Application of Visimix To The Characterization of Lab Reactors
Application of Visimix To The Characterization of Lab Reactors
Solid/Liquid
Liquid/Liquid
– Blending Tcirculation(sec)
– Heat Transfer UA (W/oK)
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Unfortunately the process rates do not change uniformly with volume and equipment
size! It is best to scale-up with one key mixing variable.
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rm2technologies LLC Blending macro-mixing
Macro-mixing describes the uniformity of composition and
temperature on the reactor scale 6 2 Liter Lab Reactor, T =10 cm;
(Top-Bottom), OC
Heater Marine Propeller, D =6.9 cm;
Temp. Top Fluid m =985 cp, r =1.25 gm/cc
Reactor T,
Temp.
Bottom Hot Temperature Zone 4
Procedure 300 rpm
agitation off Re = 30
400 rpm
heater on 2 Re = 40
heater off 500 rpm
agitator on Re = 50
record temperature 0
0.0 0.5 1.0 1.5 2.0 2.5
– T(top) - T(bottom) Time, minutes
1
N = 300 rpm,
kmix = 0.63 1/min
T/Tmax
kmix = 1.6 1/min
0.1
mix 1 N = 500 rpm,
N kmix = 2.6 1/min
M ixing can be correlated with
N mix kmix = -2.303* Slope
0.01
0.0 0.5 1.0 1.5 2.0 2.5 3.0
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Time, minutes
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(Top-Bottom), OC
Fluid m =985 cp, r =1.25 gm/cc
Mettler-Toledo
Reactor T,
V =1.2 liters
4
RC1 MP10 300 rpm
Re = 30
Local concentration
3
index 0.2 achieve 90%
l/min VisiMix
to 1 uniformity
simulation for
2
rpm VisiMix lab VisiMix 500 rpm
300 4.2 0.29 220 146
400 5.7 0.31 86 92
1
500 7.4 0.34 53 64 0 50 100 150
Time, seconds
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Temperature at top ( C)
Liquid:1380 ml water
seconds 17.9 Impeller: PBT, D = 45 mm
o
VisiMix (Composition) = 2 Height impeller: 51 mm, C/T = 0.5
Agitation rate: 300 rpm
seconds 17.8 Tank diameter: T=103mm, D/T=0.437
Liquid height: Z=166 mm; Z/T = 1.61
Measured mixing rate constant :
17.7 k = 0.13 s-1 or 7.8 min -1
Estimate based on kmix = 8 min -1
impeller pumping
17.6
Qp N Q ND 3 VisiMix
17.5
kmix 1/Tcirc.= 20 min-1
Vreactor Vreactor
0.6 300rpm 4.5 cm
3 17.4
kmix 0 5 10 15 20 25 30 35 40 45 50 55 60
1440 cm 3 Time (s)
1
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mix 7 11 min
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rm2technologies LLC Heat transfer
Cooling curves for glycerol in a stirred tank reactor
100
90 Reactor temperature at
How long 80 impeller rotation rate, rpm
will it take 100 175 300 Jacket Temp.
temperature, oC 70
to cool the 60
reactor 50
contents to 40
20oC? 30
20
10
time to reach 20oC 192 min. 242 min. 316 min.
0
0 50 100 150 200 250 300 350 400
time, minutes
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W/K
U heat transfer coefficient, W
m2 K 600 0.6
A heat transfer area contacted 400 0.4
by the reaction mass, m 2
200 0.2
Treactor temp. of the reaction mass, K
0 0.0
T jacket ( average ) average temp. of the
10 20 30 40 50 60 70 80 90 100
coolant in the reactor jacket, K
reactor temperature, oC
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Heat transfer 3
characteristics of RC1
Log [Nu/(Pr0.33)]
MP10 is similar to 2
large scale reactors
1
m fluid
0.14
Nu C Pr Re
1 2
3 3
Slope = 0.69
mwall 0
m fluid Cp fluid -1
Pr Prandtl Number 0 1 2 3 4 5 6
k fluid
ρ fluid ND 2 Log (Re)
Re Reynolds Number
μ fluid
h fluid TTank Diameter
Nu Nusselt Number
k fluid
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rm2technologies LLC Mechanical power input
One way to characterize agitation intensity uses universal
power curves to describe impeller performance
1000 Np1/Re rND 2
Re
Anchor Agitator m
300
Inertial Force
Np=constant
Power Number
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10
r N 3D5
NP
P
r ND 2
Re 1
m 1 10 100 1000 10000
Re
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10
10 100 1000 10000
Re
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1.0
0.8
0.6
0.4
0.2
0.0
heater 0 200 400 600 800 1000 1200 1400 1600 1800
hollow
rpm
4.4 1200
4.3
1000
H2 (gas) H2 (liquid) 4.2
pressure (barg)
4.1 800
rpm
rpm 600
3.9
“rate constant” “driving force” 3.8 400
increases w/ agitation increases w/ 3.7
intensity & H2 flow pressure 3.6
200
3.5 0
-20 -10 0 10 20 30 40
time (s)
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1 1200
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agitation
Calculations of gas
1000
agitation (rpm)
800
P/Pmax
from batch absorption 0.1 600
pressure
400
V
PM PF G
model w/ kLa
1 200
C H 2 , sat = 0.077s -1
VL RT 0.01 0
-5 0 5 10 15 20 25
P PF PM PE time (s)
ln k L a t 0.90
PM PF PF PE
400 ml MeOH
0.80 600 ml MeOH
0.70 800 ml MeOH
k L a Mass transfer coefficien t
0.60
P Pressure as a function of time;
kLa (s-1)
0.50
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Summary of differences
in model
approximations for
VisiMix at 1400 rpm
measured kLa =0.42 s-1
@4.6 W/kg
Blade width, mm 4.4 (flat blade turbine 10 (actual width of
adjusted to match impeller)
measured power)
kLa, s-1 0.33 (exp. = 0.42) 0.87
vortex depth, cm 2.1 (exp. vortex ~2.5 cm) 3.6
average energy dissipation, W/kg 4.6 9.5
gas hold-up 3.5% 5.5%
Sauter mean bubble, mm 1.8 1.4
circulation rate, liters/s 1.7 2.4
micro-mixing time, s 0.14 0.088
circulation time, s 0.64 0.46
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Conductivity milli-mhos
1.8
Conductivity standard
when any solid particle spends less
than 1 second on the bottom of the 3.5
deviation x 100
1.6
reactor. 3.0
1.4 2.5
Bottom view Average conductivity
Cond. std. dev.x100 2.0
of reactor 1.2
1.5
1.0
electrodes 1.0
0.8 0.5
baffles 0.6 0.0
0
200
400
600
800
1000
1200
1400
1600
1800
2000
Rotation (rpm)
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g r
0.45
S 0.1 d p X 0.13
0.2
r
N js
D 0.85
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30%
25%
20% Series2
15% Series1
Series3
10%
5%
2mm PVC spheres
0%
1000
0
200
400
600
800
1200
1400
1600
1800
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rotation rate, rpm
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Visualizing reaction regimes in a turbulent low viscosity
system for a fast reaction
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mechanism
Viscosity
Rule-of-Thumb
Feed Number
Feed Scale-up
tube of feed
rate variable to
location points
keep constant
P/V or
Micro Yes No Yes No
N3D5/V
Meso Yes Yes No Yes nN4D3/Qfeed
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Semi-batch addition of I2
solution added to S4062-
and starch.
10%
VisiMix prediction of 4%
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(rate constant estimated) time, seconds
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Correlation of macro-mixing time with the reaction time for the iodine-
thiosulfate reaction system.
10
The reaction time trxn(s) = 0.11 t95 (s)1.1
for the
R2 = 0.88
iodine/starch black
color to disappear,
trxn(s), is measured
trxn(s)
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Contact information
Reinaldo “Ray” Machado
phone: (484) 553-3612
E-mail: info@rm2tech.com
Website: www.rm2tech.com
Ray is the instructor of short course
“Fundamentals of Scale-up”, which may be offered at your site.
Reinaldo (Ray) Machado is the developer and instructor of a popular industrial short course, “Fundamentals of
Scale-up” which he teaches part time. He is currently employed by Air Products and Chemicals, Inc. in
Allentown, Pa. in 1986 and serves as a senior consultant specializing in reaction engineering. Previously, he
managed hydrogenation and oxidation applications development for the Catalytic Reaction Solutions Group
and served as group leader for the Reaction Engineering Technology area. Ray has broad technical
experience in applied reactor engineering, scale-up of chemical reaction processes, mass transfer, heat
transfer, applied reaction calorimetry, hydrogenation, electrochemical engineering, sulfonation, amination,
propoxylation, polymerization, and plastics recycling.
Ray received a Ph.D. in chemical engineering with a concentration in chemistry from the University of
Wisconsin, Madison, and a B.A. in chemistry and mathematics from Frostburg State College. He has served
as a part-time instructor of a short course, “Scale-Up Considerations in Chemical Processes,” at Lehigh
University and currently teaches industrial courses on the fundamentals of scale-up. He holds 16 patents, has
collaborated on 15 publications, and is a member of the American Institute of Chemical Engineers and the
American Chemical Society.
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Thank you for your time
and gracious attention