Particle sizing

Why make the particles smaller?

Engineering in Chemical and Pharmaceutical
Processes
Particle sizing
Comminution

more precise dosage

increasing surface area
faster dissolution, drying

attain uniform size

better compressibility

Why make the baricles bigger?

decrease compressibility , improve flowability
fix homogeneity
improve particle shape
Engineering in Chemical and Pharmaceutical Processes
Particle Sizing, Comminution

Decreasing particle size

Fragmentation theory

Comminution processes by input particle size

Solid (crystal)

Coarse d = 20 100 cm (crushers, grinders, cutters)

Medium d = 2 20 cm (mills, raspers)
Fine d = 0,3 2 cm (mills)
Very fine (special mills)

Molecules arranged in a structure (crystal lattice)

Energy needed to break the structure

Comminution
very inefficient energy utilization

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Energy consumption

Rittingers law (1867)

Fragmentation

Assumption

energy consumption proportional to newly formed surface

area
fragmentation occurs in structural defects

energy consumption proportional to newly formed surface area

Based on balance of surface and volume of particles

Losses

elastic deformation of particles

powder bulk compaction
friction
plastic deformation of particles

V1 k V d 1

S1 k S d1

V 2 kV d 2

S2 kS d2

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

N 1 2

V1
V2

Rittingers law (1867)

Rittingers law (1867)

Newly formed surface

S 1 2 N 1 2 S 2 S 1

V1
V2

S 2 S1

d
d

k S d 2 k S d1
2

Newly formed specific surface

S spec

S spec

S 1 2
m

k 1 1
1

k V d 2
d1

KR ... Rittingers constant

fc ... material strength in compression [N.m-2]

Diferential form
Aplication

d 13

3 k S d 22 k S d 12

V1
k V d 1 d 2

S 1 2

1
1
1
1
K R fc

E C

d d
d 1
1
d2
2

Integral form
3
1
3
2

dE

dd

1
d

Suitable for very fine milling

dp < 0,05 mm
Energy consumption overestimated for larger particles

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Kicks law (1885)

Kicks law (1885)

Assumption

Integral form
d1

Energy consumption proportional

to comminution ratio

d2

Deriving differential form

d2

d1 d1

d1

E C

d1
d
d

d2

K K f c ln

d1
d2

KK ... Kicks constan

d1

lim d 0

d1

Symbols

d1

E C ln

Application
dE

dd

1
d

underestimates energy needed to comminute smaller

particles
good for coarse milling and crushing
dp > 50 mm

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Griffiths theory

Bonds law (1952)

Solid body under stress accumulates energy (deformation

energy)
Deformation energy (DE) is not distributed uniformly
throughout the body

Semiempirical, validated by application on materials

DE is concentrated on structural defects in material

Concentration factor
L, R longitudial and lateral dimension of defect

Fragmentation occurs by spreading the defects (failures) if

DE accumulated is greater than increase in surface energy by
fragmentation
there is a defect within the material (most materials contain defects
naturally)

E C

1
d2

K f
B c

d 1

1
d2

d 1

Symbols
KB ... Bonds constant
fc ... material strength in compression [N.m-2]

Aplication
for common milling processes
0,05 mm < dp < 50 mm

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Bonds law (1952)

Energy consumption (generalization)

Integral form

E C

d2

General formula

K f
B c

d 1

d2

d 1

Differential form
dE
dd

3 2

Practical form
W1 work index

dd

Kf c

Rittinger

1
d

Symbols

dE

10
10
E W1

d
d 1
2

energy for comminution from infinity size to 100 m

particle size approximated at F(d) = 80 %

d ... particle size

E ... energy
K ... constant
n ... process order
fc ... material strength

n = 2, K = KR

Kick
n = 1, K = KK

Bond
n = 1,5, K = KB

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Comaprison and validity of comminution

laws

General comminution principles

Degree of comminution, s
D input size of coarse particles
d output size of coarse particles

D
d

Comminution energy
depends on particle size

Comminution efficiency
low: 1 80 %
experiment needed to characterize the material in
comminutor
then possible application of laws
Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Mechanisms of comminution

Mechanisms of comminution

Compression between surfaces

Impact on surface

particle particle or particle equipment interaction

low speed 0,01 10 m.s-1
crushing and shear

particle particle or particle equipment interaction

high speed 10 2000 m.s-1
impact and shear

Shear applied by medium

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Jaw crusher

Cone crusher

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Hammer mill

FitzMill Comminutor
mln na principu kladivovho mlnu pro farmacii

Velmi univerzln podle typu kladiv

Produkuje ostr stice (vrazn hrany)
Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Vertical shaft mill

Ball mill

vc

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

gr

Roller mill

Colloidal mill

Colloidal mill
wet operation
very fine milling
narrow PSD in product

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Bead mill

Micronizer
slurry milling
friction in milling media
spheres, beads, sand

Impacts of high velocity particles

in gas stream

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Mechanisms of comminution
Direction of stress
Compression
Shear
(Tension)

Comminution affected by material properties

Material properties

Stress
Plastic
deformation
fracture

Aplication of force
direct (thin layer)

Elastic
deformation

roller mill, colloidal mill

layer (lower efficiency layer compression)

ductile x brittle
different properties in
compression/shear
different behavior in
pressure/impact
different hardness

deformation

ball mill

Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Specific requirements for equipment

Specific requirements for equipment

Due to the properties of comminuted material

Due to the properties of comminuted material

hard (brittle and abbrasive)

slippery

low speed, low contact equipment

inefficient compression

plastic

explosive

ineffective compression, effective shear, cryoprocessing

wet, cohesive

inert atmosphere, wet operation

toxic

poor flowability, possible wet operation (suspension)

process containments

temperature sensitivity
low shear, wet operation

sticky
simple equipment advantageous due to cleaning
Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Product particle size distribution

Product PSD

Empiricaly determined for each apparatus

Prediction
particle size classes
Sj Specific rate of fragmentation for class j
determines fragmentation rate for each size class
similar to rate constant
[s-1]

bi,j Comminution distribution function

which particles will form by fragmentation of j-class particle
probability of formation i class particle from j-class particle
(percentage)
Engineering in Chemical and Pharmaceutical Processes

Engineering in Chemical and Pharmaceutical Processes

Particle Sizing, Comminution

Particle Sizing, Comminution

Product PSD
dmi
dt

Simi

Fragmentation of iclass particle

i, j

S jm j

i j

Formation of i-class
particles from jclass particles

S and b are mill properties

Experimental estimation of S, b
S, b may depend on operation (e.g. rotational speed)
Engineering in Chemical and Pharmaceutical Processes
Particle Sizing, Comminution