Continuous emulsion polymerization of styrene in a single Couette–Taylor vortex flow reactor

The effect of the geometrical and operational parameters on the mixing characteristics of a Couette–Taylor vortex flow reactor (CTVFR) were investigated and were correlated with the same parameters by using the tank‐in‐series model. Continuous emulsion polymerization of styrene was conducted at 50°C in a CTVFR to clarify the effects on kinetic behavior and reactor performance of operational parameters such as rotational speed of inner cylinder (Taylor number), reactor mean residence time, and emulsifier and initiator concentrations in the feed streams. It was found that steady‐state monomer conversion and particle number could be freely varied only by varying the Taylor number. In order to explain the observed kinetic behavior of this polymerization system, a mathematical model was developed by combining the empirical correlation of the mixing characteristics of a CTVFR and a previously proposed kinetic model for the continuous emulsion polymerization of styrene in continuous stirred tank reactors connected in series (CSTRs). On the basis of these experimental results, it was concluded that a CTVFR is suitable for the first reactor (prereactor) of a continuous emulsion polymerization reactor system. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 1931–1942, 2001     

W/O/W Multiple Emulsions as the Functional Component of Dairy Products

Water‐in‐oil‐in‐water (w/o/w) multiple emulsions are considered that could be suitable components of functional dairy products. Such emulsions enable the preparation of low‐calorie products, encapsulation of bioactive components or microorganisms, and their protection during digestion. Because of the large phase interface, w/o/w emulsions are thermodynamically unstable. Therefore, their preparation and stabilization requires specific conditions. This review describes a potential industrial application of w/o/w emulsions in dairy products in detail and summarizes the value, preparation, stabilization, and evaluation of w/o/w emulsions in a dairy system.     

Mechanical Entrainment in W/O/W Emulsion Liquid Membrane

Abstract

An experimental study of mechanical entrainment in W/O/W emulsions is conducted. W/O/W emulsions are stirred for various stirring times under the conditions that mechanical entrainment solely occurs, and changes in volume of the W/O emulsions and size distribution of the internal water droplets are measured. The rate of change in number of the water droplets entrained is found to be proportional to the volume fraction of W/O emulsions. Based on this result, a new model for mechanical entrainment is developed. The calculated change in W/O emulsion volume with time agrees with the observed ones except in the region near phase inversion. Then, phase inversion is discussed.     

Operating Regimes and Hydrodynamics of a Rotating‐Disc Contactor

The operating regimes for a pilot‐scale rotating‐disc contactor (RDC) were investigated by a computational fluid dynamics/population balance model (CFD‐PBM) simulation. The model successfully predicted the critical rotor speed, which divided the entire operating range into two regions. In the low rotor speed region, the input energy was insufficient to break droplets, resulting in an almost constant droplet diameter. Therefore, the increasing revolution slightly affected the interfacial area, while the axial mixing became severe. In contrast, the interfacial area increased significantly in the high rotor speed region because of the increased breakage rate. Moreover, the axial mixing extent increased slightly because the dispersed‐phase accumulation enhanced the advection effect. The results indicate that the CFD‐PBM approach can be applied to engineering practice for extractors.     

W_1/O/W_2乳液油相薄化速率的影响因素

用乳粒发生器制备约2 mm的大直径W1/O/W2乳粒,研究了油相中Span80和水相中CaCl2对油膜薄化的影响,同时也研究了外相水用氟苯(FB)溶剂饱和后对双重乳粒体系油膜薄化的影响。结果表明:Span80和CaCl2的浓度越大,油相的薄化速率越大;外相水中FB的加入将降低乳液体系油相的薄化速率。     

Three‐Dimensional CFD Simulation of Stratified Two‐Fluid Taylor‐Couette Flow

Two‐fluid Taylor‐Couette flow, with either one or both of the co‐axial cylinders rotating, has potential advantages over the conventional process equipment in chemical and bio‐process industries. This flow has been investigated using three‐dimensional CFD simulations. The occurrence of radial stratification, the subsequent onset of centrifugal instability in each phase, the cell formation and the dependency on various parameters have been analyzed and discussed. The criteria for the stratification, Taylor cell formation in each phase have been established. It can be stated that the analysis of single‐phase flow acts as the base state for the understanding of radial stratification of the two‐fluid flows. The extent of interface deformation also has been discussed. A complete energy balance has been established and a very good agreement was found between dissipation rate by CFD predictions and the energy input rate through the cylinder/s rotation.     

Numerical Simulation of Sterilization Processes for Shear‐Thinning Food in Taylor‐Couette Flow Systems

The performance of the Taylor‐Couette flow apparatus as a heat sterilizer is numerically investigated. The destruction of Clostridium botulinum and thiamine (vitamin B1) was selected as model reaction. When Taylor vortices were formed in the annular space, the heat transfer significantly enhanced as compared to the case without vortex flow. As a result, the equivalent lethality calculated from the temperature field increased, which is regarded as a quantum leap. Conversely, the improvement of heat transfer induced destruction of thiamine. These results suggest that there is a trade‐off relationship between the enhancement of heat transfer and the avoidance of thermal destruction of nutritional components. In conclusion, the Taylor‐Couette flow sterilizer has the potential for process intensification in heat sterilization processes.     

Modeling of Slug Velocity and Pressure Drop in Gas‐Liquid‐Liquid Slug Flow

Gas‐liquid‐liquid slug flow in a capillary reactor is a promising new concept that allows one to incorporate gas‐liquid reaction, liquid‐liquid extraction, and facile catalyst separation in a single unit. In order to assess the performance of a gas‐liquid‐liquid slug flow reactor, it is necessary to predict the slug velocity and pressure drop to ascertain residence times and reaction rates. New empirical models for velocity and pressure drop were developed based on existing models for two‐phase gas‐liquid and liquid‐liquid slug flows, and these were validated experimentally.     

Effect of Rotor Disc Diameter on Holdup,Axial Dispersion and Droplet Size in a Taylor‐Couette Disc Contactor

Application of liquid‐liquid extraction is on a steady rise. Although there are considerable designs of extraction devices, equipment design and optimization is still on the research agenda. Utilization in the biorefinery industry or metallurgy requires robust technologies and equipment. The simple design and stable operation performance of the Taylor‐Couette disc contactor suffices the technical needs for these harsh operation conditions. The effect of different rotor disc diameter on the dispersed phase holdup, axial dispersion, and droplet size was investigated. It was shown that with smaller rotor disc diameter stable operation is still feasible but higher axial backmixing has to be expected.     

Pipeline Flow Behavior of Water‐in‐Oil Emulsions with and without a Polymeric Additive in the Aqueous Phase

New experimental results are presented on the pipeline flow behavior of water‐in‐oil (W/O) emulsions with and without a polymeric additive in the aqueous phase. The emulsions were prepared from three different oils of different viscosities (2.5 mPa s for EDM‐244, 6 mPa s for EDM‐Monarch, and 5.4 mPa s for Shell Pella, at 25 °C). The W/O emulsions prepared from EDM‐244 and EDM‐Monarch oils (without any polymeric additive in the dispersed aqueous phase) exhibited drag reduction behavior in turbulent flow. The turbulent friction factor data of the emulsions fell well below the Blasius equation. The W/O emulsions prepared from EDM‐244 oil exhibited stronger drag reduction as compared with the EDM‐Monarch oil. The W/O emulsions prepared from Shell Pella oil exhibited negligible drag reduction in turbulent flow and their friction factor data followed the Blasius equation. The Shell Pella emulsions were more stable than the EDM‐244 and EDM‐Monarch emulsions. When left unstirred, the EDM‐244 and EDM‐Monarch emulsions quickly coalesced into separate oil and water phases whereas the Shell Pella emulsions took a significantly longer time to phase separate. The Shell Pella oil emulsions were also milkier than the EDM emulsions. The addition of a polymer to the dispersed aqueous phase of the W/O emulsions had a significant effect on the turbulent drag reduction behavior.     

Determination of the interfacial area and mass transfer coefficients in the Taylor gas–liquid flow in a microchannel

The interfacial area in the Taylor (slug) gas–liquid flow in a microchannel was measured by the Danckwerts' (chemical) method, using CO₂ absorption from the CO₂/N₂ mixture into KHCO₃/K₂CO₃ buffer solutions, containing NaOCl as a catalyst. The rate of absorption was determined and the Danckwerts' plots were constructed. Reasonable agreement with the geometrical area measured photographically was obtained. This fact allowed to determine for the first time the mass transfer coefficients separately for liquid film and liquid caps. A correlation for the calculation of mass transfer coefficients has been proposed.     

Theoretical and Experimental Studies on Acetylene Absorption in a Polytetrafluoroethylene Hollow‐Fiber Membrane Contactor

The separation of acetylene from a gas mixture was investigated using a polytetrafluoroethylene hollow‐fiber membrane contactor and 1‐methyl‐2‐pyrrolidinone as absorbent. The effects of the gas velocity, the liquid velocity, the feed gas concentration, and the module length on the acetylene mass transfer were investigated. The results showed that the acetylene mass transfer flux increased with increasing liquid velocity, gas velocity, and feed gas concentration, but decreased with increasing membrane module length. A mathematical model was used to predict the wetting extent of the membrane and the mass transfer resistance in the acetylene mass transfer process. The wetting extent of the membrane was found to increase with increasing liquid velocity and to be effectively restrained with increasing gas velocity. The liquid phase resistance and the wetted‐membrane phase resistance controlled the acetylene mass transfer in the acetylene absorption process. The acetylene absorption efficiency was maintained at 90 % for 114 h of the C₂H₂ membrane absorption–thermal desorption cycle process.     

Influence of Surfactant on the Characteristics of W1/O/W2-Microparticles

The water-in-oil-in water (W₁/O/W₂) double emulsion evaporation technique is widely used when the microencapsulation of soluble agents like naloxone HCl is intended. The present work shows the effect of HLB emulsifiers added to phase O on microsphere morphology, size, release, drug encapsulation efficiency. The addition of sorbitan ester to first emulsion (W₁/O) and the HLB of the surfactant have an important effect on the characteristics of poly-lactide-co-glycolide (PLGA) microparticles (MP). This MP with sorbitan esters added were smaller and released the hydrophilic drug, naloxone, with no-significant difference at pH 5 versus pH 7.5 (phosphate medium). This is an important fact when long-drug release is considered since it is known that PLGA degradation leads to media acidification. The HLB value had an important effect on drug loading. Sorbitan monooleate led to the highest naloxone loading. Because of its low HLB (4.3), it is most suitable for stabilizing the W₁/O emulsion, which is fundamental for the successful entrapment of a hydrophilic compound in MP prepared by double emulsion technique. Finally, drug solubility in the MP matrixes cannot be considered as a predictive parameter for drug encapsulation. Both surfactants increased the naloxone solubility in the polymer PLGA and only sorbitan monooleate increased the drug entrapment.     

Flow Regimes of Viscous Immiscible Liquids in T‐Type Microchannels

A computational and experimental study of the flow regimes of a mixture of castor and paraffin oils in a T‐type microchannel with 200 × 400 µm cross section was carried out. The ranges of parallel, slug, droplet, and rivulet flow regimes of the tested mixture were defined. According to the experimental results, a flow regime map was constructed for this mixture depending on the Weber number multiplied by the Ohnesorge number. A correlation of the length of paraffin oil slugs to the fluid flow ratio was established. The experimental data were compared with results of numerical simulation. A good agreement between calculation and experimental data was achieved in terms of reproduction of flow regimes, phase boundaries, and slug length.     

Preparation of microcapsules of W/O/W emulsions containing a polysaccharide in the outer aqueous phase by spray‐drying

A water‐in‐oil‐in‐water (W/O/W) multiple emulsion containing a hydrophilic substance, 1,3,6,8‐pyrenetetrasulfonic acid tetrasodium salt (PTSA), and a wall material in its inner and outer aqueous phases, respectively, was prepared by a two‐step emulsification using a rotor/stator homogenizer, and was further homogenized with a high‐pressure homogenizer. Maltodextrin or gum arabic were used as wall materials, and olive oil was used as the oily phase. The high encapsulation efficiency for PTSA (>0.9) was realized. The emulsion was spray‐dried to produce microcapsules of W/O/W type. The efficiencies of the microcapsules prepared with maltodextrin and gum arabic were 0.82 and 0.67, respectively. Stability of the microcapsules was examined at 37 °C and 12%, 33% and 75% relative humidity. Microcapsules prepared with maltodextrin were more stable than those prepared with gum arabic.     

Taylor流下微细颗粒增强CO2:吸收研究（英文）

The physical absorption of CO2 in water containing different types of particles was studied in a microchannel operated under Taylor flow.The maximum enhancement factors of 1.43 2.15 were measured for activated carbon (AcC) particles.The analysis shows that the enhancement effect can be attributed to the shuttle mechanism.Considering the separate contributions of mass transfer from bubble cap and liquid film,a heterogeneous enhancement model is developed.According to this model,the enhancement factors E Cap,E Film and E Ov are mainly determined by mass transfer coefficient KL (KL,Cap and KL,Film),adsorptive capacity of particles m,and coverage fraction of particles at gas-liquid interface ζ.With both effects of particle-to-interface adhesion and apparent viscosity included,the model predicts the enhancement effect of AcC particles reasonably well.     

CFD approaches for the simulation of hydrodynamics and heat transfer in Taylor flow

Previous studies on heat and mass transfer in the Taylor flow regime in microchannels have shown the transport (heat/mass) rates to be dependent on the length of the liquid slug. In order to understand the effect of slug length on transport rates and to have a one-to-one comparison with experimental data, a computational approach is required to simulate flows with liquid slugs and bubbles of controlled lengths.Here we describe and benchmark two approaches. The first, and conceptually simplest, is to generate bubbles and slugs in a long tube using a time-dependent boundary condition. In the second method, the flow and heat transfer in a single unit cell, consisting of a bubble surrounded by liquid slugs, is solved in a frame of reference moving with the bubble velocity. Both methods were implemented in ANSYS-Fluent.Simulations for a two-phase (liquid-only) Reynolds number of 713, Capillary number of 0.004 and void fraction of 0.366 for nitrogen-water flow were performed to compare the two techniques. There was a very large difference between the required computational mesh sizes and times for the two methods, with a wall clock time of 38 h on a single processor for the moving domain compared with 1460 h using four processors for the stationary domain approach. In addition, for a constant wall heat flux boundary condition, even with 14 bubbles present in a long tube thermal development was not achieved. The hydrodynamic and heat transfer results obtained from the two approaches were found to be very similar to each other and with results from our earlier verification and validation studies, giving a high degree of confidence in the implementation of both methods.     

Factors affecting droplet size of sodium caseinate‐stabilized O/W emulsions containing β‐carotene

This work was initiated to prepare an oil‐in‐water (O/W) emulsion containing β‐carotene by microfluidization. The β‐carotene was dissolved in triolein and microfluidized with an aqueous phase containing sodium caseinate (SC) as the emulsifier. Microfluization at 140 MPa resulted in O/W emulsions with a mean droplet diameter of ca. 120 nm, which was further confirmed by transmission electron microscopy analysis. The influences of SC concentration and microfluidization parameters on the droplet size of the emulsions were studied. The results showed that the mean droplet diameter decreased significantly (p <0.05) from 310 to 93 nm with the increase in SC concentration from 0.1 to 2 wt‐%. However, a further increase in SC concentration did not much change the droplet diameter, although the polydispersity of the emulsions was slightly improved. The droplet diameter of the emulsions was found to decrease from 200 to 120 nm with increasing microfluidization pressure, with narrower droplet size distribution. The storage study showed that the emulsions were physically stable for about 2 weeks at 4 °C in the dark. The results provide a better understanding of the performance of SC in stabilizing the O/W emulsions.     

Preparation of W1/O/W2 emulsions and droplet size distribution measurements by pulsed‐field gradient nuclear magnetic resonance (PFG‐NMR) technique

Multiple emulsions of W₁/O/W₂ type are of major interest in life sciences, offering possibilities for the encapsulation of water‐soluble active agents. In food science, they are also applied for fat reduction. The droplet size distributions of the inner and outer emulsions are of main importance as they influence the rheological and sensorial properties, the release kinetics, as well as the structural and microbial stability. However, the determination of the inner and outer droplet size distributions is a major challenge, as conventional measurement techniques cannot be applied. Pulsed‐field gradient nuclear magnetic resonance (PFG‐NMR) is well known as a non‐destructive tool for droplet size determination, especially in simple emulsions. In this work, double emulsions of the W₁/O/W₂ type were prepared with polyglycerol‐polyricinoleate (PGPR) and polyoxyethylen‐20‐sorbitan monolaurate (Tween 20) as emulsifiers by means of rotor‐stator emulsification machines. PFG‐NMR was applied for measurements of the inner phase (W₁) droplet size distribution as well as for the characterization of the O phase. The W₁ values were compared with results from laser light diffraction of simple emulsions (W₁/O type) and were found to be consistent within the experimental errors, if restricted diffusion in the outer water phase (W₂) and additional effects are considered.