al) as adsorbent for the separation of carbon dioxide from methane. Among the alternatives considered, a vacuum pressure swing adsorption was chosen in the detailed design phase. The combination of a design with columns in parallel and the possibility of recirculating some of the streams ensures a high degree of separation and a final product with high quality without compromising the operation costs. A comparison with the state-of-the-art technology, amine scrubbing, and with a process based on membranes demonstrates that the proposed process is competitive as a result of its low operation costs and the energy demand. A vacuum pressure swing adsorption process, based on the usage of the metal-organic framework NH 2 -MIL-53(Al) for the separation of CO 2 from CH 4 , is proposed based on a conceptual process design methodology. The analysis includes a technical evaluation, an economic study, and a comparison with the most widely applied technologies, proving the competitiveness of the proposed process.
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    Bidisperse Shrinking Core Model for Supercritical Fluid Extraction (2015)
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    Publication Date: 2015-06-03
    Description: The broken-and-intact-cell model is conventionally used for interpretation of overall extraction curves (OECs) observed in supercritical fluid extraction (SFE) of ground oilseeds. Another possibility, considered here, assumes that the packed beds of the ground material always contain a significant amount of very small particles, i.e., dust, which control the initial extraction rates. The bidisperse representation of particle ensembles allows accurate description of OECs on the basis of the modified shrinking core model. A simple asymptotic solution has been derived for bidisperse granulometric distributions under typical SFE conditions. Special microscopic observations have been performed to reveal and examine the dust fraction in ground seed substrates. A generalization of the shrinking core model for supercritical fluid extraction is introduced which takes into account the polydisperse nature of ground plant material. Model simplification adjusted for common extraction conditions, resulting in bidisperse approximation and simple asymptotic formulas is developed and successfully verified on experimental data from literature.
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    Application of Statistical Design to an Industrial-Scale Dead-End Ultrafiltration Process (2015)
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    Publication Date: 2015-06-03
    Description: An industrial-scale dead-end ultrafiltration system was optimized using statistically designed experiments. Given a certain level of pollutant, a two-level full factorial design and a central composite design were used to optimize the filtrate production of a single 8-inch industrial ultrafiltration membrane while manipulating the levels of four factors: feed pressure, backwash pressure, forward filtration time, and backwash time. Analysis of variance and residual analysis were used to validate and check the adequacy of the developed regression models. The optimal levels were later validated experimentally. The predicted filtrate production was in reasonable agreement with the experimental data. A two-level full factorial design and a central composite design were used to optimize the filtrate production of an industrial ultrafiltration membrane while manipulating the feed pressure, backwash pressure, forward filtration time, and backwash time. The obtained regression models were validated by analysis of variance and residual analysis. The optimal levels were then validated experimentally.
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    Formation of Salicylic Acid/4,4′-Dipyridyl Cocrystals Based on the Ternary Phase Diagram (2015)
    Wiley
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    Publication Date: 2015-05-27
    Description: The solubility behavior of salicylic acid (SAA)/4,4′-dipyridyl (4,4′-dipy) cocrystals is investigated in an ethanol solvent. The phase solubility diagram (PSD) of SAA/4,4′-dipy cocrystals is determined which are formed in a 2:1 stoichiometric ratio in ethanol. The objective is to improve the fundamentals of the formation mechanisms, solution behavior, and solid-state properties of SAA/4,4′-dipy cocrystals. The solubility behavior and solution chemistry of cocrystals are studied. It was found that the thermodynamic stability regions of the cocrystals and its components are defined by the phase solubility diagram. Besides the kinetic also the thermodynamic factor turned out to be important for the crystallization of cocrystals. Physical properties of active pharmaceutical ingredients can be tuned by pharmaceutical cocrystals without changing the chemical identity. The solubility behavior of salicylic acid/4,4′-dipyridyl (SAA/4,4′-dipy) cocrystals is investigated in an ethanol solvent to improve the fundamentals of the formation mechanisms, solution behavior, and solid-state properties of these cocrystals.
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    Inline Monitoring of Taltirelin Crystallization in Batch Cooling Mode Using Raman Spectroscopy (2015)
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    Publication Date: 2015-05-27
    Description: The polymorphic formation of taltirelin (TTL) was monitored inline by Raman spectroscopy in batch cooling crystallization. The concentrations of the polymorphic forms and supersaturation were measured during crystallization and transformation processes. Polymorphic transformation was detected by monitoring the Raman spectra of the two polymorphs in slurry state. The effect of cooling rate and concentration on the polymorphic crystallization was assessed. At a slow cooling rate and a low concentration, the stable form, i.e., the β -form, was nucleated directly without transformation from the α -form. The nucleation mechanism of the two TTL polymorphs was studied using the supersaturation profile tracked by Raman spectroscopy. In cooling crystallization, supersaturation can be controlled by the cooling rate. Profiles of concentration are helpful for understanding polymorphic crystallization. At a low cooling rate, the α -form of taltirelin is nucleated and then transformed to the β -form. The α -form is formed at a high cooling rate, while the β -form is generated at a very slow cooling rate.
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    Size Control of Atorvastatin Calcium Particles Based on Spherical Agglomeration (2015)
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    Publication Date: 2015-05-27
    Description: Atorvastatin calcium (AC) spherical crystals were prepared by spherical agglomeration. CH 2 Cl 2 acting as bridging liquid was added together with the drug solution or after the antisolvent precipitation process. Polymorph transformation in antisolvent crystallization and agglomeration processes was observed by focused-beam reflectance measurement (FBRM). The results suggested the occurrence of an immediate agglomeration when CH 2 Cl 2 was added together with the drug solution. Size-controllable AC spherical crystals with improved flowability and compressibility can be obtained by adjusting the amount of CH 2 Cl 2 and the stirring speed. The improved compaction behavior of the AC particles can be applied for direct tableting. A higher stirring speed can reduce the amount of bridging liquid which is required for effective agglomeration. It was a prerequisite for fine particles to be wetted by the bridging liquid in the spherical agglomeration process. Spherical agglomeration is an effective method to improve the flowability and compressibility of Atorvastation calcium particles. A polymorph transformation occurred during the antisolvent precipitation and agglomeration process. The final size distribution of the particles is controllable by adjusting the amount of bridging liquid and stirring speed.
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    Overview Contents: Chem. Eng. Technol. 6/2015 (2015)
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    Publication Date: 2015-05-27
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    Evaluation of a modified photobioreactor performance for bio-fixation of carbon dioxide by Chlorella vulgaris at different light intensities (2015)
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    Publication Date: 2015-05-27
    Description: The performance of a modified bioreactor inside a light enclosure for carbon dioxide (CO 2 ) bio-fixation by Chlorella vulgaris was investigated. The influence of different light intensities on CO 2 bio-fixation and biomass production rates was evaluated. The results showed that the photon flux available to microalgal cultures can be a key issue in properly optimizing microalgae photobioreactor performance, particularly at high cell concentrations. Although the optimal pH values for C. vulgaris range from 6-8, cell growth can take place even at pH 4 and 10. Batch microalgal cultivation in a photobioreactor was used to investigate the effect of different light intensities, including 30, 50, 100, 185 and 300 μmol m -2 s -1 . The maximum biomass concentration of 1.83 g L -1 was obtained at a light intensity of 100 μmol m -2 s -1 and 2 L min -1 of 2% CO 2 enriched air aeration. The performance of a modified bioreactor inside a light enclosure for carbon dioxide (CO 2 ) bio-fixation by Chlorella vulgaris was investigated. The influence of different light intensities on CO 2 bio-fixation and biomass production rates was evaluated. The results showed that the photon flux available to microalgal cultures can be a key issue in properly optimizing microalgae photobioreactor performance, particularly at high cell concentrations. Although the optimal pH values for C. vulgaris range from 6-8, cell growth can take place even at pH 4 and 10. Batch microalgal cultivation in a photobioreactor was used to investigate the effect of different light intensities, including 30, 50, 100, 185 and 300 μmol m -2 s -1 . The maximum biomass concentration of 1.83 g L -1 was obtained at a light intensity of 100 μmol m -2 s -1 and 2 L min -1 of 2% CO 2 enriched air aeration.
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    High-Throughput Synthesis of Uniform Silver Seed Particles by a Continuous Microfluidic Synthesis Platform (2015)
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    Publication Date: 2015-05-28
    Description: Controlled silver particle geometries require at least a synthesis in two steps which strongly differ in their reaction kinetics. For the first step, the very fast seed formation, chaotic advection-based micromixers are tested in combination with a batch reactor for the growth step. Nanoparticles with narrow size distribution and excellent shape uniformity can be prepared in large batches. To achieve a highly reproducible and homogeneous particle solution, a microfluidic system containing three different micromixers for optimal mixing of the chemical precursors is established, allowing stringent control of every synthesis step. The produced silver particles can be used as seeds for forming anisotropic particles. Their further potential is demonstrated by preparation of anisotropic silver triangles. The thus generated seed particles are better suited for growing to triangles than those from conventional batch synthesis. The synthesis of silver nanoprisms is realized in a novel microfluidic platform consisting of three different micromixers. Uniform crystalline particles were prepared, acting as seed particles for a second batch reactor-based synthesis. This reproducible synthesis platform allows for large-scale synthesis of plasmonic nanoparticles with defined dimension and plasmon resonance.
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    Polymorphism, Size and Shape Control of Calcium Carbonate Crystals in the Presence of a Polyelectrolyte (2015)
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    Publication Date: 2015-05-07
    Description: The effects of the presence of a polyelectrolyte on the polymorphism and particle size and shape of calcium carbonate crystals during reactive crystallization were investigated. Crystals were created by the single-jet reaction crystallization method. When polyacrylic acid (PAA) was added, the polymorphism and particle size and shape were different for each molecular weight of PAA and each experimental method. When sodium carboxymethylcellulose was added, the polymorph became different from those made by adding PAA and the particle sizes and shapes were different for each concentration. As a result, it is suggested that the method to achieve supersaturation, such as type of feeding, feed rate, kinds of polyelectrolyte and their concentration, may affect the polymorphism and particle size and shape of calcium carbonate. The effects of polyelectrolyte addition during reactive crystallization on the characteristics of calcium carbonate crystals were investigated. The supersaturation state, the material feed order, and the polyelectrolyte type and concentration were found to have great influence on the polymorphism, particle size and shape, and the crystal number of calcium carbonate.
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    Non-Equimolar Discrete Phases Formed in the System of Malic Acid Enantiomers (2015)
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    Publication Date: 2015-05-07
    Description: X-Ray diffractometry was employed to investigate the possibility of formation of non-equimolar discrete compounds in the chiral system of malic acid S - and R -enantiomers. Samples studied were mixtures of single enantiomers or an enantiomer and the various polymorphs of the racemic compound. From samples prepared via recrystallization of the melt and grinding of initial reactants, it is demonstrated that the malic acid enantiomers can form stable stoichiometric compounds in S : R ratios of 3:1 and 1:3. Compared to the known racemic and pure enantiomer phases, the corresponding compounds S 3 R / SR 3 are characterized by a proper powder diffraction pattern and melting point. Non-equimolar discrete compounds formed by malic acid S - and R -enantiomers in ratios 3:1 and 1:3 are investigated by means of X-ray powder diffraction. The corresponding S 3 R and SR 3 compounds are found to be stable or metastable phases in dependence on synthesis conditions. The phases are characterized and discussed with regard to their identity and crystallochemical nature.
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    Solubility Characteristics and Crystallization Behavior of Oxalic Acid in the Presence of Sulfuric Acid (2015)
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    Publication Date: 2015-05-07
    Description: Acidic wastewater from industrial discharge is generally treated by neutralization. Before neutralization or water treatment, selective recovery of valuable compounds is necessary to reduce the environmental impact of this acid waste. As a contribution to the development of a novel acidic wastewater treatment, oxalic acid is set as target material which is found in acid waste from the metalworking industry. Crystallization of oxalic acid in the presence of sulfuric acid has rarely been reported. Since this acid waste also contains aluminum ions, the effect of sulfuric acid and aluminum ions on oxalic acid solubility and crystallization was clarified. As a result, sulfuric acid concentration affected the oxalic acid solubility, but aluminum ions had no influence. Oxalic acid was precipitated in columnar shape by cooling crystallization from sulfuric acid aqueous solution with aluminum ions. For effective recovery of oxalic acid from acidic wastewater by crystallization, oxalic acid solubility was investigated and found to be influenced by sulfuric acid concentration. Based on the solubility data, cooling crystallization of oxalic acid in sulfuric acid aqueous solution was conducted. Columnar-type crystals of oxalic acid precipitated in sub-mm size.
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    Production of High-Tensile-Strength Paracetamol Tablets Using the Freeze-Casting Process (2015)
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    Publication Date: 2015-05-07
    Description: A fast-dissolving solid dosage form (tablet), containing in this case paracetamol as an active pharmaceutical ingredient and modified starch as an additive, was successfully produced by means of the freeze-casting process. The structure and two key properties, namely, disintegration time and tensile strength, of freeze-casted tablets were investigated. The produced tablets exhibit a threefold faster disintegration time with equal tensile strength in comparison to the commercial compressed tablets. Sugar as a binder, however, can just improve the disintegration rate but not enhance the tensile strength due to different mechanisms working. Low tensile strength limits the applicability of freeze-casted tablets in industrial production. Modified starch may serve as a binder for solid particles of the active pharmaceutical ingredient enhancing the mechanical strength of produced tablets. Freeze-casted paracetamol tablets are able to compete with commercial compressed tablets in terms of disintegration time and tensile strength.
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    Saccharose Inversion and Metastable Zone (2015)
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    Publication Date: 2015-05-07
    Description: In the production of beverages, cookies, and candies, citric acid is often used as preservative or flavoring agent. Due to the sensitivity in stability of saccharose concerning pH and temperature, it is necessary to know how these two parameters affect the inversion of sugar and therefore the changes in the characteristics of saccharose crystallization. It can be shown that the inversion speed increases with increasing temperature. Also, the exposure time to the acid as well as the amount of acid lead to an increased inversion and therefore need to be controlled in industrial processes. With a temperature difference of 10 °C, inversion increases by the use of 2.13 % citric acid, e.g., by more than 250 %. The metastable zone shifts, but does not change in its width while inversion takes place and the solubility and nucleation curves are shifted to lower temperatures. To control the crystallization of sugar such as saccharose in foods, knowledge of the position of the process in the phase diagram, and of the metastable zone in particular, is needed. The exposure time to citric acid and the amount of acid are shown to lead to an increased saccharose inversion. The metastable zone shifts to lower temperatures, but does not change in its width during inversion.
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    Relevance of the Second Harmonic Generation to Characterize Crystalline Samples (2015)
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    Publication Date: 2015-05-09
    Description: The application of powder second harmonic generation (P-SHG), temperature-resolved SHG (TR-SHG), and SHG microscopy (SHGM) in the characterization of bulk crystalline samples is illustrated. P-SHG applied to powder samples can be an extremely sensitive approach to detect the absence of an inversion center in crystalline structures, TR-SHG serves to monitor temperature-induced phase transitions, and SHGM is used in the detection of non-centrosymmetric zones inside a heterogeneous material. These methods are of great relevance, e.g., in the pharmaceutical industry where crystalline active pharmaceutical ingredients are often made of a single enantiomer and are therefore non-centrosymmetric. Herein, several examples are provided to describe how a given SHG signal should be interpreted. A general procedure to carry out a P-SHG experiment is illustrated in detail. The application of second harmonic generation-based techniques to characterize crystalline samples is presented. Several examples are detailed for chemical purity, structural purity and polymorphism studies, with particular relevance to the pharmaceutical industry where crystalline active pharmaceutical ingredients are often made of a single enantiomer and are therefore non-centrosymmetric.
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    Effect of Seeding and pH Conditions on the Size and Shape of Au Nanoparticles in Reduction Crystallization (2015)
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    Publication Date: 2015-05-12
    Description: Efficient and simple methods for gene integration into various plants have been studied by many researchers. The particle gun method using fine metal particles is one of the most potent technologies. However, it is difficult to control the particle size distribution and shape of the metal particles and, thus, to design and create adequate particles of suitable quality for the gene-supporting media. Here, reduction crystallization of nanometer- and submicron-sized Au was investigated in order to clarify the effects of the seeding and reaction conditions on the sizes and shapes of Au particles. The seed size has an influence on the surface roughness of the Au nanoparticles. Experiments to form Au particles were also performed using pH-controlled ascorbic acid. The pH has a great influence on the size and shape of nano/submicron Au particles and the mechanism of reduction crystallization. A simple method is suggested to control the sizes and shapes of nano/submicron-sized Au particles by reduction without additive to inhibit agglomeration. The mechanism of particle growth was analyzed by TEM-monitoring the crystallization process. The mean particle diameters of the Au particles were controlled at 6–650 nm by seeding or using pH-controlled ascorbic acid solutions.
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    Hydrogen Production by a Photosynthetic Bacterium: Some Analytical Solutions (2015)
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    Publication Date: 2015-05-14
    Description: The mathematical model for hydrogen production by the photosynthetic bacterium Rhodobacter capsulatus in a batch photobioreactor is discussed. An analytical method – the homotopy perturbation method – is presented to solve the nonlinear differential equations that describe the biomass formation, substrate utilization, and hydrogen production with respect to time. Approximate analytical expressions for the concentrations of biomass, substrate and hydrogen are derived for various values of the relevant parameters. The analytical results are compared with experimental data. In addition, the sensitivity of the kinetic parameters is also analyzed. The time required to achieve the maximum growth of biomass and complete degradation of the substrate is reported. Hydrogen can be produced by the photosynthetic bacterium Rhodobacter capsulatus. Here, the mathematical model for the production in a batch photobioreactor is discussed. Approximate analytical expressions for the concentrations of biomass and substrate and the production of H 2 were obtained in terms of the kinetic parameters. The sensitivity analysis of the model parameters is also presented.
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    Performance Comparison of Trisection Helical Baffle Heat Exchangers with Different Circumferential Overlap Sizes (2015)
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    Publication Date: 2015-05-12
    Description: The circumferential overlap structure is considered as one of the key factors which influence the performances of helical baffle heat exchangers by restraining the bypass stream between adjacent baffles. The flow and thermal performances of four trisection helical baffle heat exchangers with the same angle of inclination but different circumferential overlap sizes were numerically investigated. The four schemes involve an end-to-end one and three circumferential overlap ones with triangular area covering one row (20°TCO), two rows (20°T2CO), and three rows (20°T3CO) of tubes. The flow field and combined slices with pressure contours plus velocity vectors were depicted. The 20°TCO scheme proved to be superior to other schemes since its Nusselt number as well as its comprehensive index are the highest and its secondary flow is the strongest. The circumferential overlap trisection helical baffle heat exchanger is a modification based on a quadrant baffle and anti-shortcut structure to improve heat transfer performance. The mechanisms of heat transfer enhancement for four circumferential overlap structures were investigated. Pressure contours plotted with velocity vectors on special slices reveal secondary flow and bypass stream.
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    Overview Contents: Chemie Ingenieur Technik 5/2015 (2015)
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    Publication Date: 2015-04-25
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    Growth and Dissolution Kinetics of A and B Polymorphs of L-Histidine (2015)
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    Publication Date: 2015-04-30
    Description: The growth rate of the stable polymorph A and the dissolution rate of the unstable polymorph B of L -histidine ( L -his) in aqueous solution were experimentally determined at varying temperatures. The growth and dissolution kinetics were measured by means of desupersaturation and deundersaturation techniques, respectively. Both the growth and dissolution rates increase with higher temperature. At all temperatures studied, the dissolution rate of form B is faster than the growth rate of form A, indicating that the solution-mediated transformation of the polymorphs of L -his is likely to be controlled by the growth rate of form A. Both kinetics of the polymorphs of L -his will be used to characterize the polymorphic transformations and the overall crystallization rate of L -his. The essential amino acid L -histidine has shown to exhibit polymorphism and it exists in the solid phase as a stable polymorph A and a metastable polymorph B. The kinetics of growth and dissolution of the polymorphs which contribute to the rate of transformation between the polymorphs are investigated. The results indicate that the transformation is a growth-controlled process.
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    Dynamic Search Algorithm of Solubility in a Salt-Water System Based on the Solubility Product (2015)
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    Publication Date: 2015-04-30
    Description: An adaptive dynamic search algorithm is proposed to predict the solubility of salt in a salt-water system. It is not subjected to the impact of the initial probe whether the results are convergent or not. The thermodynamic basis for the proposed algorithm is discussed in detail and the iterations of the algorithm and the calculation error are quantitatively studied. The multiple calculated results and the experimental solubility data are compared. The algorithm proves its high accuracy and efficiency in theory compared to other algorithms, such as the Newton iteration algorithm. It possesses reliable potential for application in low-salt system dissolution equilibrium calculations. A dynamic search algorithm is introduced to predict the solubility based on equilibrium equations and solubility product in salt-water systems. A comparison between the calculated results of the algorithm and the experimental solubility data proves the high accuracy and efficiency of this algorithm. It exhibits great potential for low-salt system dissolution equilibrium calculations.
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    Correlation between Thermal Properties and Chemical Composition of Palm Oil Top Olein Fractions (2015)
    Wiley
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    Publication Date: 2015-04-30
    Description: A multistep dry fractionation method for modification of palm oil was adopted to achieve a high iodine value (IV) of the obtained palm olein, herein denoted as top olein. The effect of the composition of palm oil top olein on the IV and on the crystallization properties was analyzed in detail. Thermal properties of a series of olein and stearin fractions were evaluated by means of differential scanning calorimetry upon cooling. The composition of triacylglycerols in the products was investigated by high-performance liquid chromatography. IV analysis was carried out to measure the degree of unsaturation in these oil samples. Finally, an innovative and reliable method was developed to determine the IV of palm oils by relating the thermal properties with IV. The results agree well with those obtained by the traditional American Oil Chemists' Society method. In the palm oil industry, the iodine value is normally determined by a titration method that uses toxic solvents. An innovative method is proposed to quickly determine the iodine value of oil samples. This approach can provide statistically similar results to those given by traditional official procedures, with the advantages of being extremely rapid and environmentally friendly.
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    Analytic Setup for Multicomponent High-Pressure Phase Equilibria via Dual Online Gas Chromatography (2015)
    Wiley
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    Publication Date: 2015-04-30
    Description: A high-pressure analytic phase equilibria setup, capable of operation at 150 °C and 30 MPa, was developed. The variable-volume view cell contains two height-adjustable samplers enabling simultaneous sampling from two phases. Concurrent analysis of both samples was performed with dual online gas chromatography (GC). The GC comprises two inlets, four columns, two switch valves, and three detectors, arranged in parallel pathways. Quantitative detector calibrations were used. The setup was validated by sampling from a one-phase ternary of known composition, and comparison with binary and ternary literature data. The setup produces accurate phase composition data for supercritical systems and is well-suited to handle mixture constituents ranging from volatile gases to mid-length hydrocarbons. Supercritical fluid solvents may provide improved selectivity or solvating ability and enable the execution of difficult extractions. Ternary phase behavior data assist supercritical fluid extraction process design. A high-pressure static analytic phase equilibria setup was developed. The setup produces accurate supercritical phase composition data and can accommodate diverse mixture constituents.
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    Fast Measurements of the Gas-Liquid Diffusion Coefficient in the Gaussian Wake of a Spherical Bubble (2015)
    Wiley
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    Publication Date: 2015-03-28
    Description: A fast method is proposed for determining the oxygen gas-liquid diffusion coefficient from measurements of the fluorescence quenching behind a bubble. The approach consists of capturing pictures of the concentration field at micro-scale in the laminar bubble wake. The Gaussian concentration profiles measured in the wake are demonstrated to be systematically equivalent to an instantaneous plane diffusion case. The approach permits to accurately evaluate the gas-liquid diffusivity in a very short time of around one second. Since literature data on mass diffusion coefficients are actually not sufficient, a fast method is proposed to obtain oxygen diffusion coefficients from measuring the fluorescence quenching behind a bubble. Planar laser-induced fluorescence with inhibition presents a non-intrusive alternative method to accurately evaluate the gas-liquid diffusivity in a very short time.
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    Growth Rate Dispersion at the Single-Crystal Level (2015)
    Wiley
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    Publication Date: 2015-04-28
    Description: Evidence of growth rate dispersion for symmetry-related opposite faces of centrosymmetric single crystals of ammonium perchlorate is provided. Crystallization experiments conducted by evaporation of a stagnant aqueous solution at room temperature show that some faces have high and irregular normal growth rates, in time and space, whereas the corresponding faces crystallize slowly and steadily. The faces presenting high and irregular crystal growth also form repetitive inclusions, whereas faces are not involved in any formation of vacuoles. As a consequence, it is possible to retrace the crystallization history of a single crystal by analyzing the location of series of inclusions showing the progressive displacement of its center of gravity. Crystal growth rate dispersion of ammonium perchlorate crystallized by evaporation of an aqueous solution at room temperature is evidenced by considering some Friedel pairs of faces. The relationship between the formation of inclusions and a high growth rate of crystal faces is highlighted. Considering the locations of the inclusions, the results demonstrate a high heterogeneity of crystal growth rates, from which the history of crystal growth can be retraced.
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    Electrostatic Charge Measurements of Droplets of Various Liquids Falling over a Large Distance (2015)
    Wiley
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    Publication Date: 2015-04-28
    Description: In order to contribute to a better understanding of the electrostatic phenomena appearing during splash filling of liquids and to clarify the reasons why this process is suspected to increase static electrification especially due to atomization, accurate experiments of charge measurements were made on droplets of various liquids falling over a large distance (5 m). Eleven liquids of different conductivity and surface tension were tested. The results confirm that no charge evolution appears even over a long falling distance. A possible explanation of the static charge increase in splash filling is presented. Due to the generated electrostatic charges, the splash filling process poses some dangers. Here, the charge evolution of a single droplet is examined along its fall. From experiments with droplets of many different liquids, falling over 5 m, it is confirmed that the assumption that droplets are charged by friction with air, as still discussed in the explosion hazard community, does not hold true.
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    Combination of Reaction and Separation in Heterogeneous Catalytic Hydrogenation of Ethylformate (2015)
    Wiley
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    Publication Date: 2015-04-08
    Description: Continuous hydrogenation reaction of ethyl benzoylformate was studied over a (–)-cinchonidine (CD)-modified Pt/Al 2 O 3 catalyst. The catalyst showed a good stability, and high enantioselectivity was achieved in the fixed-bed reactor. Chromatographic separation of ( R )- and ( S )-ethyl mandelate originating from a post-continuous hydrogenation reaction of ethyl benzoylformate over the (–)-CD-modified Pt/Al 2 O 3 catalyst was investigated in the same reaction mixture. A commercial column filled with a chiral selector resin was chosen as a perspective preparative-scale adsorbent. Since adsorption equilibrium isotherms were linear within the entire investigated range of concentrations, they were determined by pulse experiments for the isomers present in a post-reaction mixture. Breakthrough curves were measured and described successfully by the dispersive plug-flow model with linear driving force approximation. An integrated concept for the production of optically active chemicals by heterogeneous asymmetric catalysis and chromatographic separation was developed. Feasibility to conduct continuous heterogeneous catalytic enantioselective hydrogenation of ethylbenzoyl formate in the same solvent as considered optimal for chromatographic separation of the products is demonstrated.
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    Polycation-Grafted Poly(vinylidene fluoride) Membrane with Biofouling Resistance (2015)
    Wiley
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    Publication Date: 2015-04-08
    Description: Covalent immobilization of polycations onto a membrane surface has been shown to significantly improve the resistance to biofouling. The poly(vinylidene fluoride)-graft-poly( N , N -dimethylamino-2-ethylmethacrylate) (PVDF-g-PDMAEMA) copolymer was synthesized via radical grafting copolymerization and fabricated into a flat membrane. The polycation membrane surface was constructed by quaternization of PDMAEMA side chains with 1,5- dibromopentane and diquaternization of 4,4′-bipyridine. As revealed by membrane surface morphology, pore size, and porosity measurement, the polycations are distributed on the membrane surface and internal pore channel surface. Water contact angles confirm that the incorporation of polycations remarkably promotes the surface hydrophilicity of a membrane. The polycation membrane surface provides an excellent bactericidal efficiency against Escherichia coli. Biofouling is a major obstacle for ensuring long-term effectiveness of a membrane process. A strategy is proposed to construct an antibacterial poly(vinylidene fluoride) membrane surface by covalent immobilization of cations. The polycation membrane surface exhibited an excellent antibacterial activity. Irreversible fouling was converted into reversible fouling.
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    Effect of pH on Aerobic Granulation and Treatment Performance in Sequencing Batch Reactors (2015)
    Wiley
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    Publication Date: 2015-04-08
    Description: Two sequencing batch reactors were operated to investigate the effect of influent alkalinity and reactor pH on aerobic granulation. In the first reactor R1 with high influent alkalinity the pH was adjusted in the neutral range, and in the second reactor R2 with low alkalinity the pH was held within the acidic range. The R1-dominating species were bacteria and the appearance time of granules was three weeks after reactor start-up. On the other hand, the acidic environment of R2 provided favorable conditions for fungal growth, and rapid granule formation occurred within the first week of operation. The varying microbial structure of granules resulted in different reactor performance in terms of evolution time and morphology of granules, suspended solids in the reactors, settling ability of granules, effluent quality of treated wastewater, and physical strength of the granules. Adjusting the pH of granular bioreactors has a great impact on aerobic granulation. Lowering the pH in the early stage of operation followed by a gradual increase helps in rapid formation and high strength of granules. The results are valuable for the development of full-scale aerobic granular bioreactors for wastewater treatment with rapid reactor start-up and good system stability.
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    Experimental Investigation and Simulation of Organophilic Pervaporation in Laboratory and Pilot Scale (2015)
    Wiley
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    Publication Date: 2015-04-09
    Description: Pervaporation is a well-established separation technology for the production of anhydrous solvents, but its distribution in the chemical industry is still limited to a few individual applications. Besides the need of high-selective membranes, the development of membrane modules adapted to the specific requirements of this process needs more research effort. Furthermore, only few modeling tools for the pervaporation process are available. In this work, a three-step modeling approach ranging from a shortcut to a rigorous model is developed. A hydrophobic membrane is characterized in a laboratory test cell for the separation of 2-butanol from water in a wide temperature and concentration range. The identified performance data are used to simulate the same separation task with an industrial-scale membrane module. The results are validated by experiments conducted with a novel membrane module in pilot scale. Only few modeling tools for the pervaporation process are available. A three-step modeling approach for simulation of industrial-scale pervaporation modules is described. The models are based on the design of a newly developed membrane module. Performance data of a hydrophobic membrane are identified in laboratory-scale experiments. Simulations of an industrial-scale membrane module are compared to experiments in pilot scale.
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    Techno-Economic Comparison of a 7-MWth Biomass Chemical Looping Gasification Unit with Conventional Systems (2015)
    Wiley
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    Publication Date: 2015-04-09
    Description: The chemical looping process is an alternative method to provide conventional gasification (CG) systems with the required oxygen. The syngas produced via chemical looping has a higher calorific value than that generated by a conventional process with air. For comparison, a conventional gasification unit with pure oxygen (CGPO) and a chemical looping gasification (CLG) system were simulated with Aspen Plus. The CGPO reactor consisted of a bubbling fluidized bed and sand as bed material with oxygen supplied via a pressure swing adsorption unit. The CLG comprised a bubbling fluidized-bed gasifier working in parallel with a fast fluidized-bed oxidizer. The total capital investment (TCI) of the CLG unit was higher than that of the CGPO unit but the annual operating cost of the former was less which repays the difference in TCI in less than six years. Chemical looping is an alternative method to supply conventional gasification (CG) systems with the required oxygen. As biomass gasification scenarios to produce high-concentrated syngas, CG units working with air or pure oxygen are compared techno-economically to chemical looping gasification. The latter approach is found to be a reasonable substitute for GC with oxygen.
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    Crystallization of Terutroban Sodium Salt Hydrate from the Deliquescent State (2015)
    Wiley
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    Publication Date: 2015-04-09
    Description: Terutroban sodium salt (Teru-Na) is a solid active pharmaceutical ingredient initially produced in its anhydrous form. The crystallization of a new dihydrate was established using liquid-assisted grinding and the liquid-liquid interface process. The stability of the Teru-Na crystalline phases was investigated as a function of temperature and relative humidity. A combination of analytical tools (spectroscopic, thermal, and vapor sorption analyses) highlighted the remarkable stability of the dihydrate, in particular under variable storage conditions. A rationalization of the stability hierarchy was proposed by means of phase diagrams. Besides studies on the crystallization processes of active pharmaceutical ingredients, stability studies at varying temperature and relative humidity are required. With Terutroban sodium salt as an example, the appearance of a hydrate (initially undesired) during storage is rationalized and its improvements in terms of stability are demonstrated.
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    Extraction of Spent Bleaching Earth in the Production of Renewable Diesel (2015)
    Wiley
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    Publication Date: 2015-04-15
    Description: The extraction of oils based on animal fat and vegetable oil from two types of spent bleaching earths, namely from the acidic sepiolite and the nonacidic palygorskite, was investigated by the Soxhlet method with hexane as a solvent. The yields of oil were independent of the feedstock, whereas a much lower oil yield was obtained with palygorskite exhibiting also a smaller surface area as compared to sepiolite which provided a higher yield. The glyceride compositions were very similar in bleached and extracted oils, while slightly lower melting and crystallization energies were determined by differential scanning calorimetry for the extracted oils bleached with acidic clay indicating minor hydrolysis of triglycerides. In the production of renewable diesel the feedstock is subjected to bleaching to remove undesired or harmful by-products. Oil extraction from acidic and nonacidic spent bleaching earths was investigated. The quality of the extracted oil was found to be similar to that of the bleached oil, especially considering the glyceride composition. The yields of oil were independent of the feedstock.
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    Extension of the Rapid Design Algorithm for Twisted-Tube Evaporative Fluid Coolers (2015)
    Wiley
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    Publication Date: 2015-04-15
    Description: The thermal analysis performance of evaporative fluid coolers (EFCs) is improved by replacing plain tubes by twisted oblong tubes. Results of the system are assessed by a rapid design algorithm (RDA) and compared to conventional plain-tube EFCs and other traditional algorithms including the effectiveness number of transfer units ( ϵ -NTU). Based on the RDA, a relationship between heat transfer coefficients, pressure drops, heat transfer area, and mass transfer coefficient is derived. Using the maximum allowable pressure drops in this algorithm, the minimum required heat transfer area can be determined. The algorithm is validated by comparing the plain-tube EFC design with twisted-tube design. The RDA-designed EFCs with twisted tubes provide higher efficiency compared with the traditional designs with plain tubes in such that the new design needs a lower heat transfer area for a given heat load. The application of twisted instead of plain tubes is a promising approach to increase the thermal efficiency of evaporative fluid coolers. Thermal and hydraulic analyses were performed by conventional methods and compared with an innovative rapid design algorithm. The latter minimizes the required heat transfer area, indicating a significant reduction of capital costs of such coolers.
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    Determination of Particle Size Distributions in Multiphase Systems Containing Non-Spherical Fluid Particles (2015)
    Wiley
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    Publication Date: 2015-06-20
    Description: The results presented in this study are obtained by means of automated image analysis software capable of measuring particle diameters in photographs taken in-situ by a two-dimensional (2D) photo-optical measurement device. Initially, the applicability of this measurement method must be proven for fluid particle systems on the basis of spherical-shaped particles. As a first approach in targeting the issue of irregularly shaped fluid particles, a pure gas-liquid system is analyzed to investigate the influence of the variation of operating parameters. In the second step, the spherical shape is deviated from by reducing the surface-active auxiliaries. The usage of shape factors helps to interpret the appearance of the 2D projected objects. By examining the capabilities and limitations, it is shown that the size of fluid particles can be detected online and in-situ in order to analyze and control the particular chemical process.
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    Software for simulation of second generation ethanol production by simultaneous saccharification and fermentation process (2015)
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    Publication Date: 2015-06-20
    Description: Concern about the environmental impacts associated with the consumption of fossil fuels and the need to generate power through renewable resources, is shown to be necessary to study the use of alternative materials. The objective is the production of clean energy like lignocellulosic biomass to produce second generation ethanol (2G). This work consists in elaborating a software in the Matlab program to simulate the simultaneous saccharification and fermentation (SSF) process of lignocellulosic biomass for the 2G ethanol production in batch reactor. Studying the effects of the process variables, it was found that the higher interference is caused by cellulose concentration. Greater concentrations of the product in batch processes are obtained with the maximum cellulose concentrations (60 gL -1 ), cells (0.468 gL -1 ) and enzyme (5.58 gL -1 ).
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    Cover Chem. Eng. Technol. 7/2015 (2015)
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    Publication Date: 2015-06-25
    Description: Insight by Nanostars: SERS-Sensing using Polymer/Silver Composite Particles in Flow Arrangements Chemical monitoring is a key demand for controlled processes in microreaction technology. Surface enhanced Raman scattering (SERS) gives the opportunity to get vibrational spectra even at moderate and lower concentrations. The introduction of silver nanoparticles into a nanoporous polymer microparticle and the implementation of such particles into a microflow arrangement allow a SERS sensing in a quasi-continuous process by alternating measurement and rinsing. The title collage shows the principle of fluidic arrangement for SERS sensing in front of the background of a polymer surface with incorporated Ag nanoparticles (“star sky”) with a high Ag-loaded sensor particle at lower magnification (“moon”) and a part of a polymer particle with incorporated small silver nanoparticles at higher magnification (“planet surface”). N. Visaveliya, S. Lenke, A. Groß, J. M. Köhler* Microflow SERS Measurements Using Sensing Particles of Polyacrylamide/Silver Composite Materials Chem. Eng. Technol. 2015 , 38 (7) , 1144–1149 DOI: 10.1002/ceat.201500035
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    Baseline Model for Simulation of Bubbly Flows (2015)
    Wiley
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    Publication Date: 2015-06-26
    Description: A key parameter appearing in closure relations for the Euler-Euler two-fluid model is the bubble size. A distribution of bubble sizes is established as a result of bubble-coalescence and -breakup processes. These processes are very complex and models are considerably less developed than e.g. for bubble forces and even bubble-induced turbulence. Therefore, a two-step procedure is adopted for model validation where in a first step measured values are substituted for the bubble size distribution. In this way the uncertainties of the less developed modeling for bubble-coalescence and -breakup are bypassed and a validation of the other parts of the overall model becomes possible. In a second step the previously qualified models for bubble forces and bubble-induced turbulence are used without any change and the validity of models for bubble-coalescence and -breakup can be assessed. This procedure is illustrated by application to a set of data obtained for vertical upward flow in a pipe. In the first step satisfactory agreement is achieved like in previous investigations. A first attempt at the second step shows promising results as well. From the observed level of agreement between simulation and experiment, issues requiring further investigation are identified.
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    Influence of Bubble-Surface Contamination on Instantaneous Mass Transfer (2015)
    Wiley
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    Publication Date: 2015-09-30
    Description: The relationship between instantaneous mass transfer, bubble motions, and bubble-induced surrounding liquid motions is discussed on the basis of precise measurements in time and space. The influence of bubble-surface contamination on the above is considered quantitatively through comparison with those in a purified system. The bubble's surface motion, centroid motion, volume, and surface area were acquired precisely from moment to moment using two high-speed cameras and an own innovative image processing method. The dissolution process of CO 2 was visualized via the laser-induced fluorescence/8-hydroxypyrene-1,3,6-trisulfonic acid (LIF/HPTS) method. Combining these experimental results carefully, the effects of the surfactant on the mass transfer, bubble motions, and vortex mechanism are discussed. Influences of the Marangoni effect, which is induced by the non-uniform distribution of surfactants adsorbed on the bubble surface, on instantaneous mass transfer, bubble's centroid motion, and surface oscillation are discussed based on precise experiment results. The resulting changes in bubble and liquid motions led to a decrease in the mass transfer in contaminated water.
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    Stability Study on Ethylene Oxide Industrial Reaction from the Management of Critical Process Variables (2015)
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    Publication Date: 2015-10-10
    Description: The performance of an ethylene oxide process is measured by the selectivity reaction. A production unit was studied in order to maximize selectivity by developing a strategy to manage key process variables. A statistical analysis of data indicated that four variables account for the influence over selectivity. Regression models were developed in order to represent the process selectivity as a function of these variables. The model proposed was statistically and phenomenologically validated, demonstrating consistency with the current data process. The model was deployed in subsets, representing possible operational conditions. Surface responses were evaluated for each model deployed and provided to identify the best operational conditions.
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    Revamping an existing aromatics complex with simulated moving bed reactor for p-xylene production (2015)
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    Publication Date: 2015-10-17
    Description: A Simulated Moving Bed Reactor (SMBR) for the production of p -xylene is studied as part of a proposal to modify an existing aromatics complex to increase the production of benzene and p -xylene. The proposed complex includes a single stage crystallization unit to further purify high p -xylene streams from a selective toluene disproportionation and said SMBR units. Mass balances for two cases are estimated, current flow of reformate fed to the complex and a twofold flow. Results show an increase of 170% and 72% of benzene and p -xylene for the first case and 447% and 241% for the second one compared to the current production of the complex. Moreover, p -xylene content about 75 wt% fed to the crystallization unit leads to a theoretical recovery of 95% within the unit.
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    Oligomerization of n-butenes in a two phase reaction system with homogeneous Ni/Al-catalysts (2015)
    Wiley
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    Publication Date: 2015-10-17
    Description: This paper describes the oligomerization of n -butenes in a two phase catalyst system consisting of a Lewis acidic ionic liquid IL and a non-polar phase. A highly active catalyst system with NiCl 2 (PMe 3 ) 2 was investigated, resulting 91% dimers with N -methylpyrrole as a buffer. Furthermore, the reaction was dependent on the molar ratio of the IL to the catalyst, where a ratio of 10:0.1 was optimal at a catalyst concentration of 0.3 mol%. Additionally, the authors investigated the influence of the Lewis acid and found that AlCl 3 was the most suitable for activating the nickel complex. The concentration of AlCl 3 played an important role in achieving high catalyst activity and dimer selectivity. Several reactions with different pyrrole derivatives showed that the use of a buffer with low steric hindrance was also important with regard to increased dimer selectivity.
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    Xylene isomerization in liquid phase using large-pore zeolites (2015)
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    Publication Date: 2015-10-20
    Description: Three large-pore zeolites, Beta with a Si/Al ratio of 25 and 35 and Mordenite with a ratio of 30, were studied in the conversion of o -xylene at 493 K. Maximum conversion was achieved by the catalyst with the highest Si/Al ratio due to faster diffusion of the isomer inside the zeolite channels because of the lower acidity of the solid even with larger crystal size. A kinetic study was then carried out over said catalyst between 473 and 513 K in a batch reactor in liquid phase. The activation energies obtained do not indicate the presence of diffusional constraints towards any isomer. Finally, the kinetic model obtained was simulated in a fixed-bed reactor and compared to ZSM-5 in the temperature range from 493 to 533 K. An increment of 20 % on average in p -xylene production was obtained.
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    Stereoselective Behavior of Nafion Membranes towards (+)-α-Pinene and (-)-α-Pinene (2015)
    Wiley
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    Publication Date: 2015-07-08
    Description: The α-pinene enantiomers were sorbed in Nafion membranes. The membranes included a commercial extruded Nafion® 115 membrane and the membranes prepared by casting a Nafion solution, evaporating the solvent and a thermal treatment at either 25°C or 60°C or 110°C. The microstructure of membranes was studied using SAXS, WAXS and MAS NMR spectroscopy. The change of membrane weight during the sorption process was determined using a sorption microbalance. A cast Nafion membrane treated at 25 °C sorbed considerably (-)-α-pinene however nearly did not sorb (+)-α-pinene, a cast membrane treated at 60 °C sorbed both (+/-)-α-pinenes to an intermediate extent while a cast membrane treated at 110 °C sorbed considerably (+)-α-pinene but sorbed negligibly (-)-α-pinene. The sorption of (+)-α-pinene and (-)-α-pinene in an extruded Nafion membrane was rather low.
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    Flow Simulation and Performance Comparison of Rough-cut Cyclones with Different Structures—in Dilute Phase (2015)
    Wiley
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    Publication Date: 2015-07-08
    Description: The gas-solid flow behavior and dust distribution in four rough-cut cyclones was numerically simulated on the platform of FLUENT 6.2. Reynolds stress model (RSM) and stochastic particle tracking model were used to describe the gas flow and particle motion respectively. The calculation results visualized that the particle distribution patterns of the four rough-cut cyclones were similar. Adding solid particles into the gas phase weakened the gas swirling intensity inside the cyclones. The most importantly, data of rough-cut cyclone down-flow ratios were gained by simulation for the first time. By analyzing the key factors (separation efficiency, gas down-flow ratio and pressure drop) of rough-cut cyclone performance, it was revealed that rough-cut cyclones with wider diplegs had massive gas down-flow through dipleg, which might cause serious coke generation inside the disengager. Among the four simulated structures, cyclone structure with its vortex finder wider than dipleg and a hopper installed behaved the best. The conclusion was expected to provide indications for industrial anti coke research and rough-cut cyclone design.
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    The Effects of Restitution and Specularity Coefficients on the Solid-liquid Fluidized Bed Hydrodynamics (2015)
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    Publication Date: 2015-07-08
    Description: An Eulerian-Eulerian two fluid model in combination with the kinetic theory of granular flow is used to simulate a solid-liquid fluidized bed filled with stainless steel particles. A set of experiments have been conducted in a solid-liquid fluidized bed and it has been shown that the drag model of Gidaspow used in CFD simulations is the appropriate model for predicting the bed hydrodynamics. At the next stage, the effect of particle’s restitution coefficient on the bed hydrodynamics was investigated numerically and it has been shown that the best results obtained at e=0.9. For the solid phase wall boundary condition according to Johnson and Jackson a specularity coefficient introduced and evaluated. The results showed that the change in specularity coefficient does not affect considerably the bed behavior at the middle part but at the walls it has a considerable effect on granular temperature. Moreover, it has been shown that for specularity coefficients more than 0.5 the results do not change noticeably.
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    Sequential Modeling of Heavy Liquid Fuel Combustion in a Fluidized Bed (2015)
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    Publication Date: 2015-07-08
    Description: A sequential model is developed to predict the fluidized bed reactor performance for combustion of heavy liquid fuels. The model consists of both hydrodynamic and reaction sub-models. The hydrodynamic sub-model is based on the modified two-phase theory and the reaction sub-model is adopted from the literature. Main reactions are assumed to be carried out in dense bed zone due to the rapid combustion reactions, and as a result the modeling has been done in this area. Dense bed is divided axially into several sections. Based on the source of bubbles, there are two types of bubbles: distributor bubbles which contain air bubbles from distributor and are free of fuel vapor and jet bubbles which are produced by jet (nozzle) and contain fuel vapor. In each section, the flow of gas through the emulsion phase is considered as completely mixed and through the both bubble phases as plug flow. Results of the model are presented in terms of combustion efficiency and exhaust emission concentrations. Effect of various parameters such as excess air, initial bed height and dispersing air rate on these two parameters is investigated. The model is validated with the experimental data reported in literature and a close agreement is observed between calculated and experimental values. Therefore, the proposed model can be applied for simulation of non-ideal fluidized bed combustors using heavy liquid fuels in industrial process simulators.
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    ReDrop - A simulation tool for the design of extraction columns based on single-drop experiments (2015)
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    Publication Date: 2015-07-16
    Description: The design of extraction columns based on information from lab experiments and appropriate simulation tools allows reduction of time and costs compared to conventional design methods using pilot-plant experiments. For this purpose, the behavior of drops and drop swarms is investigated in lab-scale experiments in order to create mathematical models containing system-specific parameters that have to be fitted to those experiments. These models are implemented in a simulation program that solves drop-population balances in extraction columns. At AVT-Thermal Process Engineering of the RWTH Aachen University this concept was implemented in the program ReDrop. ReDrop can predict the separation performance and flooding point of pulsed sieve-tray and structured as well as random-packing extraction columns for standard and technical systems. The program has successfully been extended to columns with rotating internals.
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    Comparison of Overall Gas-Phase Mass Transfer Coefficient for CO2 Absorption between Tertiary Amines in a Randomly Packed Column (2015)
    Wiley
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    Publication Date: 2015-07-16
    Description: The mass transfer performance of CO 2 absorption into an innovative tertiary amine solvent, 1-dimethylamino-2-propanol (1DMA2P), was investigated and compared with that of methyldiethanolamine (MDEA) in a packed column with random Dixon-ring packing. All experiments were conducted under atmospheric pressure. The effects of inert gas flow rate, amine concentration, liquid flow rate, CO 2 loading, and liquid temperature on mass transfer performance were analyzed and the results presented in terms of the volumetric overall mass transfer coefficient ( K G a v ). The experimental findings clearly indicate that 1DMA2P provided better mass transfer performance than MDEA. For both 1DMA2P and MDEA solutions, the K G a v increased with rising amine concentration and liquid flow rate, but decreased with higher CO 2 loading. The inert gas flow rate only slightly affected the K G a v . A satisfactory correlation of K G a v was developed for the 1DMA2P-CO 2 system. Tertiary amines are considered as potential solvents for CO 2 capture, but still suffer from low reaction rates with CO 2 . Compared to a common tertiary amine, 1-dimethylamino-2-propanol provided a higher mass transfer performance and CO 2 removal efficiency as well as a significant reduction of equipment cost of the CO 2 absorption process in packed columns.
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    Hydrogenation of Nitrobenzene over a Pd/Al2O3 Catalyst – Mechanism and Effect of the Main Operating Conditions (2015)
    Wiley
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    Publication Date: 2015-07-16
    Description: The catalytic hydrogenation of nitrobenzene (NB) was studied in a three-phase basket reactor and the catalyst used was a commercial 1 wt.% Pd/Al 2 O 3 sample. The kinetic experiments allowed a better understanding of the mechanism behind aniline (ANL) and by-products formation, a topic not yet well understood. The effect of some operating conditions was studied and it was found that there are more by-products than those referred in the literature; specifically, benzene formation was verified. It was also found that both the reaction kinetics and selectivity are strongly dependent on the temperature, while the effect of total pressure is not that pronounced. Moreover, the high selectivity of the catalyst used in the present work was put in evidence, and as such the deep hydrogenation of ANL to form by-products only occurs in considerable extension when NB concentration in the reaction mixture becomes negligible.
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    Effects of Electrospinning Parameters on Gelatin/Poly(ϵ-Caprolactone) Nanofiber Diameter (2015)
    Wiley
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    Publication Date: 2015-03-28
    Description: An electrospinning procedure was carried out to fabricate gelatin/poly( ϵ -caprolactone) (Gt/PCL) nanofibers. Response surface methodology based on a three-level, four-variable Box-Behnken design technique was used to model the resultant diameter of the as-spun nanofibers. A second-order model was obtained to describe the relationship between the fiber diameter and the electrospinning parameters, namely Gt concentration, PCL concentration, content of acetic acid in the overall solvent, and content of Gt solution in the blend solution. The individual and the interactive effects of these parameters on the fiber diameter were determined. Validation experiments verified the accuracy of the model which provided a simple and effective method for fabricating nanofibers with a controllable and predictable fiber diameter. In order to use the electrospinning process as a tool for producing materials with targeted fiber diameter for different applications, a simple method was developed for predicting the diameter of electrospun fibers. Validation experiments verified the accuracy of the model which offers an efficient method for fabricating nanofibers with a controllable and predictable fiber diameter.
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    Fluidized-Bed Chemical Vapor Deposition of Silicon on Very Dense Tungsten Powder (2015)
    Wiley
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    Publication Date: 2015-05-30
    Description: A very dense tungsten powder was coated by silicon from silane using the fluidized-bed chemical vapor deposition process. A reactor of reduced diameter was developed in order to decrease the weight of powders treated. Results show that the fluidization of this powder is possible in this reactor, but with non-optimal gas solid contact induced by the high powder density. Important disturbances of the fluidized-bed temperatures appeared in the presence of silane, due to a partial bed defluidization related to the cohesive nature of the deposit. These disturbances are clearly exacerbated by the exceptional density of the particles. This is probably why a powder agglomeration has been unavoidable when the bed temperature was too low and/or the silane inlet concentration too high. However, a set of operating parameters could be found, allowing a uniform and continuous coating of the whole powder surface. Very dense tungsten powders simulating nuclear fuel particles were coated by silicon from silane using fluidized-bed chemical vapor deposition in a reactor with reduced diameter. Fluidization of such particles could be reached, but with non-optimal gas-solid contact due to their high density. Conditions were found to form 0.5 µm thick continuous silicon layers on the powder surface.
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    Fabrication of a Chitosan-Coated Magnetic Nanobiocatalyst for Starch Hydrolysis (2015)
    Wiley
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    Publication Date: 2015-05-30
    Description: The preparation of chitosan-coated magnetic nanoparticles (MNPs) and covalent immobilization of α -amylase for starch hydrolysis was investigated. Surface morphology, chemical composition, and structural characteristics of the MNPs were analyzed by scanning electron microscopy, energy dispersion spectrometry, and X-ray diffractometry, respectively. Surface functional groups of MNPs, chitosan-coated MNPs, and α -amylase-immobilized MNPs were characterized by Fourier transform infrared spectroscopy. Response surface methodology based on three levels was implemented to optimize three immobilization conditions and a regression model was developed. α -Amylase-immobilized MNPs provided better stability towards pH and temperature. The prepared thermostable nanobiocatalyst is well-suited for industrial processes involving starch hydrolysis. Magnetic nanoparticles (MNPs) can serve as a superior solid matrix for enzyme immobilization. Covalent immobilization of α -amylase onto chitosan-coated MNPs was optimized by response surface methodology. This nanobiocatalyst with high temperature and pH stability can be applied in industries for economical and highly efficient starch hydrolysis.
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    An Experimental and Modeling Investigation on Catalyst Deactivation for Pd-Ag/α-Al2O3 for Acetylene Selective Hydrogenation (2015)
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    Publication Date: 2015-10-17
    Description: The selective hydrogenation of acetylene to ethylene over Pd-Ag/α-Al 2 O 3 catalysts prepared by different impregnation/reduction methods was studied. The best catalytic performance was achieved with the sample prepared by sequential impregnation. A kinetic model based on 1 st order in acetylene and 0.5 th order in hydrogen for the main reaction and 2 nd order independent decay law for catalyst deactivation was used to fit the conversion-time data and to obtain quantitative assessment of catalyst performances. Fair fits were observed from which the reaction and deactivation rate constants were evaluated. Coke deposition amounts showed a good correlation with catalyst deactivation rate constants, indicating that coke formation should be the main cause of catalyst deactivation.
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    An Investigation of the relationship between surface roughness, internal crystal perfection and crystal growth rate (2015)
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    Publication Date: 2015-10-17
    Description: This study investigates potential mechanisms affecting growth rate dispersion (GRD). Previous studies have identified surface roughness and internal lattice perfection as key mechanisms; this study investigates them both with respect to GRD. Crystal growth of potassium dihydrogen phosphate (KDP) was studied in two solvent mixtures, water and water-ethanol. The surface roughness was analyzed by atomic force microscopy (AFM) and the internal crystal perfection was analyzed by x-ray diffraction using a synchrotron source. The crystals grown at higher supersaturation have more pronounced and more frequent surface irregularities supporting previous findings on a feedback mechanism between surface roughness and growth rate. No significant relationship was seen between internal crystal perfection and growth rate, however, this is likely due to the size of the crystals analyzed in this study and not the absence of any such mechanism in small crystals.
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    Overview Contents: Chem. Eng. Technol. 11/2015 (2015)
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    Publication Date: 2015-10-24
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    Highlights: Chem. Eng. Technol. 11/2015 (2015)
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    Publication Date: 2015-10-24
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    Filter Press Performance for Fast-Filtering Compressible Suspensions (2015)
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    Publication Date: 2015-10-16
    Description: In some batch filtration processes, highly permeable suspensions dewater fast compared to the rest of the process. This work explores the impact of fast-filtering compressible materials on the throughput of fixed-chamber filter presses. The dewatering properties for a compressible yet highly permeable minerals processing slurry are used as inputs to a filter press model to explore the effects of operating and design parameters. For fast-filtering materials, maximum throughput is achieved with wide cavities and minimal handling time, while membrane resistance can be significant. Pressure affects the maximum achievable concentration, as given by the strength of the material. Overall, this work demonstrates the combined use of material characterisation and device modelling for filter press optimisation.
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    Influence of wall effects during solid liquid filter test on filter up-scaling (2015)
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    Publication Date: 2015-10-16
    Description: Industrial solid liquid filtration units are up-scaled based upon laboratory tests, often by a resistance meter. Wall or boundary effects are more pronounced during lab tests compared with full scale units where these effects might be negligible. Thus, simply using area specific rates from lab tests may lead to a significant up-scaling error. Intentional alterations of wall lengths and filtration areas are performed to allow quantitative description of this effect. Smaller area and longer wall length result in faster cake build-up as well as higher air consumption during subsequent cake drying. This indicates that the permeability close to the walls is different. Extrapolation towards negligible specific wall areas is used to improve up-scaling calculations.
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    Modeling of a methanol synthesis reactor with MATLAB for the storage of renewable energy and the conversion of CO2 – comparision of two frequently used kinetic models (2015)
    Wiley
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    Publication Date: 2015-10-16
    Description: The storage of renewable energy over a long time period, via methanol synthesis, will become very important to reach a greenhouse gas free energy supply. In this work a steady state methanol synthesis flowsheet, containing a 2-D pseudo-homogeneous reactor, flash and recycle, is modeled in MATLAB. With the kinetic models of Graaf and Bussche and Froment, two frequently used kinetic models used for conventional methanol synthesis are compared and evaluated for applicability regarding methanol synthesis from CO 2 /H 2 . The results are presented for different cases of synthesis gas compositions. Both kinetic models produce similar results when the system is limited by thermodynamic equilibrium. Differences in reaction rates are however observable from the reactor axial molar component profiles of the reaction products.
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    Dynamic Modeling of Filter-Aid Filtration Including Surface- and Depth-Filtration Effects (2015)
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    Publication Date: 2015-10-20
    Description: A new mechanistic model for filter-aid filtration with incompressible cakes is presented. Surface- and depth-filtration effects are considered based on a continuum mechanics approach. This leads to a moving boundary problem with sharp moving fronts. Proper mathematical and numerical methods for its solution are identified which allow fully transient simulations concerning all process variables and parameters. All relevant physical phenomena known from experimental studies are captured by the model, some of them for the first time. In two case studies, the effects of changing the filter-aid particle diameter at a discrete time point and continuously varying the amount of filter aid with time are considered. Significant influences on the separation efficiency, the local deposit profile within the filter cake, and the overall pressure drop are found.
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    Heterogeneous Catalytic Polymerization of Ethylene in Micro Tubular Reactor Systems (2015)
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    Publication Date: 2015-10-20
    Description: The feasibility of using a micro tubular reactor for heterogeneous polymerization of ethylene has been investigated experimentally. Chemically inert polymer tubing of inner diameter 800 ~2300 μm has been fabricated and used as a polymerization reactor at 75 o C and 2.72 bar of ethylene pressure. 400 nm-diameter nonporous silica nanoparticles were synthesized and used as a support for a high activity rac -ethylene(indenyl) 2 ZrCl 2 catalyst with methylaluminoxane as a cocatalyst and toluene as a diluent. Large diameter micro tubular reactors were also successfully used to conduct heterogeneous polymerization of ethylene in continuous reaction operations. High initial catalyst activity was obtained and the overall polymerization activity per volume or reactor length was quite high. No particle fragmentation occurred and the polymer particles were covered with small subgrains or nanofibrils of diameter of 30 nm.
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    Cover Chem. Eng. Technol. 11/2015 (2015)
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    Publication Date: 2015-10-24
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    Modeling of a methanol synthesis reactor with MATLAB for the storage of renewable energy and the conversion of CO2 – comparision of two frequently used kinetic models (2015)
    Wiley
    Details
    Publication Date: 2015-10-16
    Description: The storage of renewable energy over a long time period, via methanol synthesis, will become very important to reach a greenhouse gas free energy supply. In this work a steady state methanol synthesis flowsheet, containing a 2-D pseudo-homogeneous reactor, flash and recycle, is modeled in MATLAB. With the kinetic models of Graaf and Bussche and Froment, two frequently used kinetic models used for conventional methanol synthesis are compared and evaluated for applicability regarding methanol synthesis from CO 2 /H 2 . The results are presented for different cases of synthesis gas compositions. Both kinetic models produce similar results when the system is limited by thermodynamic equilibrium. Differences in reaction rates are however observable from the reactor axial molar component profiles of the reaction products.
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    Virtual Force Term Based on the Velocity Distribution Surrounding a Spherical Particle Settling in a Simple Shear Flow (2015)
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    Publication Date: 2015-10-16
    Description: Recently, the inside-out property of the interaction term in the two-fluid model equation was revealed, and the mathematical expression for the virtual force term, which compensates the gap between the correct interaction term and the conventional interaction term, was given. In this work, analytical solutions are given for the velocity field surrounding a spherical solid particle settling in a simple shear flow. The convection term in the Navier-Stokes equation was neglected. The virtual force term is calculated on the basis of the analytical solutions. The horizontal and vertical components of the virtual force term are 2.5 times the product of the viscosity, the velocity gradient, and the holdup gradient. These terms should be considered in the two-fluid model equation to simulate the dispersed multiphase flow with spatial distributions of velocity and holdup. Two-fluid model equations have been widely used to calculate macroscopic properties of multiphase flow across time and space. Here, analytical solutions are given for the velocity field surrounding a spherical solid particle settling in a simple shear flow, neglecting the convection term in the Navier-Stokes equation and a simple model for the virtual force term is proposed.
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    Production Rate - Dependent Key Performance Indicators for a Systematic Design of Biochemical Downstream Processes (2015)
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    Publication Date: 2015-10-20
    Description: Key performance indicators have become a common tool in bioprocess development, as they allow an objective and independent rating and ranking of process alternatives screened. Disadvantage of all key performance indicators developed so far is their strong focus on costs, which makes them neglect the influence of the production rate on the process’s profit. But, since both production costs and production rate have equally strong impact, both should be considered when decisions have to be made. Therefore, two new key performance indicators are introduced in this work, one for batch and one for continuous processing. They combine product yield, purity performance, variable manufacturing costs, and production rate to one objective. Thereby, misguided trade-offs between these four individual measures can be replaced by one key performance indicator. This ensures a systematic development of biochemical downstream processes.
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    Overview Contents: Chemie Ingenieur Technik 11/2015 (2015)
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    Publication Date: 2015-10-24
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    Multiscale Multiphase Process Engineering (2015)
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    Publication Date: 2015-10-24
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    A microbial biosensor platform for in-line quantification of acetate in anaerobic digestion: potential and challenges (2015)
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    Publication Date: 2015-12-17
    Description: Real time measurement of volatile fatty acids (VFA) in anaerobic digestion (AD) is crucial for process monitoring and management. It is essential for establishing demand-driven biogas production, however to date it is not commercially available. We propose a novel microbial electrochemical sensor for in-line measurement of acetate and other VFA in AD. The measurement range as well as the measurement resolution and dynamic behavior of the biosensor were investigated under flow conditions. A measurement range of 0.5 to 5 mmol L -1 acetate with a resolution (R) of 0.25 and 1 mmol L -1 was determined. For application in AD the achieved measurement range is still too low, therefore measures to improve it as well as further application properties of the sensor are discussed.
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    Investigating Reasons for Filter Bag Failure and Developing a Method to Improve its Life Span (2015)
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    Publication Date: 2015-12-22
    Description: This paper reports a study on the reasons for filter bag failure at steel plants and suitable approach to overcome such problems is proposed. Clean and used filter bags were subjected to evaluate tensile and bursting strengths and air permeability properties. In order to simulate behavior of the filter bags under acidic conditions normally encountered in actual working environment, acid dew point test was conducted on the clean bags. The structural changes in all bags (clean, used and chemically treated) were analyzed under Scanning Electron Microscope (SEM). A significant reduction in tensile and bursting strengths was observed after acidic treatment with H 2 SO 4. One of the major reasons for the filter bag failure was attributed to poor acidic resistance of the bags. SEM images of the bags showed perceptible degradation of the fibers due to acidic treatments and also clogging of the filter bags with dust particles. In order to improve the life of the bags, these bags were coated with a mixture of acrylic binder (7% by weight) and nanoclay (2% by weight). Furthermore, filter fabrics were also produced from the spunlaced process and coated with the binder and nanoclay coatings for comparison with the commercial product. The results showed that commercial filters bags, as well as developed samples, showed improved resistance without any failure behavior.
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    Filtration process optimization: assessment of the rheological behavior of a filter cake at different moisture contents (2015)
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    Publication Date: 2015-12-23
    Description: Transferring a wet cake from a filter to a dryer or furnace could severely lower the productivity of a whole process when the wet cake exhibits high viscosity and a sticky paste behavior. Depending on their moisture content, three distinct regions of rheological behavior were identified. Among them, only the granular solid type had sufficient flowability during the transfer operation. It was possible to discriminate the flow behavior more quantitatively by determining two transition values of moisture content. Rheological measurements were carried out at a constant shear rate representative of that encountered in the mechanical transfer system used at plant scale. The use of a vane geometry for the rheometer was necessary to ensure an accurate repeatability of the viscosity measurements.
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    New Trends in Photochemical Engineering and Technologies (2015)
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    Publication Date: 2015-12-23
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    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
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    Highlights: Chem. Eng. Technol. 1/2016 (2015)
    Wiley
    Details
    Publication Date: 2015-12-23
    Print ISSN: 0930-7516
    Electronic ISSN: 1521-4125
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Published by Wiley
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