FACTORS GOVERNING SURFACE MORPHOLOGY OF SPRAY-DRIED AMORPHOUS SUBSTANCES

ABSTRACT

Changes in particle morphology (size, shape, and appearance) have been monitored during drying of drops of foods and food-related materials. The apparatus produces a single stream of drops of uniform size, using a vibrating-orifice device for drop production. The drop size and the time-temperature history of the drops as they fall can be varied and controlled.

Qualitative observations are reported for drying of aqueous solutions of lactose, maltodextrin, skim milk, and coffee extract, with different feed concentrations. Particular emphasis is placed upon the tendency for development of folds upon the particle surface. A mechanistic model is developed, relating the tendency for folding to the extent of viscous flow of surface material in response to a surface-energy driving force. This model gives semi-quantitative agreement with observations for solutes of different molecular weight (and hence different viscosity) and for different feed concentrations.     

CFD Evaluation of Droplet Drying Models in a Spray Dryer Fitted with a Rotary Atomizer

Computational fluid dynamics (CFD) modeling of spray dryers requires a simple but sufficiently realistic drying model. This work evaluates two such models that are currently in discussion; reaction engineering approach (REA) and characteristic drying curve (CDC). Two versions of the CDC, linear and convex, drop in drying rate were included. Simulation results were compared to the overall outlet conditions obtained from our pilot-scale experiments. The REA and CDC with a linear drop in drying rate predicted the outlet conditions reasonably well. This is contrary to the kinetics determined previously. Analysis shows that the models exhibit different responses to changes in the initial feed moisture content. Utilizing different models did not result in significantly different particle trajectories. This is due to the low relaxation time of the particles. Despite the slight differences in the drying curves, both models predicted similar particle rigidity depositing the wall. For the first time in a CFD simulation, the REA model was extended to calculate the particle surface moisture, which showed promising results for wet particles. Room for improvement was identified when applying this concept for relatively dry particles.     

Surface Stickiness of Drops of Carbohydrate and Organic Acid Solutions During Convective Drying: Experiments and Modeling

Drying kinetics of low molecular weight sugars such as fructose, glucose, sucrose and organic acid such as citric acid and high molecular weight carbohydrate such as maltodextrin (DE 6) were determined experimentally using single drop drying experiments as well as predicted numerically by solving the mass and heat transfer equations. The predicted moisture and temperature histories agreed with the experimental ones within 6% average relative (absolute) error and average difference of ± 1°C, respectively. The stickiness histories of these drops were determined experimentally and predicted numerically based on the glass transition temperature (T_g) of surface layer. The model predicted the experimental observations with good accuracy. A nonsticky regime for these materials during spray drying is proposed by simulating a drop, initially 120 µm in diameter, in a spray drying environment.     

HEASUREHENT OF INSTANTANEOUS RATES OF LOSS OF VOIATILE COMPOUNDS DURING DRYING OF DROPS

A novel technique serves to monitor instantaneous rates of loss of a volatile solute from a suspended drop during drying. A highly sensitive electron capture detector is used to monitor concentrations of SF6 released into a flowing gas stream from a suspended, drying drop. Simultaneously, the appearance and morphological development of the drop are monitored with a video camera. This provides the wherewithal of relating instantaneous rates of loss of the volatile solute to particular events during the development of particle morphology.

Initial experiments have been carried out with drops of aqueous solutions of glucose, sucrose, maltodextrin and coffee extract. The results clearly display the onset of the volatiles-retentive selective diffusion phenomenon. There is also substantial loss of the volatile component later in the drying process, when the drops undergo repeated ex ansion, bursting and cratering due to the formation of internaf bubbles. These experiments appear to be the first quantitative demonstration of major losses accompanying changes in drop morphology.     

Pressure-drop predictions in a fixed-bed coal gasifier

In the Sasol Synfuels plant in Secunda, Sasol-Lurgi fixed-bed dry-bottom gasifiers are used for the conversion of low-grade bituminous coals to synthesis gas (syngas). The gasifiers are fed with lump coal having a particle size in the range from 5 to 100 mm. Operating experience shows that the average particle size and particle-size distribution (PSD) of feed coal, char and ash influence the pressure drop across the bed and the gas-flow distribution within the bed. These hydrodynamic phenomena are responsible for stable gasifier operation and for the quality and production rate of the syngas. The counter-current operation produces four characteristic zones in the gasifier, namely, drying, de-volatilization, reduction and combustion. The physical properties of the solids (i.e. average particle size, PSD, sphericity and density) are different in each of these zones. Similarly, the chemical composition of the syngas, its properties (temperature, density and viscosity) and superficial velocity vary along the height of the bed. The most popular equation used to estimate the pressure drop in packed beds is that proposed by Ergun. The Ergun equation gives good predictions for non-reacting, isothermal packed beds made of uniformly sized, spherical or nearly spherical particles. In the case of fixed-bed gasifiers, predictions by the Ergun equation based on the average or inlet values of bed and gas flow parameters are unsatisfactory because the bed structure and gas flow vary significantly in the different reaction zones. In this study, the Ergun equation is applied to each reaction zone separately. The total pressure drop across the bed is then calculated as the sum of pressure drops in all zones. It is shown that the total pressure drop obtained this way agrees better with the measured result.     

Drop properties and pressure fluctuations in liquid–liquid–solid fluidized-bed reactors

Characteristics of size, rising velocity and distribution of liquid drops were investigated in an immiscible liquid–liquid–solid fluidized-bed reactor whose diameter was 0.102 and 2.5 m in height. In addition, pressure fluctuations were measured and analyzed by adopting the theory of chaos, to discuss the relation between the properties of liquid drops and the resultant flow behavior of three (liquid–liquid–solid) phase in the reactor. Effects of velocities of dispersed (0–0.04 m s⁻¹) and continuous (0.02–0.14 m s⁻¹) liquid phases and fluidized particle size (1, 2.1, 3 or 6 mm) on the liquid drop properties and pressure fluctuations in the reactor were determined. The resultant flow behavior of liquid drops became more irregular and complicated with increasing the velocity of dispersed or continuous liquid phase, but less complicated with increasing fluidized particle size, in the beds of 1.0 or 2.1 mm glass beads. In the beds of 3.0 or 6.0 mm glass beads, the effects of continuous phase velocity was marginal. The resultant flow behavior of liquid drops was dependent strongly upon the drop size and its distribution. The drop size increased with increasing dispersed phase velocity, but decreased with increasing particle size. The drop size tended to increase with approaching to the center or increasing the height from the distributor. The size and rising velocity of liquid drops and correlation dimension of pressure fluctuations have been well correlated in terms of operating variables.     

Evolution of particle properties during spray drying in relation with stickiness and agglomeration control

Spray drying consists in atomizing a solution into liquid drops in a hot air flow to get dry solid particles after solvent evaporation. The convective drying at the drop surface leads to a very fast evolution of temperature and water content due to initial high differences of temperature and water vapour pressure between the drop surface and the drying air. During drying, the drop surface viscosity is increasing due to potentially amorphous polymers reaching a rubbery state. The drop surface is becoming sticky with consequences on wall deposit. This sticky behaviour which appears in the range of 10 to 30 °C above the glass transition temperature Tg, may be utilized in a positive way for agglomeration of drying particles with dry powders, either recycled fines or new dry powder, to improve instant properties.The evolution of water content of drops along drying, is deduced from measurements of air temperature and relative humidity, at different places in the dryer and used to predict the drying and sticky behaviour of two maltodextrin solutions (DE12 and DE21) with different Tg. The studied parameters in a co-current spray dryer were the inlet air temperature (144, 174, 200 °C) and flow rate (80 and 110 kg h^− 1), the liquid flow rate (1.8, 3.6 and 5.4 kg h^− 1) and the rotation speed of the wheel atomizer. The results on particle water content combined with the evolution of Tg showed that particles are sticky close to the atomiser for the two maltodextrins, and also along the chamber for maltodextrin DE21 due to its lower Tg. The introduction of dry particles at different places in the chamber allowed validating the method to control agglomeration.     

Drying regime maps for particulate coatings

Key microstructural properties of particulate coatings such as porosity and particle order are established during drying. Therefore, understanding the evolution of particulate distributions during drying is useful for designing coating properties. Here, a 1D model is proposed for the particle distribution through the coating thickness at different drying times and conditions, including Brownian diffusion, sedimentation, and evaporation. Effects of particle concentration on diffusion and sedimentation rates are included. Results are condensed onto a drying regime map which predicts the presence of particle surface accumulation or sediment based on two dimensionless numbers: the Peclet number and the sedimentation number. Cryogenic scanning electron microscopy (cryoSEM) is used to image the transient particulate distributions during the drying of a model system comprised of monodisperse silica particles in water. Particle size and evaporation rates are altered to access various domains of the drying map. There is good agreement between cryoSEM observations and model predictions. © 2010 American Institute of Chemical Engineers AIChE J, 2010     

Retracted: Effects of the Operating Conditions and Geometry Parameter on the Filtration Performance of the Fibrous Filter

The gas‐solid two‐phase flows in fibrous filters were simulated by computational fluid dynamics (CFD) technology. The pressure drops and filter efficiencies with different operating conditions and geometry parameter, including face velocity, particle size, and solid volume fraction (SVF) were calculated. The effects of the operating conditions and geometry parameter on the filter performance of the fibrous filter were obtained. The results indicate that the pressure drop increases linearly with the face velocity and the predicted values of the pressure drops are in excellent agreement with the experimental correlation. Filtration efficiency decreases with the face velocity for submicrometer particles (0.1 μm) and, for larger particles (1 μm) the tendency is just the opposite. The filtration mechanism is different for different particle sizes. For the filter in this paper, when the particle size is smaller than 0.2 μm, Brownian diffusion plays a significant role in the filtration process. When the particle size is greater than 0.5 μm, inertial impaction becomes an important capture mechanism. For particle sizes in the range of 0.2–0.5 μm, the Brownian diffusion and inertial impaction are both relatively weak and, therefore, the filtration efficiency has the least value in this range. Additionally, the SVF distribution is an important geometry parameter in the filter. The filtration efficiency of the filter with a decreased SVF (geometry B) along the thickness of the filter is higher than that of the filter with the even SVF (geometry A), while maintaining a low pressure drop.     

Online monitoring of drop/particle size and size distribution in liquid–liquid dispersions and suspension polymerizations by optical reflectance measurements

Evolutions of drop/particle size and size distribution in liquid–liquid dispersions and suspension polymerizations of methyl methacrylate (MMA) were monitored by using an online optical reflectance measurement (ORM), and effects of operating parameters such as the agitation rate, concentration of poly(vinyl alcohol) (PVA) dispersant, and initial concentration of poly(methyl methacrylate) (PMMA) in MMA monomer on the Sauter mean diameter (d₃₂) and size distribution of drop/particle were investigated. According to the variations of d₃₂ of drops/particles with time, four characteristic particle formation stages can be identified for suspension polymerization process. The factors that lead to increase the rate of drop break up, such as increasing of concentration of PVA and decreasing of viscosity of dispersed phase, would postpone the particle growth stage. The d₃₂ and size distribution breadth of drops/particles were significant increased when the liquid–liquid dispersions or suspension polymerizations were conducted at low PVA concentrations or MMA/PMMA solutions with high PMMA contents were used as the dispersed phase, in consistent with the scanning electron micrograph observation on final PMMA particles. It is clear that ORM can be effectively applied in online monitoring of size and size distribution of drops/particles in the liquid–liquid dispersions and suspension polymerizations. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43632.     

Deagglomeration testing of airborne nanoparticle agglomerates: Stability analysis under varied aerodynamic shear and relative humidity conditions

Occupational exposure to nanomaterial aerosols poses potential health risks to workers at nanotechnology workplaces. Understanding the mechanical stability of airborne nanoparticle agglomerates under varied mechanical forces and environmental conditions is important for estimating their emission potential and the released particle size distributions, which in consequence alters their transport and human uptake probability. In this study, two aerosolization and deagglomeration systems were used to investigate the potential for deagglomeration of nanopowder aerosols with different surface hydrophilicity under a range of shear forces and relative humidity conditions. Critical orifices were employed to subject airborne agglomerates to the shear forces induced by a pressure drop. Increasing applied pressure drop was found to be associated with decreased mean particle size and increased particle number concentrations. Rising humidity decreased the deagglomeration tendency as expressed by larger modal particle sizes and lower number concentrations compared to dry conditions. Hydrophilic aerosols exhibited higher sensitivities to changes in humidity than hydrophobic particles. However, the test systems themselves also differed in generated particle number concentrations and size distributions, which in turn altered the responses of created aerosols to humidity changes. The results of the present study clearly demonstrate that (a) humidity control is essential for dustiness and deagglomeration testing, (b) that (industrial) deagglomeration, for example, for preparation of aerosol suspensions, can be manipulated by subjecting airborne particles to external energies, and (c) that the humidity of workplace air may be relevant when assessing occupational exposure to nanomaterial aerosols.

Copyright © 2016 American Association for Aerosol Research     

Some surface tension and contact angle problems in industry

Contact angle, surface tension and wetting properties are of fundamental importance in many industrial processes, e.g. coating of television screens and fluorescent lights. In addition, different stages of many processes may involve immersion cleansing and subsequent drying. We consider two different problems: one being very practical and involving cleansing and drying of silicon substrates in the semiconductor industry, and the other being theoretical whereby the problem of the shape of scssile and pendant drops is addressed with a possible practical application for making contact angle and surface tension measurements. In the case of cleansing of silicon substrates, we model a process whereby dirt particles are removed as a result of the surface tension forces exerted on a particle passing through a water/air interface and give a possible explanation as to why the efficiency of the process is vclocity dependent. For the case of small liquid drops, a new formulation of the governing equation yields solutions for multiple pendant and extended sessile drops.     

Surface Stickiness of Drops of Carbohydrate and Organic Acid Solutions During Convective Drying: Experiments and Modeling

Abstract

Drying kinetics of low molecular weight sugars such as fructose, glucose, sucrose and organic acid such as citric acid and high molecular weight carbohydrate such as maltodextrin (DE 6) were determined experimentally using single drop drying experiments as well as predicted numerically by solving the mass and heat transfer equations. The predicted moisture and temperature histories agreed with the experimental ones within 6% average relative (absolute) error and average difference of ± 1°C, respectively. The stickiness histories of these drops were determined experimentally and predicted numerically based on the glass transition temperature (T _g ) of surface layer. The model predicted the experimental observations with good accuracy. A nonsticky regime for these materials during spray drying is proposed by simulating a drop, initially 120 µm in diameter, in a spray drying environment.     

Surface Composition and Morphology of Particles Dried Individually and by Spray Drying

This study investigates how the morphology of spray-dried particles is related to the formulation and properties of the components in the formulation. Further, the scale effects in comparisons of levitation-dried single particles and spray-dried particles in a lab-scale spray dryer have been addressed. The Drying Kinetics Analyzer^TM generates single particles from a levitated drop under simulated spray-drying conditions. A set of surface-active polymers (bovine serum albumin, hydroxypropyl methyl cellulose, and triblock co-polymer Poloxamer), in combination with lactose, were analyzed for their dynamic surface properties in solution, and their effect on particle morphology and surface composition were determined by low-vacuum SEM and XPS analyses. The morphology obtained in spray drying was reproduced in the single-particle drying. The surface compositions were also similar, but higher levels of surface-active materials were found at the surface of the single particles as compared to the spray-dried particles. Further, the adsorption rate of surface-active compounds at the drop surface estimated by dynamic surface tension was found to be an important parameter to estimate the surface composition at different drying scales. The particle morphology was primarily determined by the surface rheological properties of the feed solution and, to a lesser extent, by the surface composition.     

Identical Feed Drops in a Flow Vessel May not Always Be Desirable

In this paper, the effect of feed size and daughter drop size distributions on the steady‐state drop size distribution in a continuous flow vessel is discussed. For identical sizes of feed drops, a new criterion has been proposed to ensure the complete breakage of the feed drops giving rise to smooth continuous drop size distributions. This has been predicted on the basis of two competing time scales, namely, breakage and residence times.     

Modeling the effect of drop charge on coalescence in turbulent liquid—liquid dispersions

In this work, a mechanistic model of drop coalescence based upon a stochastic film-drainage analysis is developed. The coalescence model accounts for previously considered factors, such as turbulence intensity, drop size, and drop deformability, while additionally describing the dual effects of drop surface potential and system electrolyte concentration. Model results indicate that electrostatic repulsion may strongly inhibit small drop coalescence, as well as coalescence between larger deformable drops. Comparison of model predictions to data from several transient coalescence experiments shows good agreement in most cases.     

Control of particle segregation during drying of ceramic suspension droplets

Ink-jet printing of thick film combinatorial libraries involves the deposition and drying of drops of suspension containing many different powders. During drying, a peripheral ring of powder develops and segregation of the more mobile particles to the remaining liquid pool in the centre leaves behind a drop residue with non-uniform composition. The present work investigates the effectiveness of organic ink additives that contribute a degree of thixotropy to the ink in reducing particle mobility and inhibiting particle segregation.     

Spray Drying of Green Corn Pulp

Maize (Zea mays) is a cereal grown in Brazil, and its availability is limited to the harvest season. An alternative processing route is based on the production of green corn powder, which has a longer shelf-life and increased versatility. This study aimed to evaluate the influence of drying conditions on the physical characteristics, size, and morphology of green corn powder. Drying experiments were performed on a spray dryer according to a central composite rotational design to evaluate inlet air temperature, feed flow rate, and pulp concentration. The yield of dried pulp corn had an average value of 36.19%. The following mean values for the physical properties of the powder were measured: solubility of 94.37 g/100 g, wettability of 128.05 seconds, moisture content of 1.97%, water activity of 0.13, density of 0.79 g/mL, and a particle diameter of 31.02 µm. The powder was also yellow with less intensity, and the particle surface was smooth at higher temperatures and had a tendency to form agglomerates. The estimated optimal conditions for spray drying were 48% (w/w) pulp concentration, 172°C inlet air temperature, and feed flow rate of 0.56 L/h.     

High speed imaging of drop formation from low viscosity liquids and polymer melts in spinning disk atomization

An investigation of drop formation in a recently developed spinning disk atomization (SDA) technique is presented. In‐situ observations of drop formation at the disk rim, using a high speed imaging installation, are made. Atomizations covering two orders of magnitude in flow rate show that ligaments can also form at low flow rates. Sequences of pictures indicate that drops undergo a rotary motion as they detach from a ligament. In the direct drop regime, oscillating motions dominate. The effect of teeth shape at the disk rim on the resulting drops is compared. The effect on drop size and size distribution is found to decrease with increasing rotation rate and corresponding images are studied. Experiments with liquid viscosities ranging from 1 to 120 mPas reveal a fundamental difference in drop breakup, but a negligible change in drop size. Likewise, only a small effect of liquid density is detected. The surface tension's influence on the liquid spreading at the disk rim is described and the subsequent drop formation is qualitatively analyzed.     

Contact of a spherical particle with a droplet

The collection of particles by liquid drops is profoundly influenced by the contact angle of the particles with the drops and the surface tension of the drops. The present investigation was undertaken to establish an equation with reference to the force which acts on a particle by surface tension after contact of a particle with a drop, and to simplify its solution. Moreover, the approximate equations obtained can be applied as regards the arbitrary contact angle of a particle with a drop and the arbitrary ratio of the radius of the drop to the particle. The agreement between theoretical and experimental values could be verified by this experiment.It is considered from these results that the approximate equations can be utilized when it is necessary to know the behaviour of a particle after contact with a liquid drop.