Static mixers: Mechanisms,applications, and characterization methods – A review

Static mixers and multifunctional heat exchangers/reactors (MHE/R) are qualified as efficient receptacles for processes including physical or chemical transformations accompanied by heat transfer due to their high productivity and reduced energy expenditures. The present work reviews recent conceptual and technological innovations in passive static mixers and continuous in-line reactors. Current industrial applications are discussed from a process intensification perspective, focusing on mixing and mass transfer performance. Typical experimental techniques employed to characterize and quantify the mixing process are explored. The work is complemented by a review of mixing fundamentals, knowledge of which allows the development of theoretical models crucial for the analysis of experimental data, like the chemical probe mixing assessment method. Considering the development of continuous flow equipment in numerous processes, advances in this field will certainly be of increasing interest to the scientific and industrial communities.     

Preparation and characterization of aluminium – containing MCM-41

Mesoporous aluminosilicate molecular sieves with the MCM-41 structure (Si/Al=20) have been synthesized using tetraethoxysilane (TEOS) and sodium aluminate (NaAlO₂) as Si and Al sources and hexadecyltrimethylammonium bromide (HTMABr) and varying several parameters during the preparation process. All the samples were characterized by X-ray diffraction (XRD), Fourier transformed infrared (FT-IR) and solid state MAS NMR spectroscopy. A significant improvement in the structure by using a novel method for template removal has been evaluated.     

Preparation and characterization of RuCl3 – Diamine group functionalized polymer

Gel-type resin with diamine functional groups, FCN, was used as a matrix for immobilization of ruthenium complexes. By reacting of RuCl₃ with swollen matrix of FCN polymer a series of Ru/FCN composites with various Ru loading (1%, 2%, and 4%) was prepared. All the characterization techniques (FT-IR, XRD, SEM, EDS, STEM, XPS, and DSC) proved the participation of functional groups in the coordination of Ru(III). These complexes contained both Cl- and N-ligands in various proportions depending on ruthenium loading in polymer. Taking into account the chelating character of N-ligands a hypothetical structure of octahedral Ru(III) complex coordinated to FCN polymer was proposed. 2%Ru/FCN when reduced by NaBH₄ exhibited catalytic activity in liquid phase hydrogenation of acetophenone. Higher selectivity in the presence of FCN supported Ru as compared to 2%Ru/Al₂O₃ catalyst toward 1-phenylethanol was observed.     

Preparation and characterization of alkali-free glass substrates with enhanced properties for TFT–LCDs applications

To obtain an alkali-free glass substrate with enhanced properties for thin-film transistor–liquid crystal displays (TFT–LCDs) applications, we chose a base glass composed of 3B₂O₃-15Al₂O₃-58SiO₂-22MgO-0.5SrO-1.5MgF₂ (mol%) for nucleation–crystallization. The results show that when the nucleation–crystallization processes of the base glass are 810 °C/6 h + 880 °C/6–9 h, the prepared GC/6–GC/9 glass-ceramics exhibit enhanced properties because of the precipitation of nano-sized cordierite. The transmittances in the visible range of the GC/6–GC/9 glass-ceramics exceed 85%, the densities are 2.564–2.567 g/cm³, thermal expansion coefficients are 2.934–3.059 × 10^-6/°C (25–300 °C), compressive strengths are 417–589 MPa, bending strengths are 141–259 MPa, Vickers hardnesses are 6.8–7.8 GPa, and strain points are approximately 735 °C. Considering these properties, the prepared GC/6–GC/9 glass-ceramics have good potential as candidate materials for alkali-free glass substrates. Additionally, these results demonstrate that it is feasible to improve the properties of alkali-free glass substrates by nucleation–crystallization.     

Preparation, characterization, and antibacterial activity evaluation of collagen–Zn complex

The different kinds of collagen–Zn complexes were prepared by zinc acetate, zinc chloride, zinc nitrate, and zinc sulfate reacted with collagen protein. Their antibacterial activities have been investigated by MIC method. It was found that the antibacterial activity of collagen–ZnSO₄ complex is better than that of others. To obtain a better antibacterial activity, collagen–ZnSO₄ complexes with different zinc amount were prepared using zinc sulfate as starting material. These complexes were characterized by FT-IR, XRD, and atomic absorption spectrometry. The results showed that zinc ion could chelate with N–H, C–O, and C=O group in collagen to form the stable complex. Antibacterial activities of collagen–ZnSO₄ complexes containing different Zn amount were evaluated against Escherichia coli and Staphylococcus aureus. The results suggested that antibacterial activity increases with the increase of zinc amount.     

Preparation and characterization of chitosan–zeolite composites

Double crosslinked chitosan–zeolite (CZ-2) and noncrosslinked chitosan–zeolite (CZ-0) composites were prepared and characterized by using Fourier transform infrared (FTIR) spectrometer, surface area analyzer, scanning electron microscope coupled with energy dispersive X-ray (SEM-EDX) spectrometer, thermogravimetric analyzer (TGA), X-ray diffraction analyzer (XRD) and carbon, hydrogen, nitrogen (CHN) analyzer. After crosslinking, CZ-2 showed a reduction in surface area and CHN content in comparison to chitosan, zeolite, and CZ-0. Crosslinking resulted in improved stability of CZ-2 in distilled water, acetic acid and NaOH as CZ-2 recorded the lowest percentage of swelling. XRD diffractograms confirmed the formation of composites as there was a marked difference in the peak intensity at 2θ = 19.8°. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Novel 3D scaffolds of chitosan–PLLA blends for tissue engineering applications: Preparation and characterization

This work addresses the preparation of 3D porous scaffolds of blends of chitosan and poly(l-lactic acid), CHT and PLLA, using supercritical fluid technology. Supercritical assisted phase-inversion was used to prepare scaffolds for tissue engineering purposes. The physicochemical and biological properties of chitosan make it an excellent material for the preparation of drug delivery systems and for the development of new biomedical applications in many fields from skin to bone or cartilage regeneration. On the other hand, PLLA is a synthetic biodegradable polymer widely used for biomedical applications. Supercritical assisted phase-inversion experiments were carried out in samples with different polymer ratios and different polymer solution concentrations. The effect of CHT:PLLA ratio and polymer concentration and on the morphology and topography of the scaffolds was assessed by SEM and Micro-CT. Infra-red spectroscopic imaging analysis of the scaffolds allowed a better understanding on the distribution of the two polymers within the matrix. This work demonstrates that supercritical fluid technology constitutes a new processing technology, clean and environmentally friendly for the preparation of scaffolds for tissue engineering using these materials.     

Preparation and characterization of poly-carboxymethyl-β-cyclodextrin superplasticizer

A new superplasticizer of poly-carboxymethyl-β-cyclodextrin (PCM-β-CD) was prepared by ring-opening polymerization of epoxy chloropropane and CM-β-CD using sodium hydroxide as initiator. The structure of PCM-β-CD was characterized by FTIR and NMR as well as GPC. The performances of the CM-β-CD were tested by measuring paste luidity, setting time, adsorption and zeta-potential. The result showed the performances of PCM-β-CD closed to the control polycarboxylate superplasticizer (PCs) used in this study, especially the fluidity loss is smaller and the setting time is longer than the PCs. The reason might be the synergism of the steric hindrance with the hollow truncated cone and the electrostatic repulsion from –COO^? groups. The mechanism of dispersion and retardation by PCM-β-CD was elucidated based on the results of adsorption properties and zeta‐potential of the cement particles. The study offers a new approach to synthesize superplasticizer based on β-CD and an alternative to concrete engineering.     

Preparation and characterization of MnOOH and β-MnO2 whiskers

MnOOH and β-MnO₂ whiskers are obtained for the first time in our work. MnOOH whiskers are chemically synthesized in the presence of cationic surfactant cetyltrimethylammonium bromide (CTAB). The product is obtained under extremely low surfactant concentrations under basic conditions, using MnSO₄·H₂O as the manganese source and ethylamine as the alkali source. After the subsequent heat treatment of MnOOH at 300 °C for 1 h, β-MnO₂ whiskers retaining the similar morphologies are obtained. Powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and thermogravimetry analysis (TGA) are used to characterize the products.     

Advantageous mechanochemical synthesis of copper(Ⅰ)selenide semiconductor,characterization,and properties

Copper(I)selenide-nanocrystalline semiconductor was synthesized via one-step mechanochemical synthesis after 5 min milling in a planetary ball mill.The kinetics of synthesis was followed by X-ray powder diffraction analysis and specific surface area measurements of milled 2Cu/Se mixtures.The X-ray diffraction confirmed the orthorhombic crystal structure of Cu₂Se with the crystallite size～25 nm.The surface chemical structure was studied by X-ray photoelectron spectroscopy,whereby the binding energy of the Cu 2p and Se 3d signals corresponded to Cu⁺and Se^2?oxidation states.Transmission electron microscopy revealed agglomerated nanocrystals and confirmed their orthorhombic structure,as well.The optical properties were studied utilizing ultraviolet-visible spectroscopy and photoluminescence spectroscopy.The direct bandgap energy 3.7 eV indicated a blue-shift phenomenon due to the quantum size effect.This type of Cu₂Se synthesis can be easily adapted to production dimensions using an industrial vibratory mill.The advantages of mechanochemical synthesis represent the potential for inexpensive,environmentally-friendly,and waste-free manufacturing of Cu₂Se.     

Preparation and characterization of poly ε-caprolactone-gelatin/multi-walled carbon nanotubes electrospun scaffolds for cartilage tissue engineering applications

Abstract

Designing scaffolds with appropriate mechanical properties is a challenge in tissue engineering. In this study the poly ε-caprolactone (PCL)/gelatin with 1?wt.% of multi-walled carbon nanotubes (MWNTs) fabricated through electrospinning method. The presence of MWNTs led to an increase in the hydrophilicity and tensile strength, while maintaining an appropriate level of porosity percentage. The bioactivity and biodegradation evaluation demonstrated that the scaffolds containing MWNTs presented more bioactivity and slower degradation rate. Cell culture study showed that the nanocomposite scaffolds did not have any cytotoxicity. According to the results, the PCL-gelatin/MWNTs nanocomposite scaffold can be appropriate for cartilage tissue engineering applications.     

Preparation and characterization of poly (ethylene glycol) grafted Ca-alginate fibers by γ-irradiation for biomedical applications

Radiation processing, being a physical process, is an environmentally friendly alternative to chemical modifications. It is economically viable, safe, and possesses several advantages over other conventional methods employed for modification and grafting. To improve the physico-mechanical properties of Ca-alginate fiber (CaAF), poly (ethylene glycol) (PEG) was grafted by applying γ-radiation of different intensities. The effect of γ-irradiation on the physico-mechanical, thermal, morphological, thermal and water aging, water, and simulated body fluid (SBF) uptake were evaluated. FT-IR results confirmed that PEG was successfully grafted onto Ca-alginate fibers by γ-irradiation. From the detailed experimental results, irradiation doses and PEG concentration were optimized for grafting processes. The results showed that 50% PEG and 2.5?kGy irradiation dose yielded the highest tensile strength. Differential scanning calorimetric (DSC) analysis showed that with increasing γ-intensity a decrease of dehydration temperature of the fibers had occurred. On the other hand, the glass transition temperature (T _g) increased with increasing irradiation dose. The tensile cracked surfaces of the grafted alginate fibers were analyzed by scanning electron microscope (SEM) in order to monitor their surface morphologies. The SEM images of the cracked surfaces demonstrated that spherical shape rods were present for irradiated fiber sample while no such rods were observed for non-irradiated fibers. The characteristic data obtained from SBF and water uptake, and water and thermal aging experiments indicated that CaAF grafted with 50% PEG by applying 2.5?kGy γ-irradiation can be potentially employed for biomedical purposes, such as surgical suture.     

Mullite/ β-spodumene composites: Preparation and characterization

Mullite/ β-spodumene composites were fabricated by the addition of 5 up to 20 mass% β -spodumene powder to mullite matrix. Both mullite and β-spodumene were prepared by sol-gel technique. The batches were uniaxially pressed into discs and rectangular bars, then pressureless sintered at 1400 °C up to 1700 °C for 1 h. Mechanical and thermal properties, as well as microstructure and phase composition were carried out on the sintered composites. The results show that although the increase in the soft β-spodumene reduces the hardness and the thermal expansion of the composites, they lower the firing temperature and enhance the flexural strength. The study indicates that β-spodumene content has a noticeable effect on the composites thermal expansion coefficient. It also shows that it is possible to tailor mullite/ β-spodumene composite with adjusted thermal expansion coefficient by changing the mullite to β-spodumene ratio.     

Preparation and characterization of electrospun polyurethane–polypyrrole nanofibers and films

Polyurethane (PU)–polypyrrole (PPy) composite films and nanofibers were successfully prepared for the purpose of combining the properties of PU and PPy. Pyrrole (Py) monomer was polymerized and dispersed uniformly throughout the PU matrix by means of oxidative polymerization with cerium(IV) [ceric ammonium nitrate Ce(IV)] in dimethylformamide. Films and nanofibers were prepared with this solution. The effects of the PPy content on the thermal, mechanical, dielectric, and morphological properties of the composites were investigated with differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), Fourier transform infrared (FTIR)–attenuated total reflection (ATR) spectroscopy, dielectric spectrometry, and scanning electron microscopy. The Young's modulus and glass-transition temperatures of the composites exhibited an increasing trend with increases in the initially added amount of Py. The electrical conductivities of the composite films and nanofibers increased. The crystallinity of the composites were followed with DSC, the mechanical properties were followed with DMA, and the spectroscopic results were followed with FTIR–ATR spectroscopy. In the composite films, a new absorption band located at about 1650 cm⁻¹ appeared, and its intensity improved with the addition of Py. The studied composites show potential for promising applications in advanced electronic devices. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Eutectic bonding of copper to ceramics for thermal dissipation applications – A review

Metallic copper, which has low electrical resistivity and high thermal conductivity, is widely used as an interconnector or substrate within microelectronic packages. If a small amount of oxygen is introduced to the surface of the copper, a eutectic liquid forms above 1065 °C. The eutectic liquid wets many ceramics well; it is thus possible to bond slightly oxidized copper to many ceramics directly. The present report summarizes previous results on three systems, Al₂O₃/Cu, AlN/Cu, and Si₃N₄/Cu laminates, prepared by the eutectic bonding process. The reported data demonstrate that ceramic/copper interfaces prepared with this technique are strong. Though little attention has been paid to the thermal characteristics of ceramic/copper laminates, the limited data suggest that the thermal conductivity of the laminates is high, the potential for using the laminates for thermal dissipation is thus high. In the present report, the current status for the technique is summarized; critical topics for further improvement are also proposed.     

Combustion synthesis and characterization of spherical α-MnMoO4 nanoparticles

In this study, α-MnMoO₄ nanoparticles were prepared by combustion synthesis method. The structural, morphological and electrical characteristics of α-MnMoO₄ were investigated using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, transmission electron microscopy and impedance spectroscopy. The structural parameters were calculated from XRD pattern which confirmed the monoclinic structure of α-MnMoO₄. FT-IR and Raman spectroscopy results revealed the presence of MoO₄ surface functional groups. The TEM and HRTEM investigations evidenced the presence of homogeneous distribution of spherical nanoparticles and high crystallinity of α-MnMoO₄. Moreover, the SAED patterns clearly revealed the polycrystalline nature of the material. The conductivity measurements had inferred the semiconducting property of α-MnMoO₄ and the maximum conductivity of 1.94 × 10^? 6 S/cm was attained at 540 °C.     

Synthesis and characterization of thermosensitive core–shell polymeric nanoparticles

Thermosensitive core–shell nanoparticles were synthesized by semicontinuous heterophase polymerization of styrene, followed by a seeded polymerization for forming a shell of poly(N-isopropyl acrylamide) (PNIPAM). Nanoparticles characterization by scanning transmission electronic microscopy showed core–shell morphology with average particle diameters around 40 nm. An inverse dependence of the particle size with temperature in the range 20–55 °C was identified by quasielastic light scattering measurements. As was expected for core–shell particles with PNIPAM as the shell, a volume phase transition near 32 °C was detected. In spite of thermosensitive properties of core–shell nanoparticles synthesized here, the volume percentage loss values were not so high, probably due to their relatively low content of PNIPAM.     

Hydrogels containing caffeine and based on Beetosan® – proecological chitosan – preparation,characterization, and in vitro cytotoxicity

Abstract

In paper preparation and characterization of hydrogels based on chitosan of bees’ origin and modified with caffeine have been reported. Surface morphology of hydrogel materials including their average porosity has been determined. Furthermore, study of the release of caffeine from hydrogels in different environments was determined. Subsequently, studies on cytotoxicity of hydrogels to fibroblasts and cancer cells has been defined. Based on the research it can be stated that honeybees constitute an interesting material that could be a valuable source of chitosan. Prepared hydrogels had a significant negative impact on the cancer cells and did not affect negatively on fibroblasts.