Particulate solids

Blending of solid Particles

 Mechanisms of mixing
1. Convective mixing: group of particles are moved from
one position to another (trough mixer with ribbon
spiral)
2. Diffusion mixing: particles are distributed over a freshly
developed interface (simple barrel mixer)
3. Shear mixing: shear stresses give rise to slip zones
and mixing takes place by interchange of particles
between layers within the zone.
 Types of mixture
• Perfect mixture of two types of particles: if group of particles is
taken from any position of mixture, it will contain the same
proportions of each particle as the proportions present in the whole
mixture. In practice cannot be obtained
• Random mixture: the probability of finding a particle of any
component is the same at all locations and equal to the proportion of
that component in the mixture as a whole
• Segregation mixture: Particles of one component have a greater
probability of being found in one part of the mixture due different
physical properties
 Segregation
• Causes of segregation are deference in:
– Size −Surface characteristics : SA and tendency to hold
– Density (bulk and true): very important in gas fluidization surface charge
– Shape −Flow characteristics
– Particle size distribution −Friability
– Moisture content
−State of agglomeration
• Mechanisms of segregation
1. Trajectory segregation : when particles move through the air or fall from the end of
conveyor
v p D p2 l- distance traveled
v – fluid velocity
l ρp- particle density

18
dp- particle diameter
µ fluid viscosity

2. Percolation of fine particles: fine particles percolate down through the gaps between
larger ones. Occurs during mixing, shaking, vibration or pouring particles into heap
 Segregation
3. Rise of course particles on vibration: If a mixture of particles of different
size vibrated the larger particles move upward. This may be explained
by buoyancy effect created by the carrying pressure generated across
the vibrated bed

4. Elutriation segregation: when a powder contains large proportion of

particles <50 µm is charged into a storage hopper, air is displaced
upward. If the air v >vterm of particles they will remain in suspension
 Segregation
• Segregation can be reduced by:
– Making the size of components as similar as possible. Reducing the size of both
components. Segregation is not problem for particles <30 µm (if ρ=2000-
3000kg/m3) as interparticle forces > gravitational
– Adding small quantity of fluid to reduce the mobility and to permit better mixing
– Using of ordered or interactive mixtures which are made of small particles (<5
µm) adhered to surface of carrier particles (used in pharmaceutical industry)
 Mixing Equipment
1. Tumbling mixers: closed vessel rotating about its axis (cube, cone, V shape).
– Mechanism: diffuse mixing
– Problem: segregation in free-flowing powders (to minimize use baffles)
 Mixing Equipment
2. Convective mixers: circulation patterns are set up within static
shell by rotating blades or paddles
• Main mechanism is convective mixing
• Accompanied with diffuse and shear mixing
 Mixing Equipment
3. Fluidized bed mixers: rely on the natural mobility
afforded particles in the fluidized bed
• Mechanism is largely convective with circulation patterns set
up by bubble motion within the bed
• Several processing steps are carried out in the same vessel
(mixing, reaction, coating, drying, etc.)

4. High shear mixers: high shear stresses are created by

devices similar to those used in comminution
• Dominant mechanism is shear mixing
• Breaks down agglomerates of cohesive powders rather than
particles
• Ex. Low speed compression roller
 Assessing the mixtures
• Sampling: required to determine the quality of mixing
• Statistics relations relevant to mixing
– Mean composition: the true composition is often not known but
can be estimated
1 N
y   yi
N i 1

– Standard deviation and variance

(y i   )2
S2  i 1 If the true composition µ is known
N
N

(y i  y)2
S2  i 1 If the true composition is not known
N 1
 Assessing the mixtures
– Theoretical Limits of variance: for two
component system
A. Upper limit: true standard deviation for a
completely unmixed system, σ0
 02  p(1  p)
B. Lower limit: true standard deviation of random
p(1  p) n- number of particles
binary mixture, σR
– where p, 1 - p : fractions of two components in the whole  
2
R
in the sample

–
mixture
The actual value of variance lie between these two values
n
– Degree of Mixing (Mixing indices)
A. Lacy mixing index is the ratio of ‘mixing achieved’
to ‘mixing possible’
 02   2
If =0- complete segregation Lacy.mixing .index (b)  2
If =1- completely random mixture  0   R2
B. Poole mixing index
• Gives better discrimination for practical mixtures and

approaches unity for completely random mixtures
IP 
– Standard error: for normally distributed sample
STRD dev of the variance is known as standard R
error (E(S2))
 Assessing the mixtures
• Tests for precision of mixture composition and variance
– Assuming normal distribution of the sample compositions
1. Sample composition t is student test value for the specified confidence
tS level. For example, at 975% confidence level, t =
  y 2.0 for N = 60, and so there is a 975% probability
N that the true mean mixture composition lies in the
range: y ±0.258S.
2. Variance
 2  S 2  t  E ( S 2 )
– For N>50
2
E (S 2 )  S 2
N
S 2 ( N  1)
 2

– For N<50 L
2
S 2 ( N  1)
 2

U
12
Where α is the significance level (for 90% confidence range, α= 0.5(1-90/100)=0.05); for 95%

confidence range , α= 0.5(1-95/100)=0.025). For  2

they can be found in  2 distribution tables
 Sampling
• Only very rarely it is possible to perform a size analysis on the entirety of the powder
of interest. The aim of sampling is to obtain a fraction which is representative of the
whole. The "golden rules" of sampling are:
– a powder should always be sampled while in motion
– it is better to take the whole of the powder for a short time than some of the powder for a
longer time.
• The enemy of good sampling is segregation which is the word used to describe the
separation of particles due to differences in physical properties such as shape and
density.
• One of the most common forms of segregation occurs when particles are tipped onto
surfaces or into bins and the coarser particles tend to roll down the sloping sides of
the tip, leaving a greater concentration of fine particles near the centre.
• When obtaining a small sample for analysis, it is advisable to use a device such as a
"riffler" to divide the bulk into many smaller samples, and to further subdivide these
samples by the same technique until a sufficiently small sample is obtained.
• It is necessary to sample particles from a flowing suspension, where in practice it is
impossible to collect all of the suspended material.
• Two general methods of measurement are employed: those in which the sample is
extracted from a duct and analyzed outside it, and those in which some form of a
measuring instrument is inserted
 Cone and Quartering

1. 2.

3.
Take A and D or C and B
A B
C D

Error – 20%
True Fractional
Shovelling
Splitting ratio   1/ N  1/ 5
 Riffling

Error - 5%
Riffling
Rotary Sample Division

Error < 1%  used for chemical analysis

 Example

The performance of a solids mixer has been assessed by calculating the variance occurring
in the mass fraction of a component amongst a selection of samples withdrawn from the
mixture. The quality was tested at intervals of 30 s and the results are
Sample variance
(σ2) 0.025 0.006 0.015 0.018 0.019

Mixing time (s) 30 60 90 120 150

If the component analysed is estimated to represent 20% of the mixture by mass and each
of the samples removed contained 100 particles, comment on the quality of mixing of the
mixture produced and present the data in graphical form showing the variation of mixing
index with time