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060- Batch mixing of fluids and particles

Liquid blending

Dr Gül Özcan-Taşkın
Professor Chris D Rielly
• Check CSTR geometries-Pip Jones
• HIM for blending with jets

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Liquid Blending - Lecture outline
➢ Introduction
➢ Mixing mechanisms in fluid flows
➢ Experimental techniques
➢ Blending regimes
➢ Mixing time correlations
➢ Blending high viscosity liquids
➢ Blending non-Newtonian liquids
➢ Blending liquids of different physical properties
➢ CSTRs
➢ Blending with a liquid jet

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Blending applications
❖ Homogenisation/ to reduce concentration and temperature gradients
• Adjusting viscosity, pH, temperature
❖ To promote reaction (polymerisation, acid-base reactions)
❖ Minimum degree of liquid motion to prevent stratification in storage tanks:
• De-stratification

❖ All parts of the tank are blended


❖ Blending rate is adequate
❖ Appropriate equipment is selected
Industrial needs for liquid blending
❖ Comparative performance of agitator types
❖ Scale-up
❖ Non-Newtonian fluids
❖ Non-standard geometries
❖ Multiphase systems
❖ High viscosity liquids or dispersions
❖ Fluids with different viscosity/density
Single phase flow regimes
❖ In stirred vessels, the flow regime depends on
N is the impeller speed (s-1)
rND 2
Re  D is the impeller diameter (m)
m r is the density (kg/m3)
m is the viscosity (Pa s)

Re  10 10  Re  10 4 Re  10 4
laminar transitional turbulent
❖ Mixing occurs by
• extension, shear and rotation
• molecular diffusion
• turbulent dispersion

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MECHANISMS OF MIXING

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Mechanisms of mixing
❖Laminar conditions

• Laminar shear flows


• Rotational shear flows
• Extensional flows

❖ Thinning layers, elongating threads and flattening of lumps or


agglomerates
• Molecular diffusion: slower than under turbulent conditions
Laminar mixing mechanisms
Velocity variation in
Shear deformation Increasing time of deformation
simple shear flow

u(y)

L 
L
y . du
  Striation thickness decreases
x dy Interfacial area increases

❖ High velocity close to the impeller reduce concentration differences


❖ very thin laminae mix by molecular diffusion

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Laminar mixing mechanisms
Rotational
shear tracer
flows

start after 2 3/4 turns


Laminar mixing mechanisms
Extensional deformation
Converging streamlines
Volume is conserved decreasing thickness
increasing width
y

x
vx

Elongational flow
.
Elongational rate of strain =  = vx
x

❖ Stretching + folding  mixing


❖ very thin laminae mix by molecular diffusion

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Fluid mixing mechanisms
❖ General requirements:
• convective flow and no stagnant regions
❖ Laminar mixing
• low Reynolds number, viscous dominated flows
• inertial effects quickly damped by viscosity
• impeller blades must sweep through whole mixture volume
• large velocity gradients exist close to these blades, producing stretching and folding of
fluid elements
• molecular diffusion produces final smearing of concentration gradients, but is only
effective at small scales or long times
• in liquids, in 10 s a species diffuses a distance of
x ~ Dt  10 9  10  10 4 m

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Distributive mixing
Distributive mixing by repeated cutting and twisting operations
Relevant to static mixers
twist twist

cut
cut
cut

twist

first operation second operation

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Distributive mixing
Distributive mixing by repeated
cutting and twisting operations Slice

Slice
Twist

Twist

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Laminar mixing
dye
addition
pvp solution

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Mechanisms of mixing
❖Turbulent conditions

• Long range convective flow (bulk flow, bulk diffusion or bulk dispersion)
• Local turbulent diffusion (eddy diffusion or eddy dispersion) : energy transfer
from large groups of molecules (primary eddies) to smaller ones
• Molecular diffusion: caused by relative motion of molecules  homogeneity
at molecular scale
Homogenisation
Liquid blending to form a uniform mixture is a common process operation, which
conceptually takes place in two parts
❖ Macro-mixing
• process which reduces large scale concentration gradients by convection
• usually the rate-limiting step (see below)
❖ Micro-mixing
• final approach to molecular homogeneity brought about by mixing in
Kolmogorov scale eddies and molecular diffusion
   
1/ 4
• typically,  ~ 1 W/kg, so lK   / 
3
  10 6
1/ 4 3
/ 1  30  10 6 m
 

t micro ~ l k / D  30  10
2

6 2 9
/ 10  1 s

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Turbulent flow parameters
❖ Integral length scale of turbulence (energy containing eddies)
  w / 2  D / 10
❖ Kolmogorov length scale (dissipative scales)

lK   3 /  
1/ 4
w = blade width
D = impeller diameter
P
❖ mean dissipation rate  
rV
P = power input
V = liquid volume
u = velocity fluctuation

❖ turbulence kinetic energy k 


1 2
2
u   v 2  w 2 

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The energy spectrum
energy cascade
impeller size smallest eddies

Energy spectrum
anisotropic universal equilibrium range
largest
eddies
locally isotropic
smallest
eddies
log E()

energy inertial subrange


containing viscous
eddies dissipative
subrange

1 / le log 
eddy wave number,  / 2 = l-11 / lK

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Turbulent flows
❖ Turbulence is characterised by
• chaotic, three dimensional velocity fields
• random variations in space and time
• dissipation of mechanical energy to heat
• wide range of eddy sizes
• increased rates of momentum, heat and mass transport
❖ Turbulent diffusion is very important
• in liquids, in 10 s a species diffuses a distance of
x ~ Dt t  10 3 10  10 1 m
• since now the turbulent diffusivity is several orders of magnitude larger

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Turbulent dye
addition
mixing

water

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Laminar
mixing dye
addition

pvp solution

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TECHNIQUES TO
DETERMINE MIXING TIME

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Definitions
❖ Mixing time (, s): time taken to reach an arbitrary state of mixedness from an
arbitrary state of unmixedness.
Probe output

❖ Quantitative methods: time taken from


the release of a tracer until the
amplitude of the output signal is within a
set limit of the final reading;

❖ Visual methods: time for the


disappearance of the last traces of
gradients.
time time
Determination of macro-mixing times
Physical methods
• tracer test: passive scalar (dye or salt) is added to the
flow
• detector: light absorption / conductivity / visual / PLIF
• 95% mixing time, 95, is time for concentration
fluctuations to decay to within ± 5% of the final mean
concentration

Chemical methods
• reactive tracer is added which changes colour
following chemical reaction

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Mixing time
Measurement
Techniques
Mixing times using max/min deviation from the mean
1.4

C*, Dimensionless Concentration


95% Mixing Time
1.2
+ 5%
 95
1.0
– 5%
0.8

0.6
C t   C0
0.4 C* 
C  C0

C * t  0  0
0.2

and C * t   1 as t  
0.0
0.95  C  1.05 for all t  95
*
0 10 20 30 40 50
Time

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Measurements with multiple probes

Under turbulent blending conditions mixing time values from probes in different positions are the same.
Under transitional and laminar conditions, different results are obtained from probes close to the
impeller and away.

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Dimensionless
mixing time
Mixing times using s
From simultaneous probe measurements, 95% mixedness corresponds to C*t= 0.95
logs 2  log(Ct*  1)2

-2.6

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Experimental Techniques
When mixing time is measured using a quantitative method (with a probe), its
value for a given degree of mixedness can be determined as follows:

C  s c2
M
C

M is the mixedness index


C is the difference between initial and final concentration
sc2 is the mean square concentration fluctuations
Experimental Techniques (2)
➢ If mixing time to reach 95% mixedness, i.e. M=0.95 is determined,
mixing times for different end-point criteria can be calculated as
follows:
 n 
ln 1.0  
n
 
100 
 95 ln 1.0  0.95

 99 ln 1.0  0.99 
➢ Thus, for example   1.54
 95 ln 1.0  0.95
BLENDING REGIMES

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Dimensionless mixing time in different flow regimes
Close
clearance
impellers Open impellers
mixing time (Nθ)
Dimensionless

Laminar
blending
regime
Turbulent blending regime

Transitional
blending regime

Remin Recrit Reynolds number


Fourier number
Hoogendoorn and den Hartog (1967) defined a “vessel Reynolds number”
which is also called the Fourier number (1), Fo:
 m 
 Fo  1.5 0.5 
 rT H 
For H=T this becomes
 m 
 Fo  
 rT2 
(1) Handbook of Industrial Mixing (Paul et al, 2003)

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Blending regimes
Close
clearance Open impellers
impellers
Dimensionless mixing

1/Fo=1239 or Po1/3 Re<6440:


threshold value between
time (Nθ)

turbulent and transitional


blending regimes

Reynolds number

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MIXING TIME CORRELATIONS

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Turbulent Mixing Time Correlation
Po 3 Re Fo  5.2  10%
1

Rearranged equation:
2
D
Po 3 N95 1.5 0.5  5.2  10%
1
For H=T
T H
2
D
Po 3 N 95    5.2  10%
1

T 
Turbulent Mixing Time Correlation
Rearranged equation:

5.2 T 1.5H 0.5 5.2 T 2.0


 95   95  1 / 3 2
Po1 / 3ND2 Po ND

or for H=T
1 1
 1   T  3 233
     T
  D
P 2 N 
 
l i qui dma s s m
Mixing time correlation for turbulent blending regime
1 1
 rV   T  3
2
3 3
     T
 P   D

➢  can be reduced by increasing P/m or D


➢  is independent of μ in the turbulent regime
➢ scale up on constant power per unit mass: mixing time increases
➢ We also know that N is constant in the turbulent regime
Mixing Time Correlation for Transitional Blending Regime (1)

1832 T 2 m
 95  2 / 3 2 4  31.1%
Po N D r
Rearranged:
Po 3 Re Fo 2  183  31.1%
1 1

2 2
r  m 
2
 V   
T 3  3
      T 3
 P  D  r 
(1) Handbook of Industrial Mixing (Paul et al, 2003)
Transitional blending correlation (Po1/3 Re< 6440)
2 2
 rV   T   m  3
2
3 3
      T
 P  D r

➢  can be reduced by increasing P/m or D


➢ θ depends on μ in the transitional blending regime
➢  decreases as the scale of operation increases
➢ We also know that N  Re-1 in the transitional blending regime
➢ Multiple impellers recommended particularly in “tall” vessels where H > T.
Design considerations
Tips for design and scale up
– In geometrically similar systems at constant P/V:
 in the turbulent regime
 in the transitional regime
when scale is increased.
keeping  constant in turbulent regime can require a very high P
when scaled up.
Design considerations
Tips for design and scale up

Calculations for a second scale can be based on the


knowledge of N at another scale

• Constant over the turbulent regime


• Proportional to Re-1 in the transitional regime.
BLENDING LIQUIDS OF HIGH VISCOSITY
❖ Blending of high viscosity liquids  laminar regime

N  Rea ….. a>>1 for open impellers


N = constant for close clearance impellers

❖ Close clearance impellers such as anchors, helical ribbons or


helical screws recommended
Blending high viscosity liquids
Turbine
8 3 9 1
(baffled)
107 2
P 2
75 2
Turbine
(unbaffled)
D 3 mL
7 3 PBT
106 1
6 4 4
PBT in draft-
5 tube
5 Screw
P 752
 constant Screw in
105 D 3 mL 6
draft-tube
3 7 Ribbon

rLD 2 8
Propeller +
draft-tube
104 -3
10 10-2 10-1 100 101 102  75 m L 9 Anchor
(Hoogendoorn & den Hartog, 1967)

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BLENDING LIQUIDS OF HIGH VISCOSITY
Practical design implications

• Draught tubes can allow open impellers to be used


• Anchor impellers may not provide sufficient top-to-bottom
mixing
• Helical ribbons and helical screws commonly used to
provide good bulk blending and heat transfer.
• Helical screw impellers fitted in a draft tube can also provide
good axial mixing
RHEOLOGY- REMINDER

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Flow curves of Newtonian and non-Newtonian fluids
BLENDING
NON-NEWTONIAN LIQUIDS

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Pseudoplastic liquids
Often we will handle shear-thinning liquids: apparent viscosity decreases with increasing shear rate

m0
100 Shear-thinning region

lower Newtonian
Viscosity, ma / Pa s

upper Newtonian
10-1
power-law
region

region
10-2
m

10-3 Shear rate, s-1


10-2 10-1 100 101 102 103 104 105
.
 -1

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Blending shear thinning liquids
• In a stirred bulk, there is a spectrum of shear
rates.
• In Newtonian liquids the viscosity is independent
of the shear rate.
• In shear thinning liquids, this results in higher
viscosities away from the impeller(s) where shear
rates are lower.
• Regions to mix last are close to walls and base
where viscosity is highest μw

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Blending Shear thinning Liquids
❖ Need for estimating the shear rate at the vessel wall where blending takes
place last

❖ Practical recommendation:
• low Po impellers (hydrofoils) to operate in the turbulent flow regime
• turbines that generate high shear (low viscosity) in the transitional flow
regime.
Estimating wall shear by torque balance
The use of a torque balance for an agitator in a stirred tank is
discussed in Bird et al. “Transport Phenomena”
Surface integral Baffles

 v  
  m  R  dS   pbaff dGbaff
S 
r w A

Torque Radius x tangential velocity gradient


Apparent viscosity (shear rate)
Wall shear stress
❖ The integral of the surface shear stress (walls + base) plus the baffle
force must balance the shaft torque
❖ Assuming uniform wall shear rate and shear stress
• Flawed for single impellers in turbulent regime; much better for
multiple impellers at lower Re
❖ Valid when n > 0.5 and Rewall > 200
❖ A simplified expression to estimate the shear stress at the wall has
been proposed as follows (1): 1 Λ
τw 
(1)
Handbook of Industrial Mixing (Paul et al, 2003) 1.622 T 3

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Mixing time for shear thinning liquids
Mixing time correlation for Newtonian liquids can be applied for shear thinning
liquids using τw
1 
w 
1.622 T 3
where .n
w  K  W

and . n 1
mw  K  W

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Blending shear thinning liquids
❖ Need for estimating the shear rate at the vessel wall where blending takes
place last

❖ Practical recommendation:
• low Po impellers (hydrofoils) to operate in the turbulent flow regime
• turbines that generate high shear (low viscosity) in the transitional flow
regime.
Flow curves of Newtonian and non-Newtonian fluids
Blending non-Newtonian liquids
❖ Yield stress liquids (plastic or viscoplastic liquids):

• Well mixed zones, caverns, around the impeller with little liquid motion
away from the impeller. Blend time for the whole of the vessel contents
cannot be defined.

• Practical recommendation: Large D/T, dual impellers and high impeller


speeds to increase the cavern diameter.
Blending liquids with a yield stress
 1.36  PrLN D 
3
 Dc 
2 2
❖ Cavern formation: no flow outside impeller region     2 
D    y 

N (rps)
50
42
33
Dc
27
D/T
20 0.6
0.5 (Nienow & Elson, 1988)
17
13
8 0.25
0.33

(a) D/T = 0.5 (b) N = 8 rps

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Normal stress phenomena

• Weissenberg effect (rod climbing)


• normal stress differences are
manifest as hoop stresses
• can climb into seals and gearboxes

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Normal stress phenomena
• Weissenberg effect (rod climbing)
• normal stress differences manifest
as hoop stresses
• can climb into seals and gearboxes

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Blending viscoelastic liquids
Viscoelastic liquids:
  much longer than in Newtonian liquids of similar consistency at a
given P/V.
 Complex interaction of elastically driven flows with inertially driven
flows.
 Other properties, such as shear-thinning behaviour also affect the
flow fields. Detailed knowledge of the rheological properties
required to choose the optimum impeller geometry for a given
scale.
BLENDING LIQUIDS OF
DIFFERENT PHYSICAL
PROPERTIES

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BLENDING LIQUIDS OF DIFFERENT DENSITY AND VISCOSITY

❖ Small differences in physical properties of the added and bulk liquids


  can be approximated to that for liquids of similar properties.

❖ Large differences in ρ and/or μ  extremely long 


BLENDING LIQUIDS OF DIFFERENT DENSITY AND VISCOSITY (2)

Two operational regimes

1. Stirrer controlled regime.

2. Added liquid controlled regime. Added liquid mixes slowly, sticking


to vessel internals. Mixing time depends on physical properties,
impeller type, N and addition method.
BLENDING LIQUIDS OF DIFFERENT DENSITY AND VISCOSITY (3)

Density differences:
Richardson number (Ri)

r g l a
Ri 
rN 2 D 2

La: ratio of volume to surface area of added stream


BLENDING LIQUIDS OF DIFFERENT DENSITY AND VISCOSITY (4)

Viscosity differences:
Modified Reynolds number
r N D 2 mb
Re *  
mb ma
Effect of viscosity difference on Nϑ
10000

Dimensionless mixing time [-]


1000

100

Jones and Őzcan-


10
0.001 0.01 0.1 1 10 100 Taşkın, 2003
Added liquid viscosity [Pa s]
45 rpm 60 rpm 85 rpm 120 rpm 180 rpm 240 rpm

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Blending liquids with r & m
10000

0.001Pa s

1000 0.5 Pa s
N[]

2.9 Pa s

100 10 Pa s

Prediction for

Similar µ liquids
10
1000 10000 100000 1000000

Re (-)
c
Recommendations
❖ Avoid stratification where possible
❖ Blending of stratified layers can be improved by operating the impeller
such that it pumps towards the “interface”
❖ If possible, operate in the stirrer controlled regime to minimise mixing
time.
Re*>102 and/or Ri<5x10-2 correspond to the stirrer controlled
regime.
Recommendations
❖ If this is not possible, the following are recommended
Additions as a stream  minimise the risk of the added liquid being drawn
into zones of low circulation and will provide an initial deformation
• High N
• Additions in the impeller suction rather than discharge  will promote the
deformation of the added liquid before reaching regions of high shear and
turbulence.
• If the added liquid is less dense, the addition should be close to the impeller
to prevent it from rising to the surface.
Effect of pumping mode- viscous addition
Hydrofoil, D=T/2, 326 rpm, addition above impeller PD, addtn
in impeller suction
PU, addtn in impeller discharge

Jones, P. PhD thesis, KCL

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Effect of pumping mode- viscous addition
Hydrofoil, D=T/3, 633 rpm, addition above impeller PD,
addtn in impeller suction

PU, addtn in impeller discharge

Jones, P. PhD thesis, KCL

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CSTR

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Example CSTR Geometries

“Z” “X”
“(REVERSE) T”

Initial dip pipe set-up Alternative dip pipe set-up


CSTRs
• Potential disadvantages

– Poor design can result in short circuiting, wasting reactants, and


higher downstream processing efforts/costs
– Control can be more complex than for a batch system - adapting
to variations in inlet feed rate and concentration can be complex
– For some processes (e.g. pharmaceuticals), batch systems are
preferred for traceability
– Small product runs favour batch mixing
Results from experiments and CFD
– Impeller Dominated

– Jet Dominated
CSTR Studies - Streamline Visualisation

N = 30 rpm, Q = 0.32 l/s


CSTR Studies - Streamline visualisation

N = 300 rpm, Q = 0.32 l/s


Time (s) 0 0.4 0.8
Time (s) 1.2 1.6 2.0
Scale-up of CSTR’s
• Keeping / constant on scale-up can give similar results at
different scales for geometrically similar systems
• However, this gives unrealistically high power inputs at large
scale:
– Vessels are larger to increase productivity while keeping τ constant
– If  and / are kept constant, then =constant and N is constant on
scale-up
Scale-up of CSTR’s
– Power = Po ρ N3D5
– Torque = Power/(2 π N)
– Power per unit volume  N3D2

Mixing Impeller Power input Torque Power/volume


time speed

5 5 2
Constant Constant T T T
Scale-up of CSTRs
• Scale-up with /=constant leads to excessive power and
torque requirements on scale-up
– Small scale processes may be over-designed. Small scale testing
must check operating conditions that give inadequate mixing
– Large scale processes may not perform adequately
– Changes in system geometry may minimise the impact of imperfect
mixing.
BLENDING WITH A LIQUID JET

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BLENDING WITH JETS
• Jets commonly used in large storage tanks in order to
avoid stratification.
• Advantages over mechanical agitation :

– Low capital cost. A pump unit often cheaper than an agitator


drive and may already exist. No need for the tank to be
reinforced to support the gear box, shaft and impellers.
– Safe, easy maintenance with hazardous liquids, where the pump
is outside the tank and only rotating seal is on the shaft.
BLENDING WITH A LIQUID JET
• A number of correlations in literature to calculate the mixing time.
• The correlation proposed by Fossett and Prosser (1949) was found to
correlate well mixing time (θ) with the vessel diameter (T), nozzle
diameter (d) and jet velocity (U) :

𝑇2
θ∝
𝑈𝑑
BLENDING WITH A LIQUID JET
•The dimensionless mixing time (U/d) is independent of Re in the
turbulent flow regime. Therefore, when re-arranged:

U
2
d 
   ct
d T 
Liquid Blending - Lecture outline
✓ Introduction
✓ Mixing mechanisms in fluid flows
✓ Experimental techniques
✓ Blending regimes
✓ Mixing time correlations
✓ Blending high viscosity liquids
✓ Blending non-Newtonian liquids
✓ Blending liquids of different physical properties
➢ CSTRs
➢ Blending with a liquid jet

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