Novel Microwave-Assisted Synthesis of Renewable-Resource Based Carbon-Magnetite Nanocomposites

Abstract

Magnetic carbon-iron oxide nanoparticles have been synthesized using tannin, a renewable resource material, in combination with a microwave-based thermolytic process without the addition of any inert or reducing gas during the synthesis. The predominant iron oxide species present in these particles has been determined by XRD and FT-IR to be magnetite (Fe₃O₄). These iron oxide nanoparticles are embedded within a carbon matrix in small clusters generally ≤100 nm in size. The resulting powder is approximately 48% (w/w) magnetite, and has been characterized by magnetic susceptibility and SQUID analysis.     

Effective separation of magnetite nanoparticles within an industrial-scale pipeline reactor

ABSTRACT

Within the field of wastewater treatment, nano-adsorbents are a significant emerging technology; however, separation of the nano-scale particles after loading has proved to be an impediment to widespread industrial implementation. Magnetic collection of nanoparticles is a potential strategy for effective separation. Nano-scale magnetite is an effective adsorbent, is sufficiently magnetically susceptible, and is superparamagnetic, allowing re-dispersion following magnetic collection.

In this work, an in-line, water-cooled magnetic collection module was developed with collection efficiencies regularly exceeding 98%. Models were developed over various flow regimes. The role of cooperative magnetophoresis was demonstrated and a physical model has been proposed for adsorption upon particle agglomerations about magnetic core wires.     

Electrically Stabilized Expanded Beds for Sorption Separations

Abstract

Recent studies have shown that when high electric fields are imposed on expanded fluidized beds, motion of the particles can cease. This provides the potential for fixed bed operations with the void fraction sufficiently large that only moderate pressure drops are required, even with small particles. This paper explores the dielectric forces that inhibit particle motion in alternating-current electric fields and the potential and limitations of the concept for adsorption operations. The dielectric constants of the particles and the fluid, the size of the particles, the density and viscosity of the fluid, and the imposed electric field gradient are the variables of most importance to bed stabilization. In adsorption tests, the expanded-stabilized beds perform essentially as well as densely packed fixed beds but with only a fraction of the pressure drop.     

Diethylenetriamine Functionalized Silica Coated Magnetite Nanoparticles for Selective Palladium Ion Extraction from Aqueous Solutions

Abstract

The extraction of Pd(II) over Cu(II) from aqueous solutions by diethylenetriamine functionalized silica particles with superparamagnetic nanosized magnetite core (FeSiDETA) was compared to that of bare magnetite and silica coated magnetite (FeSi). FeSiDETA was found to quantitatively and selectively (at pH <4) extract Pd(II) ions as compared to the magnetite and FeSi with a considerable improvement in material robustness with regards to iron dissolution. FeSiDETA particles could potentially provide ion exchanger surface areas orders of magnitude greater than conventional ion exchangers and offer alternative novel magnetic processing techniques.     

Universal Delineation of Particle Separation Systems and Separation Results of Stratified Material

Abstract

Elements needed for a meaningful delineation of particle separation systems and prediction of separation results have been identified and characterized. The most important elements of particle separation systems are balance of forces or equivalent quantities such as energy, momentum, probability, etc., as well as particle trajectory, stratification of particles, and splitting the stratified material into products.     

Contributions of TMAH Surfactant on Hierarchical Structures of PVA/Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>–TMAH Ferrogels by Using SAXS Instrument

The magnetic hydrogels combining polyvinyl-alcohol (PVA) and Fe₃O₄ (magnetite)–TMAH (tetra-methyl ammonium hydroxide) have been successfully fabricated via a Freezing-thawing route. The magnetite nanoparticles were prepared from iron sands by using coprecipitation method. The transmission electron microscopy image revealed that the magnetite nanoparticles with a reaction temperature of 30 °C had the average particle size of 12 nm in clusters of aggregation. The result was similar to the particle size obtained from X-ray diffraction data analyzed by Scherer equation. Furthermore, synchrotron small angle X-ray scattering data were analyzed by using two lognormal distributions to calculate the distribution of the individual magnetite particles. Meanwhile, Teubner-Strey and Beaucage models were employed to observe the distribution of magnetite particles coated by TMAH as a surfactant. The data analysis showed that the magnetite particles within the magnetic hydrogels formed aggregations with diameters of cluster particles in the range from 13.1 to 31.8 nm. Interestingly, the diameter of clusters particle increased from 13.1 to 31.8 nm along with the increasing concentration of ferrofluids from 1 to 15 wt%. This phenomenon was predicted to result from the effect of TMAH as a surface reactant agent that prevented the aggregation by coating the surface of the magnetite nanoparticles.     

Synthesis and characterization of chitosan-coated magnetite nanoparticles using a modified wet method for drug delivery applications

Abstract

Immobilizing various chemical functionalities on the surfaces of magnetite nanoparticles extends these applications without affecting the overall magnetic properties of the coated nanoparticles. In this study, magnetite nanoparticles have been prepared in the presence of chitosan using a simple modified wet method. Composition, morphology and magnetic properties of the chitosan-coated nanoparticles were investigated. Results showed the formation of coating with various thicknesses on the surfaces of the superparamagnetic nanoparticles. This in turn reduced the magnetization of the nanoparticles to some extent. The least particle size obtained in the presence of chitosan was 10?nm.     

The deposition of haematite particles from flowing water

Deposition of 0.2 μ haematite (α – Fe₂O₃) particles from suspension in turbulently flowing water, Reynolds Number = 11000, onto metal tube surfaces has been studied with particular reference to the effect of pH. Measurements on stainless steel showed trivial deposition outside the pH range 5 to 8. Within this range deposition rose sharply to a peak at pH = 6.2. This is similar to the findings of Kuo and Matijevic (1980) who studied haematite particle deposition onto a packed bed of stainless steel beads under laminar flow conditions. This shows that particle/surface interactions govern deposition in this system and that hydrodynamic and geometric factors are secondary.     

Composite magnetic particles: 1. Deposition of magnetite by heterocoagulation method

In this paper we report synthesis and characterization of composite polymeric particles bearing magnetite inclusions and reactive β-diketone groups on the surface. Composites were prepared by two-step method in which first step requires preparation of the functionalized polystyrene core and during second step magnetite was deposited onto core particle surface. This procedure gives a possibility to obtain composite particles with core-shell morphology and both the core size and magnetite shell thickness can be varied. Highly monodisperse PS/AAEM microspheres were synthesized by surfactant-free emulsion polymerization. Change of monomer fleet-ratio gives a possibility to change effectively the final particle size of dispersions without strong changes in particle size distribution. PS/AAEM particles were characterized by light scattering techniques (DLS, SLS) and electron microscopy (SEM) with respect to their particle size and morphology of the surface layer. Magnetite was deposited in form of nano-crystals onto PS-AAEM particle surface by heterocoagulation process. It has been established that more uniform magnetite coating was obtained at lower base amounts used for synthesis of magnetite. Amount of the magnetite on the polymeric particle surface can be effectively controlled by changing the initial FeCl₂ and FeCl₃ concentrations and/or variation of the PS/AAEM core dimensions. It has been confirmed by separation centrifugation technique, that stepwise increase of the magnetite content on the particle surface decrease gradually the stability of colloidal system. Magnetization curves for composite particles indicate that deposited magnetite content is high enough to achieve considerable magnetic response to external magnetic field.     

THE STABILITY OF WET SPOUTED BEDS

ABSTRACT

In granulation, coating or drying of slurries on inert particles a liquid phase is added to a gas-spouted bed. The effect of liquid injection on spouting velocity, fountain height, bed pressure drop and stability of the spouting regime is examined in a 0.15 m diameter bed with four types of inert particles 2 to 5 mm in size, 1140 to 2880 kg/m³ in true density, and 1.3 and 1400 mPa·s in liquid viscosity. Key factors are the liquid content and the presence of cohesive forces due to liquid bonds between particles. In a spoutability chart the maximum spoutable liquid content is related to the ratio of inertial force of a particle to the viscous or cohesive force exerted onto the particle by the liquid film. The spoutability chart serves to define regions of stable spouting.     

STUDIES OF MAGNETITE DEPOSITION FROM A FLOWING SUSPENSION

The deposition of magnetite from flowing water suspensions is a problem particularly important in boiler plant. Measurements have been made of the rate of deposition of magnetite particles from suspension in demincraliscd water pumped through vertical aluminium tubes of 19 mm bore over a range of temperatures I2-75°C and Reynolds number 7900 to 88500 under isothermal conditions. Bulk concentrations of magnetite particles (of the order of 2 μm diameter) were in the range 200-600 ppm.

It would appear that deposition is mass transfer controlled. The initial deposilion rate for a given temperature and concentration varies as the suspension velocity to the power 0.73. The measured asymptotic deposition quantity varies as the suspension velocity to the power ?0.66.

The conclusions imply a sticking probability for the magnetite on to the aluminium lube walls as 1 for the experimental conditions.     

Synthesis of magnetite powder from iron ore tailings

Iron ore tailing—a waste material of mineral beneficiation plants, is used as a source of iron for synthesizing magnetite powder. Iron ore tailings containing 15.98% Fe₂O₃, 83.36% SiO₂ and 0.44% Al₂O₃ have been subjected to HCl digestion on a hot plate to extract the entire amount of Fe₂O₃ as FeCl₃. A portion of extracted FeCl₃ solution has been used to convert it to FeCl₂ via metallic iron formation by using NaBH₄ as a reducing reagent. Then, the left out FeCl₃ solution and derived FeCl₂ solutions (from FeCl₃) are mixed in an appropriate molar ratio (2:1) for synthesizing magnetite powder by the addition of alkali solution. The magnetite powder samples have been characterized by means of powder XRD, SEM, vibrating sample magnetometer and laser particle size analyzer. XRD study confirms the formation of magnetite phase. The magnetite particles synthesized in different ways show varying degrees of magnetization behavior which is attributed to the change in their particle size induced by the use of different precipitating reagents.     

The Sedimentation of Bimodal Distributions of Unflocculated Microspheres

Abstract

An improved analysis for sedimentation of binary mixtures (two particle sizes) is proposed and tested with data that include differences in both the particle sizes and densities and sedimentation in both the viscous region and the transitions region, between viscous and turbulent (inertial flow). The new analysis can be used for any ratio of particle sizes even when the particle sizes are relatively close. It has been successfully tested beyond the viscous region and with variations in particle density as well as particle size. Although one previous analysis has been successful in predicting most earlier binary data with particles of different size, the new analysis is believed to be better supported by physical principles and thus more reliably extrapolated to different conditions.     

Removal of Submicron Silica Particles from tert-Amyl Alcohol by Dielectric/Electric Packed Bed Filtration

Abstract

A packed bed with an applied electric field is used to remove submicron and nanometer particles from a nonconducting or slightly conducting solution. Several studies have shown that the application of an electric field to a packed bed significantly increases the performance of the filtration. To enhance the electric-field filtration efficiency, it is desired that the packing materials have a higher dielectric constant than the solution so that the electric-field lines will be diverted into the packing materials.

In the present studies, a dc voltage of 0 to 8 kV/cm is applied to a packed bed (2.5-cm diameter and 3.0-cm length) filled with 1-mm-diameter glass beads. The filtration medium contains submicrometer or nanometer SiO₂ particles dispersed in tert-amyl alcohol. Two particle sizes are investigated: the average particle sizes are about 300 nm and 50 nm, respectively.

Visible light spectrophotometry is used to estimate the amount of SiO₂ particles in the effluent. The experimental results are presented as a series of breakthrough curves. The effect of the applied electric field on the breakthrough curve on two different particle sizes is presented. Depending on the applied electric field and the conductivity of the system, heating of the packed bed may occur. The operating current and temperature of the packed bed are also presented.     

Decomposition of pyrite during pulverized coal combustion

The decomposition of pyrite in air, 2% oxygen in nitrogen and nitrogen atmospheres, has been studied at temperatures ranging from 300 to 1100 °C. Pyrite was found to lose sulphur from 300 °C upwards, to form pyrrhotite and haematite. In both 2% O₂ and N₂, magnetite forms above 800 °C in preference to haematite. In 2% O₂, an atmosphere which closely resembles boiler conditions, the maximum amount of haematite was found in the range 800–900 °C. Drop-tube experiments, using finely ground pyrite and pyrrhotite as starting materials, have shown that liquid iron sulphides form from 1000 °C upwards. This enables a deposit to adhere well to a metal substrate surface. Microstructural analysis has shown that these deposits consist of deformed spherical agglomerates with a porous internal structure. Burner impeller deposits, rich in iron, taken from a pulverized coal-fired utility boiler have been examined. By comparing the microstructures of the deposits with those from the drop-tube experiments, it has been possible to propound a mechanism for their formation. Preferential deposition of liquid iron sulphides followed by in situ oxidation, is believed to be the mechanism by which these deposits form.     

Simultaneous Elemental Composition and Size Distributions of Submicron Particles in Real Time Using Laser Atomization Ionization Mass Spectrometry

Composition and size of individual submicron particles have been measured using a laser atomization ionization mass spectrometry technique, the Particle Blaster. Individual particles are quantitatively converted to atomic cations, providing information on both their complete elemental composition and particle size. Measured average atomic ratios for 100 nm particles of sodium chloride is 1.12 +- 0.36 (Cl:Na), for 50 nm particles of silica is 1.93 +- 0.52 (O:Si), and for 64 nm polystyrene latex spheres (PSL) is 1.13 +- 0.19 (H:C), in excellent agreement with the empirical formulae. Calculated particle sizes agree well with electrostatic classifier or TEM measurements in the size range of 17-900 nm diameter for particles of sodium chloride, silicon, and PSL. Size distributions are also obtain able, giving narrower distributions than are measured with an electrostatic classifier, for particles of alumina, silica, sodium chloride, and PSL spheres. Comparison with TEM data shows comparable primary particle sizes, but numerous particle aggregates are detected by the Particle Blaster which are unreported by the TEM measurements.     

Effect of Angle of Attack on the Performance of an Airborne Counterflow Virtual Impactor

Abstract

A three-dimensional model has been developed within the framework of the commercial computational fluid dynamics program, FLUENT®, to investigate the collection efficiency of an airborne counterflow virtual impactor (CVI). The model assumes steady-state, isothermal, compressible, and turbulent flow. Particle trajectories are computed based on the Lagrangian discrete phase model (DPM). In addition to predicting the effects of flight velocity and counterflow rate on the particle collection efficiency, as do prior models, the model quantifies the effect of flight attack angle on the particle collection efficiency. With an angle of attack as small as 5^?, the CVI collection efficiency drastically degrades at large particle sizes, and only particles with intermediate sizes are collected. Smaller particles do not have sufficient inertia to fight the counterflow, and larger particles tend to impact the CVI inner walls and are lost to the CVI walls. The modeling results show that the alignment between the free stream flow and the CVI inlet is critical to the performance of the CVI.     

Picobubble Enhanced Fine Coal Flotation

Abstract

Froth flotation is widely used in the coal industry to clean ?28 mesh fine coal. A successful recovery of particles by flotation depends on efficient particle‐bubble collision and attachment with minimal subsequent particle detachment from bubble. Flotation is effective in a narrow size range beyond which the flotation efficiency drops drastically. It is now known that the low flotation recovery of particles in the finest size fractions is mainly due to a low probability of bubble‐particle collision while the main reason for poor coarse particle flotation recovery is the high probability of detachment. A fundamental analysis has shown that use of picobubbles can significantly improve the flotation recovery of particles in a wide range of size by increasing the probability of collision and attachment and reducing the probability of detachment.

A specially designed column with a picobubble generator has been developed for enhanced recovery of fine coal particles. Picobubbles were produced based on the hydrodynamic cavitation principle. They are characterized by a size distribution that is mostly below 1 µm and adhere preferentially to the hydrophobic surfaces. The presence of picobubbles increases the probability of collision and attachment and decreases the probability of detachment, thus enhancing flotation recovery. Experimental results with the Coalberg seam coal in West Virginia, U.S.A. have shown that the use of picobubbles in a 2″ column flotation increased fine coal recovery by 10–30%, depending on the feed rate, collector dosage, and other flotation conditions. Picobubbles also acted as a secondary collector and reduced the collector dosage by one third to one half.     

Charged Particle Trajectory Statistics and Deposition in a Turbulent Channel Flow

The statistical properties of charged particles and their wall deposition in a turbulent channel flow in the presence of an electrostatic field is studied in this paper. For a dilute concentration, the influence of small particles on the fluid motion is neglected. The instantaneous velocity field is generated by a direct numerical simulation of the Navier-Stokes equation via a pseudospectral method. The case in which each particle carries a single unit of charge and the case in which the particles have a saturation charge distribution are analyzed. Ensembles of 8192 particle trajectories are used for evaluating various statistics. Effects of size and electric field intensity on particle trajectory statistics and wall deposition rate are studied. RMS particle velocities and particle concentrations at different distances from the wall are evaluated and discussed. The results for deposition rates are compared with those obtained from empirical equations.     

An Investigation of Milk Powders Produced by a Laboratory-Scale Spray Dryer

ABSTRACT

A mini spray dryer has been used to investigate morphological changes that occur to milk particles during the spray drying process. We have found that the mini spray dryer is ideal for such investigations, because phenomena such as skin and vacuole formation in particles can be analyzed without the added complication of particle agglomeration, which only occurs in much larger spray dryers where particle number concentrations are higher. We have confirmed observations made by various researchers that the bulk density of spray-dried milk powder is greatly affected by the drying temperature, due to the strong influence of the latter on the porosity of the particles. In addition, we have attempted to explain observations made by various workers that fat accumulates preferentially at the surface of a particle during drying by postulating that fluid fat is transported towards the surface, via a network of cracks and pores, by the development of a vacuole overpressure which is also responsible for the inflation of the particle. Finally, we have shown that milk powders can be spray dried a second time, by reconstitution with water, with no change to the thermodynamic characteristics of the resultant powder. Thus, milk concentrates for spray drying research can be prepared from already-spray-dried milk powders rather than using the more arduous evaporation method to concentrate unprocessed milk.