Influence of process parameters on microcapsules loaded with n-hexadecane prepared by in situ polymerization

A series of melamine–formaldehyde microcapsules containing n-hexadecane were synthesized by in situ polymerization from partial etherified melamine–formaldehyde resins. This research was conducted to clarify the influence of different parameters on the encapsulation process, i.e. during the emulsion formation step and during the shell formation using surface tension measurement, Fourier-transform infrared spectroscopy and differential scanning calorimetry. By carefully analyzing the influencing factors including phase volume ratio, types of surfactants and content, stirring rate and time, pH, reaction time, feeding weight ratio of core/shell pre-polymer, the optimum synthetic conditions were found out. The results indicated that a binary mixture of Tween-20 and Brij-35 was found suitable emulsifier at low pH. Furthermore, formaldehyde/melamine (F/M) mole ratio influenced not only the shell formation mechanism but also the particle size distribution, microcapsule morphology and resin conversion rate.     

Particle nucleation and growth in seeded semibatch miniemulsion polymerization of hybrid CeO2/acrylic latexes

CeO₂/acrylic hybrid coatings with high solids content and with nanoparticle percentages up to 5 wt% have been successfully synthesized by seeded semibatch miniemulsion polymerization process. The droplet nucleation efficiency has been assessed by Capillary Hydrodynamic Chromatography and TEM analysis. The effect of the stability of the miniemulsion, the type of initiator and the number of particles of the seed on the efficiency of the nucleation of the nanodroplets fed has been investigated. It was found that the less stable the hybrid miniemulsion, the higher the diffusion of the monomer out of the droplets and hence, the seed latex particles grew in size. However, the CeO₂ nanoparticles did not diffuse out with the monomer and remained in very small droplets that eventually nucleate leading to a bimodal population. When stable miniemulsions were produced by using a polymer as hydrophobe, droplet size increased reducing the number of particles in the seed and monomer diffusion was minimized enhancing nucleation of droplets with larger sizes that produced broad PSDs. Coalescence of droplets was negligible because the size distribution of the nanoceria particles did not change from the seed particles to the final latex. The UV–Vis absorption capacity of the films prepared with increasing the amount of CeO₂ increased, but scattering effects were observed at high loading of CeO₂ due to the large size of the CeO₂ aggregates.     

CHARACTERISTICS OF MICROMETER AND SUBMICROMETER SIZE O/W EMULSIONS PRODUCED BY RAMOND SUPERMIXER®

A novel motionless mixer named the Ramond Supermixer® (RSM®) was employed to produce O/W emulsions composed of micrometer and submicrometer-size droplets. Liquid paraffin as dispersed phase, aqueous sucrose solution as continuous phase, and anionic sodium dodecyl sulfate as emulsifying agent were used as the model emulsification system. Pressure drop, droplet size distribution, Sauter mean diameter (d₃₂), and geometric standard deviation of the droplet size distribution (σ_g) were investigated under the various combinations of process variables; superficial liquid velocity, number of mixing units, number of passages through RSM®, dispersed phase viscosity (η_d), continuous phase viscosity (η_c), and dispersed phase volume fraction. Different modes of droplet size variations with process variables were obtained, with respect to micrometer- and submicrometer-size ranges, and theoretical explanations are forwarded. For the micrometer-size range, maximum droplet diameter (d_max) was proportional to d₃₂. For the submicrometer-size range, d_max varied with d₃₂ in the range of 1.53-2.19-fold, and a correlation is proposed with K (=η_d/η_c); d₃₂ and σ_g were well correlated with the process variables. Furthermore, a semi-empirical mechanistic model was developed for the formation of droplets obtained under inertial sub-range to interpret the effect of process variables.     

PRODUCTION OF SUB-MICROMETER SIZE O/W EMULSIONS USING A HIGH-PRESSURE WET-TYPE JET MILL

Emulsions composed of sub-micrometer size droplets were obtained by a high-pressure wet-type jet mill. Liquid paraffin as dispersed phase, aqueous sucrose solution as continuous phase, and anionic sodium dodecyl sulfate as emulsifying agent were used as the model emulsification system. Droplet size distribution, Sauter mean diameter (d₃₂), geometric standard deviation of the droplet size distribution (σ_g), and emulsion viscosity (η_e) were investigated under the various combinations of process variables: dispersed phase volume fraction (Φ), dispersed phase viscosity (η_d), continuous phase viscosity (η_c), processing pressure, and number of passages through the wet-type jet mil. d₃₂ and σ_g were correlated with the process variables. For the entire experimental range, maximum droplet diameter was varied with d₃₂ in the range of 1.7-1.9-fold, and a correlation was proposed with K (=η_d/η_c) as a variable. Above a marginal value of d₃₂, at Φ ≥ 0.1, emulsions exhibited Newtonian behavior and could be described well by the Yaron and Gal-Or model. Below the marginal values, emulsions strongly depended on d₃₂ and exhibited a shear-thinning behavior. The relation between η_e and d₃₂ for such emulsions was modeled by use of particle Reynolds number.     

Effect of Ultrasonication on Droplet Size in Biodiesel Mixtures

Biodiesel fuels have become more attractive recently because of their environmental benefits and cost competitiveness compared to diesel fuel. Many processing improvements have been proposed to increase the conversion rates and the yields of vegetable oil in order to lower production costs and improve biodiesel product quality. In conventional biodiesel production chemistries, alkaline transesterifications of alcohol/oil dispersions should occur primarily near the interface. Ultrasonic mixing has already been shown to increase overall conversion rates for alcohol/vegetable oil mixtures. Our data show that ultrasonic mixing produced smaller droplet sizes than conventional agitation, leading to more interfacial area for the reaction to occur. Droplet size distributions have been measured for conventional impeller and ultrasonic mixing systems using methanol/soybean oil as a model system. The dispersions were stabilized by surfactant in order to obtain droplet size distribution for mixture samples. Ultrasonic mixing produced dispersions with average droplet sizes 42% smaller than those generated using standard impellers.     

Relationship between deposition properties and operating parameters for droplet onto surface in the atomization impinging spray

Spray coating is one of the most important applications in the industry. The deposition properties of droplet onto surface can be determined by Weber number and K number. While the relationship between the Weber number, the K number and the operating conditions is not understood. In this paper, a comprehensive numerical model based on the Navier-Stokes equation and the particle tracking method was used to simulate numerically the effervescent atomization spray with an impinging surface, and an analytical model was used to predict the droplet velocity. After performing extensive computations at different operating conditions, the formulae of droplet diameter and droplet velocity were obtained with curve fitting technique. The results calculated from the formulae agree with the experimental data. Finally the new formulae relating the Weber number and the K number to the operating parameters were deduced out. The new formulae can be conveniently used to judge the deposition property of droplet onto surface.     

PFG‐NMR on W1/O/W2‐emulsions: Evidence for molecular exchange between water phases

A major question in the investigation of multiple emulsions of WOW‐type is that of stability and ripening, which is often reflected in the droplet‐size distribution (DSD). The DSD is an important parameter for judging product properties. Instability in multiple emulsions is often linked to molecular exchange between inner and outer water phases (W₁, W₂), which has to be taken into account. For example, coalescence phenomena and Ostwald ripening affect microscopic and/or macroscopic stability and therefore the multi‐dispersity of an emulsion. This is especially important as the inner compartment can act for encapsulating active agents. NMR investigations on emulsions are mainly based on the analysis of diffusion properties of molecules in the different compartments. For determination of the DSD of the inner and outer droplets, it is crucial to know the physical effects influencing the NMR‐signal. Depending on these effects, the NMR data are analyzed by different models, depending for example on the occurrence and time scale of molecular exchange between the phases. They are shown to yield correct DSDs. Evidence for the effect of diffusion between phases is given by using the phenomenon of driven diffusion, which allows a direct detection of the exchange by NMR. The exchange is confirmed by confocal laser scanning microscopy.     

Influence of liquid binder dispersion on agglomeration in an intensive mixer

In industrial scale mixer granulation, liquid binder is usually sprayed onto the agitated powder bed by means of a nozzle in order to enhance the agglomeration process. The early stage of this process, where granule nuclei are formed and grow, is not well understood. As it is desirable to model the agglomeration state right from the beginning of the process for the purposes of control and modeling, this nucleation step is therefore an important field of interest.To investigate the influence of binder droplet size on the nucleation stage of the agglomeration process, experiments were carried out with lactose and water in an intensive mixer. Water was sprayed in to the mixer with different nozzles to vary the size of the produced droplets. As a comparison, water was also directly poured into the turning mixer. Samples of the produced granules were taken at specific time intervals and analysed for size and water content. As the experiments were focused on examining short granulation times, the first samples were taken after only half of the water was added.Particle size distribution and liquid distribution in the wet granule samples were analyzed. It was found, that the droplet size of the binder liquid has great influence on agglomerate size and binder distribution at short mixing times, with increasing time, the mechanical stresses acting in the mixer becomes more and more dominating in the process. Preliminary comparisons are also carried out with single drop penetration tests in an attempt to correlate drop size to penetration time and also to produced granule size.In conclusion this paper studies the effect of different drop size conditions and subsequent spray flux on the behaviour of the nucleation and the early stages of the agglomeration process. The context of these findings for agglomeration in an intensive mixer is examined.     

Electrostatic destabilization of water-in-crude oil emulsions: Application to a real case and evaluation of the Aibel VIEC technology

In the current study, the Aibel Vessel Internal Electrostatic Coalescer (VIEC) technology was tested for a real case scenario encountered in the production train of a UK oil field. Depressurized samples were collected both upstream and downstream of the first stage separator. The separation performance was discussed with respect to water cut and droplet size distribution of the emulsions, and the effect of chemical treatment. Issues with respect to representative sampling and testing have been discussed. The application of an external AC electrical field has been shown to significantly enhance the separation of the aqueous phase from tight emulsions, both when it was used alone and in combination with a commercial demulsifier. By using the VIEC technology, the time for separation could be reduced from 8 min to 2 min and the overall BS&W in the emulsions was improved from 45% or 60% to a residual water content of 5-20%. Destabilization of a 45% water-in-oil emulsion by electrical and chemical treatment (20/40 ppm) produced oil in the 2-7% BS&W range whereas the corresponding tests without applying an electrostatic field led to a BS&W greater than 25%. The achieved results strongly suggest that the VIEC technology can resolve the stable emulsion bands encountered in the Schiehallion train and add flexibility or increased production rate to the process. The results also suggest the importance of further studies on the destabilization performances achieved by electrostatic means.     

Prediction of droplet size distribution in sprays of prefilming air-blast atomizers

Droplet size distribution is a crucial parameter of atomization process besides droplet mean diameter. In this paper, the finite stochastic breakup model (FSBM) of prefilming air-blast atomization process has been proposed according to the self-similarity of droplet breakup. There are four parameters in FSBM, which are the initial droplet diameter D₀, the maximum stable droplet size D_c, the minimum mass ratio of a sub-droplet to the mother droplet a, and the droplet breakup probability P(D). The simulation results of droplet size distribution with this model agreed well with the experimental results of prefilming air-blast atomizers. With this model, the nonlinear relationship between the mean droplet diameters and droplet size distribution of the air-blast atomization process can be predicted exactly.     

旋流塔板上局部处的液滴粒径分布

建立了双探针法测量液滴粒径分布的新数学模型，并提出其实用的算法。在直径３００ｍｍ塔内，采用双探针法测量系统测定了旋流塔板上局部处液滴的粒径分布及频率密度，结果粒径分布可用上限对数正态分布函数描述，且得出了分布参数与操作条件的关联式。     

旋流压力式喷嘴低压喷淋液滴粒径的实验研究

以自来水为喷淋介质,对旋流压力式喷嘴低压喷淋液滴粒径进行了测试,分析了压力、喷孔直径和喷嘴流量对液滴索特平均直径(d_(SMD))的影响规律,研究了旋流压力式喷嘴液滴尺寸的分布规律。采用跨径(K)和均匀度指数(N)来揭示喷嘴低压喷淋质量。实验结果表明,d_(SMD)较大,超过250μm；d_(SMD)随喷孔直径增大而增大,随压力和喷嘴流量增大而减小；喷淋液滴尺寸分布均匀性较好,K小于0．65,N大于4。实验结果可以为旋流压力式喷嘴设计和改进提供重要的实验依据。     

SiC原料颗粒级配对Si3N4结合SiC复合陶瓷材料的影响

采用SiC粉和Si粉高温氮化反应烧结制备Si3N4结合SiC复合陶瓷材料。研究四种SiC原料粉体(0-1mm、74μm、44μm、和0.5μm)中三种不同粒度不同含量颗粒级配对Si3N4结合SiC复合陶瓷材料的影响。通过X射线衍射仪和扫描电子显微镜对试样的物相和显微结构进行表征,并对试样的耐压强度等力学性能进行测试。结果表明:采用三种SiC较细粉体颗级配且如下组成:74μm的含量为5 wt%,44μm的含量为10 wt%,0.5μm的含量为35 wt%,所制备的Si3N4结合SiC陶瓷材料的基本烧结性能较好,其体积密度为2.43g/cm3,耐压强度为324MPa。     

Impact of material property and operating conditions on mass flux profiles of monodisperse and polydisperse Group B particles in a CFB riser

Experiments directed at understanding local mass flux behavior of Geldart Group B materials in the riser of a gas-solids circulating fluidized bed (CFB) have been carried out. Three monodisperse materials (with differences in particle size and/or material density), two binary mixtures (one with only a particle size difference between the species and the other with only a material density difference), and one continuous particle size distribution (PSD) have been investigated at four operating conditions. Results show that the riser axial position has the greatest influence on mass flux behavior, especially near the top of the riser, where profile shapes consistently have an inverted U-shape or V-shape. The material type (i.e., monodisperse materials of different particle sizes and/or particle densities or different types of polydispersity) and operating conditions effects are secondary but more apparent at the riser bottom. An interesting observation involving binary mixtures is that while the mass flux profiles of the density-difference binary mixture mimics that of one of its (monodisperse) constituent components, the size-difference binary mimics neither of its two monodisperse components.     

Influence of droplet size on the release of atomic sodium from a burning black liquor droplet in a flat flame

The influence of initial droplet size on the release of atomic sodium from black liquor solids (BLS) during each stage of black liquor combustion has been assessed using a planar laser-induced fluorescence (PLIF) technique. Three different initial diameters of black liquor droplets, 1.3, 1.7 and 2.2 mm were burned in a flat flame at equivalence ratios of 0.8, 0.9 and 1.25. The temporal release of the atomic sodium under fuel rich conditions was found to be different from that under fuel-lean conditions, especially during the smelt coalescence stage. For each stage of black liquor combustion, the measured release rate of atomic sodium increases with decreasing d_i. This implies that significant release of atomic sodium could occur during the in-flight combustion of small droplets, which are known to be generated in recovery boilers from either the carryover or the ejecta.     

Effect of operating conditions and design parameters in a continuous powder mixer

An experimental investigation was carried out to study the mixing performance and flow behavior in a continuous powder mixer for a typical pharmaceutical mixture. Blender performance, characterized by the relative standard deviation (RSD) of composition of blend samples taken at the blender discharge and by the variance reduction ratio (VRR) of the blender, was measured as a function of impeller rotation rate, flow rate and blade configuration. The flow behavior in the continuous mixer was characterized using the residence time distribution (RTD) and powder hold-up measurements. To quantify the strain applied to the powder in the blender, the number of blade passes experienced by the powder in the blender was calculated using the residence time measurements. The relationship between different experimental parameters and mean residence time and mean centered variance was examined. The mixing performance was largely dominated by the material properties of the mixture, which had a larger effect than the ingredient flow rate variability contributed by the feeders. Holdup was strongly dependent on impeller rotation rate; as impeller rotation rate increased, holdup (and therefore, residence time) decreased sharply. As a result, intermediate rotation rates showed the best mixing performance. Blade configuration affected performance as well; blade patterns where some of the blades push the powder backwards improved the mixing performance.     

The study of the effect of operating parameters on the PAH formation during the combustion of coconut shell in a fluidised bed

The effect of combustion parameters on the PAH formation from coconut shell combustion in a FBC was investigated. Among the combustion parameters studied which included temperature, excess air, fuel particle size, and fuel moisture content, only excess air proved to have significant influence on the PAH formation. At 750 °C, an increase of excess air from 20 to 80% resulted in a twelfth fold reduction of PAH emission. At high excess air levels, the combustion temperature had small influence on PAH emission level. In addition to above mentioned combustion parameters, the addition of secondary air to the freeboard was investigated. Due to the relatively low temperature, the addition of secondary air resulted in higher PAH emission. A strong correlation between the combustion efficiency and the PAH emission was observed. According to the results, the CO concentration can be employed as an indicator of PAH level in the exhaust gas.     

Experimental investigation and model improvement on the atomization performance of single-hole Y-jet nozzle with high liquid flow rate

Y-jet nozzle, as an efficient multi-hole internal-mixing twin-fluid atomizer, has been widely used for liquid fuel spray in many industrial processes. However, single-hole Y-jet nozzle with high liquid flow rate is indispensable in some confined situations due to a small spray cone angle. In this paper, the atomization performance of single-hole Y-jet nozzles with high liquid mass flow rates ranging from 400 to 1500 kg/h for practical semidry flue gas desulfurization processes was investigated by the laser particle size analyzer, and the effects of spray water pressure, atomizing air pressure and air to liquid mass flow ratio on the liquid mass flow rate and the droplet size distribution were analyzed. Moreover, the secondary atomization model was modified on the basis of previous random atomization model of Y-jet nozzle. The predicted results agreed well with the experimental ones, and the improved atomization model of Y-jet nozzle was well validated to design the nozzle geometry and to predict the droplet size distributions for single-hole Y-jet nozzle with high liquid mass flow rate.     

Effects of emulsifiers on the oxidative stability of soybean oil TAG in emulsions

The effects of two types of commercial emulsifiers, sucrose FA esters and polyglycerol FA esters, on the oxidation of soybean oil TAG-in-water emulsions were studied. Both emulsifiers influenced the oxidative stability of soybean oil TAG in the emulsion, but they had little effect on the oxidation of TAG in bulk phase. When the TAG were dispersed with sucrose esters having the same FA composition, the oxidative stability increased as their hydrophilic-lipophilic balance (HLB) increased. On the other hand, when the HLB was the same, the oxidative stability increased with increasing acyl chain length of the FA esterified on sucrose ester. However, the effect of the polyglycerol ester could not be explained by the relationship with HLB or the acyl composition. When the stability of TAG in emulsion was compared under the same concentrations of TAG, emulsifier, and oxidation inducer, the TAG dispersed with sucrose esters were oxidatively less stable than with polyglycerol esters. Analysis of the emulsion droplet size suggested that the lower oxidative stability of TAG dispersed with sucrose esters was partly due to their relatively smaller droplet sizes.