Scale-up

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 1

 Objective

• Help people understand about basic chemical Engineering principles.

• To provide information on parameters to be captured during Lab observations.

• Application of data captured for scientific scale-up.

• Application of chemical Engineering Principles in Lab for Process Optimization

• To provide standard formats for data capturing purpose.

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 2

 Contents
• Reaction Engineering
• Reaction Kinetics
• Heat transfer
• Mass transfer
• Crystallization
• Filtration
• Drying
• Agitation
• Flow patterns
• Features of mixing equipment
• Types of impellers
• Power calculation
• Mixing
• Scale-up of Agitator design

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 Role of chemical Engineers
• Should work alongside chemists
• Approaches Problem from different perspective
• Understands vital importance of
– Studying kinetics
– Mass balances
– Heat & mass transfer
– Safety

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 Reaction Engineering
and
Reaction Kinetics

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 5

 Reaction Engineering
• Heat of reaction and subsequent free energy gives feasibility of a reaction.
– If Gibbs free energy is negative, reaction is feasible
– If Gibbs free energy is positive, reaction is impossible
– If Gibbs free energy is Zero, reaction is in equilibrium.
– Gibbs free energy is a strong function of temperature.

• How to calculate conversion from Heat of reaction.

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 Reaction Kinetics
• High Activation Energy.

– Reaction is very temperature sensitive

– Reaction is temperature insensitive.

• Any reaction is much more temperature sensitive at a low temperature than at a higher
temperature.

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 Reaction Kinetics - Examples
• Example 1 (Series Reaction)
k1 k2
A R S
dC A 1 ln(k 2 / k1 )
rA    k1C A t max  
dt k log mean (k 2  k1 )
dC R
rR   k1C A  k 2C R C R ,max  k1 
k 2 /( k 2  k1 )
dt   
dC S C AO  k2 
rS   k 2C R
dt
• tmax : Time at which maximum concentration of R occurs.

• CR,max : Maximum concentration of R.

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 8

 Reaction Kinetics

• Example 1 (Series Reaction : Concentration – Time profile )

CAO CS,undesired

CR max
CR, desired
C
CA
t max
t

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 9

 Reaction Kinetics
• Example 2 (Parallel Reactions)
k1 R (Desired product)
A
k2 S (Unwanted product)
dC R a1
rR   k1C A
dt
dC S a2
rS   k 2C A
dt
rR dC R k2 a1 a 2
  CA
rS dC S k1
We wish this ratio to be high as large as possible.

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 10

 Reaction Kinetics
• Example 2 (Parallel Reactions)

1. If a1 > a2, CA can be kept high by

a) Using a batch or plug flow reactor.
b) Maintaining low conversions.
c) Removing inerts from the feed.
d) Increasing the pressure in gas phase systems.
2. If a1 < a2, CA can be kept low by
a) Using mixed flow reactor.
b) Maintaining high conversions
c) Increasing inerts in the feed.
d)Decreasing the pressure in gas-phase systems.
3. If a1 = a2, product distribution is fixed by k2/k1 and can be varied
by
a) changing the temperature level of operation.
b) using a catalyst.

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 11

 Reaction Kinetics
• Example 2 (Parallel Reactions- Contacting Patterns)
1. CA and CB Both High, Add A&B all at one time.
2. CA and CB Both low, Add A&B slowly.
3. CA High CB low, start with A add B slowly.

• Semi-batch - Importance of time

CB C A k t  pA k t / H A
e e
C BO

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 12

 Reaction- Data to be captured from Lab
• Pre-requisites
– Process Flow diagram,Theoretical Material balance based on Process write-up
– MSDS Summary
– Balanced Chemical equation
– Reaction Mechanism
– Theoretical estimation of heat of reaction/Adiabatic temperature rise
– Follow the check-list
• During Lab trials,
– Make observations on the following
• Description of materials handled/produced
• Color & Clarity of Reaction mass handled.
• Homogeneousness or heterogeneity of reaction mass
• Temperature rises / pH changes
• Size of flasks & RPM of agitators
• Volume rise of the reaction mass,Gas evolution if any
– Capture data regarding
• Time Vs Conversion data ? ? ? Optimization of reaction time
• Impurity Profile as a function of time
• Impurity Profile as a function of mole ratio of reagents/Reactants
• Effect of Skin temperature on rate as well as Impurity Profile
• Effect of Agitation on reaction rate/Impurity Profile
• Effect of Heating or Cooling rate / Profile on Reaction.
• Temperature rise Vs Addition rates of reagents
• Thermal stability data of Reaction mass with respect to time taken on Plant scale.
• Material balance
• Develop Rate equation
• Calculate Heat of reaction
• Calculate Adiabatic temperature rise.
• Analytical datas & Chromatographs of typical in-process reaction monitoring

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 Heat transfer

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 Heat Transfer
• Control of temperature with respect to time is one of the most important aspects of
chemical Engineering

• Temperature needs to be controlled

– To ensure selectivity
– To prevent thermal runaways
– Achieved desired quality/purity/polymorphs
– To reproduce results accurately

• Equation’s

– Q= -K dT/dY
– Q is Heat flux
– K is thermal conductivity
– dT/dY is temperature gradient across wall thickness.

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 Factors affecting Heat transfer
• Flow properties of fluid
• Rate of agitation
• Rate of pumping
• Geometry of equipment (jacket,coil etc.,)
• Fluid Properties
• Viscosity
• Density
• Specific heat
• Increase temperature difference
• Surface area
• Material of construction and Geometry of the equipment
• Phase changes (Reflux etc.,)
• Temperature difference

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Factors to control & Improve Heat transfer
• Design of the process
– Carry out reaction at higher temperature
– Use Refluxing solvent
– Carry out reaction in semi batch mode
• Control addition rate of one reagent

– Use more dilute solutions

• Reduces reaction rate
• Reduces heat released per liter
• Reduces viscosity

– Look into the morphology of reaction mass

• Use less viscous solvents
• Alter conditions/mole ratios etc., to avoid extreme changes in reaction mass

• Design of the Reactor

– MOC (Metals- higher thermal conductivity)
– Heat transfer area (Additional coils etc.,)
– Agitation (Type & speed)

• Design of Plant
– Increase temperature difference between coolant and reaction mass
– Increase flow rates of coolant
– Do periodic de-scaling of jacket

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 Effect of scale on heat transfer area

Size (L) Radius (cm) Height (cm) Surface/

Volume
1 6.2 - 0.483
100 28.8 - 0.104
250 35.5 223.5 0.084
2000 58.4 376 0.048

Surface area increases as square of diameter,whereas volume increases “ cube” of

diameter.
Hence,as volume increases,surface to volume ratio decreases and heat transfer
becomes critical

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 Effect of scale on heat loss

Size (KL) Heat loss Time for 1 C fall with Delta T=60
W/Kg hr C (without jacket cooling)
2.5 0.054 21 min
25 0.005 233 min
100 ml 3.68 17 seconds
1 L Dewar 0.018 62 min

Rate of heat loss decreases with the increase in the reactor volume

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 Mass transfer

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 Mass Transfer
• Control of Product distribution/Selectivity is one of the most important aspects of chemical
Engineering
• Important for reactions with more than one-phase
– Solid-Solid
– Gas-Liquid
– Liquid-Liquid (Two immiscible liquids)
– Gas-Solid-Liquid
• Important
– To ensure selectivity
– To minimize the RM consumption
– To reproduce results accurately

• Equation’s

– J= -Kc dC
– J is Molar flux of transferring species
– Kc mass transfer coefficient
– dC is concentration difference between different phases.

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 Factors affecting Mass transfer
• Flow properties of fluid
• Rate of agitation
• Rate of pumping
• Geometry of equipment (jacket,coil etc.,)
• Fluid Properties
• Viscosity
• Density
• Specific heat
• Particle size etc.,
• Surface area
• Material of construction and Geometry of the equipment

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 Mass Transfer

Density
difference Sh  2.0  0.6 Re1/ 2 Sc 1/ 3
kcT 1/ 2 1/ 3
kC DP  D pG    
cm/s
 2.0  0.6    
DV     DV 
DP  Dia of particle
DV  Diffusivit y

Diameter of particle

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 23

 Factors to control & Improve Mass
transfer
• Design of the process
– Understand the side reactions
• Series and Parallel reaction with extended reaction times
• Series and Parallel reaction with varying concentrations.
– Monitor the reaction profile /product distribution at varying times/varying rates of addition in the
Lab and Plant
– Check the PSD and density of solids handled
– Dilute the reagent which is being added in semi batch mode
– Incase of two phase reactions,addition of salt can alter the rate

• Design of the Reactor

– Scale-up based on high P/v ratios
– Scale-up based on interfacial area (m2/m3)
– Agitation (Type & speed,No of blades,sweep,pitch,no of baffles)
– Add the reagent at the point of highest mixing
– Consider multiple point of injections for reagents.

• Design of Plant
– Increase temperature difference between coolant and reaction mass
– Increase flow rates of coolant
– Do periodic de-scaling of jacket

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 Crystallization

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 Factors that effect crystallization
Factors that effect Crystallization
• Degree of Super Saturation.
• Meta Stable Zone Width (MSZW).
• Type of nucleation.
• Type and degree of mixing.
• Impurities.
• Solvents.

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 Factors that effect crystallization
Process variables
• Macro scale
– Super saturation
– Solute concentration.
– Temperature / Cooling ramp.
– Solvent /Additives
– Seeding
– Impurities in the input
• Micro scale (Molecular scale)
– Nucleation rate
– Growth rate
– Growth mechanism
– Yield
• Product specifications
– Particle size & Shape
– Polymorphic form.
– Crystal purity/Impurities.

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 Crystallization

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 Factors affecting crystallization
• Factors that influence MSZW:
– Mixing.
– Seeding.
– degree of super saturation
• As degree of mixing increases the MSZW decreases.
• Presence of solids decrease MSZW.
• As degree of super saturation increases MSZW increases.

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 Crystallization-Data to be captured from
Lab
• Pre-requisites
– Physical properties of solvents used (Viscosity,Flash point,boiling point)
– Physical properties of solids used
– Solubility data of product in the solvents used
– PSD data of product
– Slurry concentration
– Crystallization yield
• During Lab trials,
– Make observations on the following
• Description of product,crystalline/amorphous
• Type of crystallization
• Size of flasks & RPM of agitators
– Capture data regarding
• Material balance
• Effect of Ageing time on yield
• Effect of Cooling Profile/Distillation rate on yield.
• Seeding temperature
• Meta Stable Zone Width determination
• Effect of Impurity in the crude on the yield.
• Calculate Heat of Crystallization.

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 Filtration

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 Filtration
• PERMEABILITY = Volume / (Time x Area)

• TIME OF FILTRATION ~ Thickness 2

• Filtration time with respect to volume

t   c  Rm
  V 
V  2 A P 
2
A P

• Rate in centrifugal filter

 2 (r2 2  r1 2 )
q
2  (mc / A 2  Rm / A)

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 32

 Filtration - Data to be captured in Lab
• Pre-requisites
– Physical properties of solvents used (Viscosity,Flash point,boiling point)
– Physical properties of solids used
– Solubility data of product in the solvents used
– PSD data of product
– Slurry concentration
• During Lab trials,
– Make observations on the following
• Description of product filtered
• Size of Buckner funnel and filtration area
• Filtration medium
– Capture data regarding
• Settling test on the filterability of slurry
• Filtration data ( Volume Vs time data)
• Cake permeability test
• Check whether cake is compressible or incompressible.
• Filtration area of the filter and Pressure drop across the filter
• Effect of Agitation on filtration
• Effect of Cooling profile/distillation rate/Agitation on filtration
• Check whether cake is compressible or incompressible.
• Stability of crystallization mass with respect to time taken for filtration
• Wet ness of cake / LOD / MC
• Effect of type of washing on quantity
• Effect of wash quantity on impurity/color/yield

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 Drying

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 Drying
Drying time
mS  X 1  X C 1 RC 
tT  t C  t f    ln 
A  RC a R2 

DRYING
RATE

X, free moisture kg/kg solid

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 Factors affecting drying rate
• Vapor pressure and relative humidity.
• moisture movement within the solid.
• The influence of temperature on drying rate.
• Air circulation.
• Particle size.

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 Drying – Data to be captured
• Pre-requisites
– Physical properties of solvent to be removed (Viscosity,Flash point,boiling point)
– Physical properties of solid to be dried (Melting Point,Bulk density,Conductivity,MIE etc.,)
– Oxidation Potential of solid
– PSD data of product
• During Lab trials,
– Make observations on the following
• Material Nature / Lump formation / coloration during drying
– Capture data regarding
• Effect of wet material LOD on drying time.
• Drying data ( Time /Weight data at uniform time intervals)
• Flow rate /Velocity of air during drying
• Humidity of air / Wet bulb /dry bulb of air during drying
• Effect of Particle size on drying rate
• Bulk density of dry powder
• PSD data of product
• Solvate formation if any during drying
• Holding time study of wet cake
• Effect of wet cake holding on drying time.
• OVI issues with high boiling solvents if any.
• Vacuum Pump capacity
• Effect of longer drying time on Impurities
• Rationale behind drying temperature & time.

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 Agitation
Agitation Contents
contents
• Agitation
• Flow patterns
• Features of mixing equipment
• Types of impellers
• Power calculation
• Mixing
• Degree of mixing
• Scale-up of Agitator design

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 Agitation –What ? Meaning
– Induces motion of a material in a specified way, usually in a circulatory
pattern inside a equipment

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 Agitation- Why ? Purpose
• Success of many process depends upon effective mixing and
agitation of fluids
• Blending of two miscible liquids
• Dissolving solids in liquids
• Dispersing a gas in a liquid as fine bubbles.
• Suspension of fine solid particle
• Agitation of a fluid to eliminate temperature gradients

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 Flow pattern
• Depends on
– Type of impeller,
– Characteristics of the fluid,
– Size and proportions of tank, baffles and agitator.
– Variations in the velocity components from point to point.

• Velocity of fluid has three components,

– Radial, longitudinal, and rotational or tangential
– Radial component acts in a direction perpendicular to the shaft of the impeller.
– Longitudinal component acts in a direction parallel with the shaft.
– Tangential or rotational component acts in a direction tangent to a circular path around the shaft.
– The radial and longitudinal components are useful and provide the flow necessary for the mixing action.

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 Flow pattern–Vortex formation
• The tangential flow follows a circular path around the shaft, and creates a
vortex at the surface of the liquid
• At high impeller speeds the vortex may be so deep that it reaches the impeller,
and gas from above the liquid is drawn down into the charge
• Vortex can be prevented by
– Off-centered or inclined mounting
– Installing baffles/draft tubes

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 Flow patterns

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 Features of mixing equipment
• Cylindrical vessel with a vertical axis
• Vessel bottom is rounded
• Liquid depth is approximately equal to the diameter of the tank
• An impeller is mounted on an overhung shaft. Shaft is driven
by a motor

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 Features of mixing equipment
1. Vessels : Vertically mounted cylindrical tanks
2. Baffles : Mounted to reduce excessive rotary motion.
– High viscous fluids have high shear stress which is sufficient to reduce rotary motion.
3. Impellers:
– Rotating part which imparts rotary motion.
– The main parts are hub and blades. Hub is attached to impeller with bolts
– Impeller may be one piece or two pieces bolted at the hub
4. Coupling : Connects the impeller shaft to the drive shaft
– Three types of couplings are
• Rigid and flexible flange, Split muff coupling and magnetic couplings
5. Bearings: Located outside the equipment. Ball or Roller
Bearing at the bottom of the shaft reduces vibration

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 Features of mixing equipment
1. Stuffing box: Contains a gland packing or mechanical seal is fixed to a pad welded to the top head of the
vessel.
1. Toxic or flammable materials, when the pressure is abnormal, the shaft should be sealed to prevent overflow
of the material from the equipment
2. Drive for Agitator: Consists of a motor and a belt drive or a gear drive
1. Usually V-Belt drive is preferred due to its simplicity and short distance between motor pulley and shaft
pulley.
2. Spur,Helical,bevel and worm gearing may be used according to conveyance and shaft arrangement
3. In vertical agitator arrangement motor can be placed in a vertical or horizontal position.
4. Agitator rotate at a lesser speed than the motor based on which a single, double or reduction gear is fixed.
5. Vertically mounted motor can be directly coupled to the input shaft on an inline vertical reducer and the
output shaft of the reducer can be directly coupled to the agitator shaft
6. Transisition from horizontal to the vertical position of the agitator shaft have to be made by using worm or
bevel gearing along with a belt drive

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 46

 Impellers
Divided into two classes:
– Axial-flow impellers
generate currents parallel with the axis of impeller
Paddles, Turbine or Propeller’s are used
– Radial-flow impellers
generate currents in a tangential or radial direction.
Anchor or Gate type agitator’s are used
RPM’s will vary with the intensity of agitation required.
• Main types of impellers:
– Propellers
– Paddles
– Turbines (Flat blade, Pitched blade, Disc)
– Anchors (Gate, Helical, Ribbons, Screws)

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 Propellers
• Usually three bladed type.
• Usually used for low viscosity liquids and high
speeds.
• Larger vessels more than one impeller can be fixed
to the same shaft.
• Do not damage dispersed particles at low speeds
• Pitch of propeller: a propeller with a pitch of 1.0 is
said to have square pitch
• Rarely exceed 18” in diameter regardless of the
size of the vessel

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 Paddles
• Flat paddle turning on a vertical shaft
• Two-bladed and four-bladed paddles are
common
• Push the liquid radially and tangentially
with almost no vertical motion
• Usually 2/3rd of vessel dia
• Low speed of Agitation
• High Intensity of Agitation

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 Turbines
• Multi-bladed paddle agitators with
short blades, turning at high
speeds
• Blades may be straight, or curved,
pitched or vertical
• Impellers may be open, semi-
enclosed, or shrouded
• Dia of impeller is smaller than with
paddles, ranging from 30 to 50%
of vessel dia
• Effective over a wide range of
viscosities

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 Anchors
• Blades follow the contour of the vessel so that
they scrape the surface or pass over with
close clearance
• Large low speed
• Prevents caking at the bottom
• Disturbs the wall film
• Mostly used for heat transfer to highly viscous
fluids
• Effective over a wide range of viscosities

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 Selection of Impellers
• In the direction of viscosity increase
Propeller  Turbine  Paddle  Anchor  Helical ribbon 
Helical screw
• Speed of impeller decreases in the above order.
• Propellers: up to 10,000 cP;
Turbines: up to 15,000 cP;
Anchors: upto 100,000 cP

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 Power consumption
• Power required to rotate a given impeller depends on:
– important measurements of tank and impeller
– viscosity  and the density  of the liquid
– speed of agitator
– acceleration of gravity g
• Empirical correlations of power with the above variables
by dimensional analysis are available.

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 Power correlation
• Power P is a function of the variables:

• By dimensional analysis:

• Taking account of shape factors:

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 Dimensionless Groups
• Power number

– Depends on Impeller type and flow regime

• Reynolds number

• Froude number

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 Power Correlations

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 Calculation of power consumption
• From the definition of NP

• At low Reynolds number

• At high Reynolds number

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 Power consumption

Type No of baffles Power No

Propeller 0 0.3

Propeller 3 to 8 0.33 to 0.37

Turbine 0 0.93 to 1.08

Turbine 4 3 to 5

Pitched blade 0 0.7

Pitched blade 4 1.3 to 1.4

Anchor 0.28

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 Mixing
• Mixing refers to the random distribution, into and
through one another, of two or more initially separate
phases
• A single homogenous material, such as a tank full of
cold water can be agitated, but it can not be mixed until
some other material is added to it

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 Factors enhancing mixing
• Low interfacial tension that inhibits the formation of interfaces

• Similar densities that prevent separation by stratification induced

by gravity and centrifugal fields

• Low viscosities that promote fluidity and the penetration of one

fluid element into another.

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 Uniformity of Mixing - Measuring
By Various kinds of tracer techniques:
• A dye is introduced and the time for attainment of uniform color is
noted
• A concentrated salt solution is added as tracer and the measured
electrical conductivity tells when the composition is uniform
• The residence time distribution is measured by monitoring the outlet
concentration of an inert tracer. The shape of response curve is
compared with that of a ideally mixed tank

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 Scale-up of Agitator Design
• When a small unit is built before the larger or production unit –
pilot plant
• When a small unit is built after the production unit - model
• Scale-up requires three types of similarity between pilot-plot
unit and full-scale unit:
– Geometric similarity
– Kinematic similarity
– Dynamic similarity

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 Geometric similarity
• Refers to linear dimensions
• Two vessels of different sizes are geometrically similar if the
ratios of the corresponding dimensions on the two scales are
the same
• If photographs of two vessels are completely super-
impossible, they are geometrically similar

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 Kinematic Similarity

• refers to motion

• requires geometric similarity and the same ratio of velocities

for the corresponding positions in the vessels

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 Dynamic Similarity
• concerns forces

• requires all force ratios for corresponding positions to be equal

in kinematically similar vessels

• the significant dimensionless parameters must be equal for

model and prototype

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 Necessary conditions for Effective
Scale-up
• First the regime must be a relatively pure one. Dynamic
similarity should depend chiefly upon a single dimensionless
group that represents the ratio of applied to the opposing
forces

• Second, the regime should not change as vessel size goes

from small to the larger scale.

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 Required Scale-up parameter for
specific duty
Duty Direction of Quantity of Turbulence Recom.,
mass flow Agitation scale-up

Heat transfer Radial Large Low Const tip

speed

Suspending Solids
Light Axial Small Low Const tip
Medium Medium Moderate speed
Heavy Large High

Blending Vertical Moderate Const tip

Miscible liq speed

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 Required Scale-up parameter for
Specific duty
Duty Direction of mass Quantity of Turbulence Recom.,
flow Agitation scale-up

Gas dispersion in Vertical Large High Constant

Liquids P/V

Dispersing Agglomerating Solids

Light Vertical Large Moderate Const P/V
Medium High
Heavy

Blending Vertical Moderate High Constant

Immiscible liquids P/V
or Emulsification

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 Tip speed required for Intensity of
Agitation
Tip speed = Pi x Dia of Agitator x RPM

Intensity of Low Medium High Very high

Agitation

Tip speed 500 to 600 650 to 800 800 to 1000

Ft/min

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 Typical Power consumptions

Degree of Agitation Power Level (W/Kg) Duty

Low 0.16 to 0.2 Suspending light solids,

blending low viscosity liquids

Moderate 0.5 to 0.6 Gas dispersion, heat transfer,

Liquid-Liquid contact

High 1.6 to 2 Suspending heavy solids,Gas

dispersion, Emusification

Very High 4 Blending pastes,Doughs

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 Questionnaire & Discussion
1. What is the significance of data capturing during Lab
observations.(2 marks)
2. Name 5 observations/data to be captured while observing
experiments in the Lab during Reaction,Work-up & distillation.
(4 marks)
3. Name 5 observations/data to be captured while observing
experiments in the Lab during filtration. (2.5 marks)
4. Name 5 observations/data to be captured while observing
experiments in the Lab during drying. (2.5 marks)
5. Filter of choice for Amorphous & incompressible cake is ____________
(Nutsche filter/Centrifuge) & Product isolated from solvents like
Toluene/Hexane / Ethers _________ (ANFD/Centrifuge) (2 marks)
6. Dryer of choice for material being isolated from water media is
____________ (FBD/RCVD) and material with very low MIE is
___________ (FBD/RCVD) (2 marks)
Total 15 marks.

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 71

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FOR
YOUR ATTENTION

Training & Development Scale-up S Lakshminarayanan, Technology Transfer 72