Dispersive mixing of immiscible liquids and gases using rotor-stator devices and membranes

Dispersing of gases or immiscible liquids within another continuous liquid fluid phase
is a standard operation for the processing of multiphase systems in the industrial
areas like food, cosmetics pharmaceuticals and fine chemicals. The commonly used
dispersing tools are rotor-stator devices with tooth-/pin geometries arranged in
circular, concentric or axial, stacked disc configurations. Depending on the gap width
between the rotor-stator pins or tooth elements and the viscosity function of the twophase
system, laminar, turbulent or transitional flow conditions act in the dispersive
mixing procedure. – A new generation of dispersing devices are the static or dynamic
membrane devices in which the disperse drops or bubbles are formed once and
detached from the membrane surface by cross- or co-flowing fluid streams. This
procedure means significantly reduced mechanical treatment of the multiphase fluid
system and allows to tailor narrow disperse size distributions.
Rotor-Stator Dispersing Processes
Our recent work concerning Rotor-Stator (R/S) dispersing process developments
has mainly focused on laminar to transition domain flow conditions. We have
investigated bubble and drop break-up in some detail under steady and transient
shear or elongation as well as mixed flow conditions. Different types of R/S (model)
flow apparatus were applied comprising concentric  /eccentric  cylinder-, four
roller- , single-  and multi-toothed  geometries. From respective experiments
expanded maps of critical bubble-/drop break-up characteristics (critical Weber
(WeC) or critical Capillary (CaC) numbers as a function of viscosity ratio
λ, deformation rate G, total deformation D and flow type α have been derived.
Figure 1 exemplarily demonstrates CaC(α) for drop break-up under pure shear (α =
0), equibiaxial (α = -1), or planar (α = 1) elongation as well as for mixtures of these
flow types. Steady and transient drop break-up were investigated experimentally (a),
by numerical flow simulation using CFD (b) and by a non- equilibrium
thermodynamics modeling approach (c) /1-3/. Consistent results from these three
approaches (a-c) were received for surfactant free as well as for surfactant covered
drop interfaces.

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Fig.1: Critical Ca- number for different flows

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Fig.2: Surfactant distribution at drop
interface in shear flow

For surfactant covered drop interfaces a criterion to distinguish between diffusion
and convection driven interfacial coverage with surfactant molecules was defined as
the ratio of Peclet number (Pe) / Capillary number (Ca), denoted as α and
implemented into a convection diffusion equation which forms the bases for
respective CFD calculations. As a result of these calculations surfactant
concentration distributions along the interfacial contour of drops deformed in shear,
elongation and mixed flows were received and satisfying comparability with
experimental drop deformation data was found. Figure 2 shows such calculated
concentration distributions of surfactant at the deformed drop interface for different
Capillary numbers and a viscosity ratio λ of 4.
The impact of transient shear and elongation flows has been investigated within an
eccentric cylinder gap and transferred to a complex multi toothed rotor-stator
dispersing geometry. CFD based simulations applying a particle tracking procedure
along distinct particle flow tracks allowed us to quantify the transient drop
deformation history of selected drops along their paths through the dispersing
apparatus. Comparisons with respective experimental results demonstrated again
good agreement as demonstrated in Figure 3.

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Fig. 3: left: Transient deformation and Ca-number; right: multi-toothed R/S geometry
Membrane / Micro-channel Dispersing Processes
In addition to rotor-stator flow devices we considered also channel / nozzle / pore
flows with respect to their dispersive mixing performance. New microfluidics devices
have been developed in our Laboratory at ETH Zürich in close collaboration with the
University of Queensland in Brisbane (Australia); Prof. J. Cooper-White. Within the
lasts two years we investigated drop formation in co-flow and cross-flow micro- and
macro channels. By means of micro particle imaging the velocimetry (Micro-PIV) we
accessed velocity fields around respective drops and used this information for
optimizing the dispersing channel flow geometries and to derive scale up criteria
(e.g. We = f (Re) characteristics) over several orders of magnitude like demonstrated
in figure 4 .
As a scaleable solution with application relevance, derived from micro channel cross
flow results, a Rotating Membrane Device (ROME) with Controlled Pore Distance
(CPD) was developed. The cross flow is generated by the rotational motion of a
membrane cylinder within a surrounding concentric housing through which the
continuous fluid phase is axially pumped. The disperse fluid or gas-phase enters

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Fig 4: Micro-/macro channel co-flow dispersing; experimental data / M. Duxenneuner
through a hollow shaft into the rotating cylinder membrane body and forms disperse
liquid droplets or bubbles at the membrane surface, from which the cross flowing
continuous fluid phase flow detaches them as soon as a critical shear stress is
exceeded .

Quantifying Mixing: The Exposure Dimension

Mixing, or Segregation, can be defined using three dimensions. The instantaneous state of segregation has two dimensions:
the scale of segregation, and the intensity of segregation. The intensity of segregation is reported as the CoV in a blending
application, while the scale of segregation is reported as the striation thickness distribution, the drop size distribution, as
examples. Previous work has shown that the two dimensions contain different and independent information. The CoV tells
us nothing about the scale of segregation, and the scale of segregation contains no information about the range of
concentrations observed.
The exposure dimension conbines the intensity and scale of segregation with a third characteristic of the system to give a rate
of reduction in segregation. Many examples of exposure equations are given in the literature. The most familiar is the mass
transfer rate, where the scale of segregation can be related to the interfacial area, the intensity of segregation to the local
concentration gradients, and the tendency of the system to reduce segregation to the mass transfer coefficient, or the
molecular diffusivity. In this case, the exposure dimension is an integral combination of the local area and intensity of
segregation, so while it is correlated to both the scale and the intensity of segregation, it is not a linear combination of the
average measures.
In this talk, the exposure dimension will be reviewed in the context of existing literature and models. The goal is to
determine the underlying mixing variables which consistently drive a reduction in segregation, and the role that these
variables play in achieving a range of process objectives

EMULSIFICATION USING A SMX SULZER STATIC MIXER IN TURBULENT FLOW FOR A MICROENCAPSULATION PROCESS

Microencapsulation is a widespread technology that has many applications, like the protection and controlledrelease
of active ingredients in the medical and cosmetics industries, or the fabrication of fragranced fabrics in the
textile industry.
This work focuses on the emulsification step of an interfacial polymerization microencapsulation process. Firstly,
an emulsion is prepared that comprises a population of droplets. This dispersed phase contains a monomer. In a
second step, another monomer, which is soluble in the continuous phase, is added to the system to begin the
reaction at the interface of droplets.
In industry, microencapsulation by interfacial polymerization is usually performed in stirred-tank reactors, where
both the emulsification and encapsulation steps are carried out. But this process is very costly in energy due to
the power input necessary for the generation of a fine dispersion, as well as the time needed to get the right drop
size distribution. Moreover, the characteristics of the final product, such as the particle size distribution with
respect to the target size, and the membrane thickness and structure, are not necessarily well controlled. These
characteristics are strongly dependant on the hydrodynamic conditions of the different steps. In particular, it is
crucial to control the drop size of the emulsion in order to control the microcapsule size distribution resulting from
this process.
In this study, the emulsification process is carried out using Sulzer SMX mixers. Such mixers are usually
employed for the dispersion of viscous liquids in the laminar flow regime. However, it is demonstrated in this study
that they are also well adapted for liquid-liquid dispersion in turbulent flow.
The influence of the dispersed phase concentration, the flow velocity and the number of mixing elements on the
drop size distribution under various turbulent flow conditions is investigated. The drop size distribution is
characterized in terms of the mean surface-volume drop diameter and standard deviation, which are measured
with a laser diffraction device. The emulsions are cyclohexane-in-water stabilised with Tween 80, which are the
same fluids involved in the system chosen for the encapsulation process.
A correlation of the Sauter mean diameter with the Weber number and the Reynolds number is proposed for the
flow rate range studied and compared with the correlation given by Streiff (1977) for SMV Sulzer mixers at low
energy input.
The dispersion process in turbulent flow is governed by the ratio of the stress forces outside the drop to the
surface forces at the interface of the drop. The external stress forces are the turbulent drag forces on the drop
surface created by local velocity differences, which are promoted by turbulent eddies. In this case, the smallest
drop size corresponds to the microscale of turbulence and the size can be correlated with the specific energy
dissipation in the mixer. The specific energy can be determined from flowrate and pressure drop through the static
mixer.
Since the correlations available to calculate the pressure drop in SMX mixers are valid for single phase Newtonian
fluid flow, the pressure drop of the liquid-liquid flow is measured in this study and used to calculate the specific
energy dissipation. A correlation of the maximum drop diameter with specific energy dissipation is proposed and
compared with that given by Hinze (1955) for isotropic turbulent flow.
Finally, the minimum number of mixer elements required to obtain a stable drop diameter is given for different
hydrodynamic conditions and dispersed phase concentrations.
The work carried out has enabled the emulsification conditions in the static mixer to be optimized, which should
allow the encapsulation process to be performed in the best conditions. Moreover, the SMX static mixers show
good performance for emulsification in turbulent flow in terms of droplet size and energy consumption compared
with the conventional stirred-tank reactor.

Session

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