1

A SUMMER INTERNSHIP
REPORT
AT
Fenix Process Technologies Pvt. Ltd.

Submitted by:
Ch Venkatesh
University college of engineering (ucek),
JNTUK KAKINADA
 2

ACKNOWLEDGEMENT

The internship opportunity I had with Fenix process technologies pvt. Ltd. was a great chance
for learning and professional development. Therefore I consider myself as a very lucky
individual as I was provided with an opportunity to be a part of it. I am also grateful for having a
chance to meet so many wonderful people and professionals who led me though this internship
period.

Bearing in mind previous I am using this opportunity to express my deepest gratitude and
special thanks to the MD of Fenix who in spite of being extraordinarily busy with his duties,
took time to hear, guide and keep me on the correct path and allowing me to carry out my
project at their esteemed organization and extending during the training.

I express my deepest thanks to Mr. Sreedhar Baddi, vice president for taking part in useful
decision and giving necessary advices and guidance and arranged all facilities to make life
easier. I choose this moment to acknowledge his contribution gratefully.

It is my radiant sentiment to place on record my best regards, deepest sense of gratitude to Mr.
Swapnil Sonar, Ms. Priyanka Parmar and Mr. Hemant Yerme of R&D Dpt., Fenix for their
careful and precious guidance which were extremely valuable for my study both theoretically
and practically.

At the last but not least I would like to express my sincere thanks to Mr. Sarath Chandra
Sharma of Maintenance Dpt., Mr. Sagar Pansare of QC Dpt., Ms. Nilam Mundhe of HR Dpt.
and all other staff for their continue guidance and support for me during this internship period.

I perceive as this opportunity as a big milestone in my career development. I will strive to use
gained skills and knowledge in the best possible way, and I will continue to work on their
improvement, in order to attain desired career objects. Hope to continue cooperation with all
of you in the future.

Sincerely,

Ch Venkatesh

Place: Fenix Factory, Jejuri

Date: 14th June 2016

 3

CONTENTS

S.NO. TOPIC PAGE NO.

1 Vapor liquid equilibrium 4

2 Lube oil Re-refining 16

3 Sieve analysis 30

4 Distillation column design by

33
McCabe-Thiele method
5 Distillation column internals 39

6 Pusher centrifuge 61

7 Mixing technology 64
 4

VAPOUR LIQUID EQILIBRIUM

Dt: 16-05-2016

OBJECTIVE: To experimentally determine the vapor-liquid equilibrium

conditions for the binary ACETONE-WATER system and correlate the results for
the use in the analysis of the distillation column.

THEORY:
Vapor-liquid equilibrium (VLE) is a condition in which a liquid and its vapor (gas
phase) are in equilibrium with each other & in this condition the rate evaporation
equals to the rate of condensation on a molecular level such that there is no net
vapor-liquid interconversion .

THERMODYNAMIC DESCRIPTION OF VLE:

PURE (Single-component) SYSTEMS:

If the liquid and vapor are pure i.e; they consist only one molecular component
and no impurities, then the equilibrium state between the two phases is
described as follow:

Pliq=Pvap ;

Tliq=Tvap ; and

Gliq=Gvap

Where Pliq, Pvap, Tliq, Tvap, Gliq, Gvap are the pressures, temperatures, Gibbs free
energies within the liquid and vapor respectively.

MULTICOMPONENT SYSTEMS:
 5

In a multicomponent system, vapour and liquid consist of more than one type of
molecule. For all components i in the system, the equilibrium between the two
phases is described by :

Pliq=Pvap ;

Tliq=Tvap ; and

Giliq=Givap

Where P and T are the temperature and pressure for each phase, and Giliq and
Givap are the partial molar Gibbs free energy also called chemical potential within
the liquid and vapor, respectively, for each phase. The partial molar Gibbs free
energy is defined by:

Gi =

Where G is the (Extensive) Gibbs free energy, and is the amount of substance
of component .

BOILING-POINT DIAGRAMS:

Binary mixture VLE data at a certain overall pressure showing mole fraction vapor
and liquid concentrations when boiling at various temperatures can be shown as
a two-dimensional graph called a Boiling-point diagram. The mole fraction of
components 1,2 in the mixture be X1,X2 respectively. Then:

X1 + X2 = 1

In multi-component mixtures in general with n components, this becomes:

X1 + X2 + + Xn = 1

The preceding equilibrium equations are typically applied for each phase (liquid or
vapour) individually.

In a binary boiling-point diagram, temperature (T) is graphed vs. X1. At any given
temperature where both phases are present, vapor with a certain mole fraction is
 6

in equilibrium with liquid with a certain mole fraction. These vapor and liquid
mole fractions are represented by two points on the same horizontal isotherm
line.

When an entire range of temperatures vs. vapor and liquid mole fractions is
graphed, two lines result. The lower one, representing the mole fraction of the
boiling liquid at various temperatures, is called the bubble point curve. The upper
one, representing the mole fraction of the vapor at various temperatures, is called
the dew point curve.

These two lines (or curves ) necessarily meet where the mixture becomes purely
one component, namely where X1 = 0 ( and X2 = 1, pure component 2) or X1 = 1 (
and X2 = 0, pure component 1 ). The temperatures at those points correspond to
the boiling point of the two pure components.

Azeotropic mixtures:

For azeotropic pairs of substances, the two curves also coincide at some point
strictly between X1 = 0 and X1 = 1. When they meet, they meet tangentially; the
dew-point temperature always lies above the boiling-point temperature for a
 7

given composition when they are not equal. The meeting point is ccalled an
azeotrope for that particular pair of substances. It is characterized by an
azeotrope temperature and an azeotropic composition. There can be maximum-
maximum
boiling azeotropes, where the azeotrope temperature is at maximum in the
boiling curves, or minimum
um-boiling
boiling azetropes, where the azeotrope temperature
is at a minimum in the boiling curves.

VLE diagrams:

These diagrams would graph liquid mole fraction on a horizontal axis and vapor
mole fraction on a vertical axis. Here also:

X1 + X2 = 1 and Y1 + Y2 = 1
 8

Raoults law:

Raoults law states that for components 1, 2, etc. in a mixture:

P1 = X1P01 , P2 = X2P02 ,.. etc.

Where P01 , P02 ,etc. are the vapor pressures of components 1,2,etc. when they
are pure, and x1 , x2, etc. are mole fractions of the corresponding component in
the liquid.

Raoults law approximately valid for mixtures of components between which

there is little interaction other than the effect of dilution by the other
components. Example: mixtures of alkanes , which are non-polar, relatively inert
compounds in many ways, so there is little attraction or repulsion between the
molecules.

Daltons law:

At boiling and higher temperatures the sum of the individual component partial
pressures becomes equal to the overall pressure ,Ptot.

Ptot = P1 + P2 + ..
 9

Then for each component in the vapor phase:

Y1 = P1 Ptot , Y2 = P2 Ptot , . Etc.

Where P1 = partial pressure of component 1 ,

P2 = partial pressure of component 2, etc.

K value:

The tendency of a chemical species to partition itself preferentially between liquid

and vapor phases is the Henrys law constant. for multi-component mixtures, the
VLE data are represented in terms of K values (vapor-liquid distribution ratios)
defined by :

Ki =

Where Xi,Yi are the mole fractions of the species i in the liquid and vapor phases,
respectively.

Assuming ideal conditions near ambient temperature and pressure, the K-value
may be described according to Henrys and Raoults laws for dilute and
concentrated solutions respectively:

Henrys Law: Ki = Hi

Raoults Law: Ki = Pis/P

Where Hi is an empirical constant, Pis is the saturation vapor pressure of pure

component i, and P is the total pressure of the equilibrium vapor mixture
assuming Daltons Law:

P=

Where Pi is the partial pressure of species i in the vapor phase.

 10

For binary mixtures, the ratio of the K values for the two components is called the
relative volatility denoted by .
/
= Ki/Kj =
/

Which is a measure of relative ease or difficulty of separating the two

components. Large-scale industrial distillation is rarely taken if the relative
volatility is less than 1.05 with the volatile component being i and the less volatile
component being j.

EXPERIMENTAL SETUP:

EQUIPMENT:
1. Equilibrium still
2. Gas chromatography instrument
3. 10 ml volumetric flask
4. 2 ml Clip lock tubes OR Sample vials
5. Digital thermometer
6. Beakers
7. Syringe

CHEMICALS:
1. Acetone
2. Water

DESCRIPTION:
A vapor-equilibrium still consists of:

A. A boiling pot
B. Central and outlet vapor tubes
C. Thermocouple
 11

D. Condenser
E. Pot sampling cock
F. Interchangeable receiver with liquid sampling cock which can hold approx.
15 ml of distillate.

EXPERIMENTAL PROCEDURE:
1. Prepare a mixture of 250 ml acetone and 60 ml water in a 500 ml beaker.
2. Feed the mixture in to the boiling pot.
3. Switch on the heater and the digital thermometer.
4. Switch on the cooling water supply to the condenser.
5. Note down the top temperature and bottom temperature for every 5
minutes of interval.
6. Note down the temperature at which condensation begins.
7. Take samples of the vapor distillate and liquid in the clip lock tubes at
different time intervals, when sufficient amount of distillate is collected in
the distillate receiver.
8. The remaining distillate obtained is kept separately and add 40 ml of water
in to the boiling pot for every sample collected.
9. The procedure is repeated until the temperature is reached up to the
boiling point temperature of water, i.e; 100 c.
10.The samples taken are analyzed in a gas chromatography instrument and
the compositions of water and acetone in different sample are noted down.
11.Draw a Temperature (T) vs. X, Y graph by plotting T on the vertical axis and
X, Y on the horizontal axis.
12.Draw another graph showing Y on the vertical axis and X on the horizontal
axis.

OBSERVATIONS:
 12

TABULAR FORM:

S.NO TIME TEMPERATURE (C) REMARKS

TOP BOTTOM
1 10:38 34 34 HEATER ON
2 10:43 35 36
3 10:48 49 43
4 10:53 53 47 CONDENSATION START
5 10:58 57 50 CUT 1
6 11:03 59 56
7 11:07 61 57 CUT 2
8 11:12 60 58
9 11:17 60 58
10 11:20 62 59 CUT 3
11 11:28 60 61
12 11:33 61 62
13 11:37 64 63 CUT 4
14 12:00 64 66 CUT 5
15 12:13 64 69
16 12:23 69 77 CUT 6
17 12:27 68 75
18 12:32 67 73
19 12:42 73 81 CUT 7
20 12:47 68 80
21 12:53 72 81
22 13:42 80 92
23 13:49 78 88 CUT 8
24 13:54 84 90
25 14:01 86 94 CUT 9
26 14:08 84 92
27 14:13 87 94 CUT 10
28 14:20 84 93
29 14:25 81 91
30 14:31 87 94
31 14:39 89 99 CUT 11
32 14:46 88 94
33 14:51 89 100
34 14:56 90 100 CUT 12
35 15:02 96 97 CUT 13
 13

GAS CROMATOGRAPHY ANALYSIS:

S.NO. TEMPEARTURE DISTILLATE COMPOSITION RESIDUE COMPOSITION

(C) (%) (%)
WATER ACETONE WATER ACETONE
1 57 18.9841 80.6359 26.3796 73.0140
2 61 8.4750 91.4310 26.8845 72.3245
3 62 8.0901 91.8180 25.6440 74.0382
4 63 8.7885 91.0941 27.5207 72.2709
5 66 10..2121 89.7174
6 69 13.1921 86.6813
7 74 19.8444 80.0890 34.1312 65.8120
8 76 23.9594 75.9805
9 86 51.6227 48.3229 55.1580 44.8421
10 87 68.5985 31.3665 62.4705 37.5295
11 89 84.7303 15.2696 66.2088 33.7912
12 91 90.5451 8.3151 72.1778 27.1413
13 95 73.7435 25.5217

CALCULATIONS:
Antoine parameters:

A B C
Water 8.07131 1730.63 233.7912
Acetone 7.6313 15566.69 273.419

Total pressure Ptot = 760 mm of Hg

Partial pressure at saturation temperature T from Antoine equation:

logP =

Using Raoults law , the acetone mole fraction in the liquid residue
(Xacetone) can be calculated from the acetone mole fraction in the
distillate (Yacetone) as:
 14

!"# $ %!"!
Xacetone =
&

The obtained results are tabulated as:

S.NO. TEMPERATURE (C) Pacetone (mm of Hg) Yacetone Xacetone

1 57 775.845 0.806359 0.78980
2 61 884.074 0.914310 0.78599
3 62 912.968 0.918180 0.76433
4 63 942.626 0.910941 0.73445
5 66 1036.34 0.897174 0.65794
6 69 1137.47 0.866813 0.57916
7 74 1323.70 0.800890 0.45982
8 76 1404.75 0.759805 0.41107
9 86 1872.18 0.483229 0.19616
10 87 1925.05 0.313665 0.12366
11 89 2034.37 0.152696 0.05700
12 91 2148.60 0.831510 0.02941
13 95 2392.39 0.255217 0.08100

Graphical representation of:

1. T vs. Yacetone , Xacetone :

100
90
80
70
60
50
T

40 T-x
30
20 T-y
10
0
0 1
x and y
 15

2. Yacetone vs. Xacetone:

0.9

0.8

0.7

0.6
vapor- liquid equilibrium
y 0.5 curve
0.4 x=y line

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
x

RESULT:
The behavior of the ACETONE-WATER system is studied at various temperatures
with various feed compositions and VLE graph is plotted showing the liquid and
vapor compositions of acetone in the binary water-acetone mixture at various
isothermal conditions.

APPLICATIONS:
1. VLE diagrams are used in the McCabe-Thiele method to determine the
equilibrium stages (or theoretical plates) needed to distill a given
composition binary feed mixture in to one distillate and one bottom
fraction.
2. In the determination of activity coefficient for the low pressure systems
containing an ideal gas phase, but a non-ideal liquid phase.
 16

LUBE OIL (USED) RE-REFINING

OBJECTIVE:
To re-refine the used lube oil which will restore the chemical composition of the
base oil so that it can be used to produce new lubricant products over and over
again.

THEORY:
Lubricants are typically comprised of 80-90 % base oil and 10-20% specialty
additives that distinguish the product such as a motor oil, transmission or
hydraulic fluid, or industrial process oil. Most all base oils originate from the
processing of crude oil. The lubricants eventually become spent and are no
longer effective because either the additives have broken down or the lubricant
has become contaminated with impurities during its use.

However, the base oil retains its original properties and usefulness. So it can be
regained in the re-refining process described as below:

Used oil re-refining is the process of restoring used oil to new oil by removing
chemical impurities, heavy metals, moisture and dirt.
 17

Re-refining is an energy efficient and environmentally beneficial method for

managing used oil. Instead of burning the used oil, which releases harmful
emission into the atmosphere, re-refining conserves the base oil.

The different process steps involved in the re-refining are:

A. Pretreatment and dewatering:

The oil is stored to allow water and solids to separate out from the oil and
the solids are separated by filtration then the oil is heated to 120c in a
closed vessel to boil off any emulsified water and some of the fuel diluents.
Then light hydrocarbons are removed by distillation.
 18

B. Diesel removal:
The residue obtained from the step 1 is further distilled at higher
temperatures to remove the diesel fraction as a distillate in the process.

C. Asphalt removal:
The residue obtained in the step 2 is further processed in a thin film
evaporator at higher temperature and high vacuum to remove the asphaltic
fraction from it.

D. Solvent extraction/ finishing:

After removing water, light hydrocarbons and asphaltic fraction, chemical
treatment of the waste oil by solvent extraction using N-methyl pyrolidine
(NMP) to remove the undesired aromatic contents present in it.
 19

E. Hydro treating:
After removing water, light hydrocarbons and asphaltic fraction, chemical
treatment of waste oil by hydrogenation is done to remove the sulphur
contents present in it.

F. Fractionation:
The obtained waste oil undergoes fractionation in distillation column to
recover the different cuts of base oil according to their boiling points.
20
21
 22

EQUIPMENTS:
Vertical thin film evaporator, heating drum, cooling tower, vacuum pump, chilling
system, separating funnel, volumetric flasks

CHEMICALS:
Used lube oil, Therminol (Thermic fluid), N-methyl pyrrolidinone (NMP)

DESCRIPTION:
VERTICAL THIN FILM EVAPORATOR:

The vertical thin film dryer consists of a cylindrical, vertical body with heating
jacket and a rotor inside of the shell which is equipped with rows of pendulum
blades all over the length of the evaporator. The hinged blades spread the feed
product in a thin film over the heated wall. The thickness of the layer is defined by
the clearance between the blade and the wall. A highly agitated bow wave is
formed in front of the rotor blades. The turbulence increases as the product
passes through the clearance before entering a calming zone situated behind the
blades. The volatile component evaporates continuously. The product layer is
typically less than a millimeter in thickness. The volatile component is then
condensed by the cooling water used in the chilling system supplied to the cetre
of the evaporator. So the volatile component is collected at the centre and other
components of the feed are collected in the outer side. The heating medium is
normally high pressure steam or oil.
 23

EXPERIMENTAL PROCEDURE:
Dt: 24-05-2016

STAGE 1: DEHYDRATION IN A VERTICAL THIN FILM EVAPORATOR:

FEED: used oil , 10.0 L

PROCEDURE:

1. The used oil is feed in to the feed tank.

2. The thermic fluid heater and chiller are started simultaneously.
3. Note down the thermic fluid temperature for every 10 minutes and raise
the temperature up to 120 c.
4. Once the temperature is achieved start the vacuum pump and rotation of
the shaft.
 24

5. Start the flow of feed in to the vertical cylindrical shell where it is heated by
the hot thermic fluid present in the shell side.
6. The lighter components present in the feed such as water boil up and are
condensed by the internal condenser and are further collected as liquid in
the distillate tank.
7. The remaining heavy components are collected in the residue tank.

OBSERVATION:

Thermic fluid temperature: 120 c

Vacuum: 300 mm Hg
Shaft rotation speed: 300 rpm

S.NO. Thermic fluid Set point Time Remarks

temperature (c) temperature (c)
1 32 38 11:10 Heating start
2 68 70 11:20
3 90 90 11:30
4 91 90 11:40 Heating stop
5 95 98 11:50 Heating start
6 100 105 12:00
7 120 119 12:10 Vacuum , shaft
rotation start
8 120 120 12:20 Flow of feed start
9 120 120 12:25
10 119 120 13:30 No distillate obtained

Dt: 25-05-2016

STAGE 2: DIESEL STRIPPING:

FEED: residue fraction from dehydration process, 9.5 L
 25

PROCEDURE:

1. The residue fraction from the dehydration process is loaded into the
feed tank.
2. The thermic fluid heater and chiller are started simultaneously.
3. Note down the thermic fluid temperature for every 10 minutes and
raise the temperature up to 220 c.
4. Once the temperature is achieved start the vacuum pump and
rotation of the shaft.
5. Start the flow of feed in to the vertical cylindrical shell where it is
heated by the hot thermic fluid present in the shell side.
6. The lighter components present in the feed such as water boil up and
are condensed by the internal condenser and are further collected
as liquid in the distillate tank.
7. The remaining heavy components are collected in the residue tank.

OBSERVATION:

Thermic fluid temperature: 220 c

Vacuum: 3-4 torr
Shaft rotation speed: 300 rpm

S.NO. Thermic fluid Set point Time Remarks

temperature (c) temperature (c)
1 46 49 10:30 Heater started
2 65 63 10:40
3 86 85 10:50
4 99 104 11:00
5 115 118 11:10
6 131 134 11:20
7 141 146 11:30
8 160 166 11:40
9 171 181 11:50
10 181 183 12:00
11 191 193 12:10
 26

12 200 205 12:20

13 217 222 12:30 Vacuum, shaft
rotation started
14 223 223 12:40 Feed flow started
15 223 223 12:50
16 220 220 13:30
17 220 220 14:15 200 ml distillate
collected

Dt: 30-05-2016

STAGE 3: ASPHALT REMOVAL:

FEED: residue from diesel stripping process, 9.0 L

PROCEDURE:

1. The residue fraction from diesel stripping process is loaded in to the feed
tank.
2. The thermic fluid heater and chiller are started simultaneously.
3. Note down the thermic fluid temperature for every 10 minutes and raise
the temperature up to 265 c. When the temperature crosses 100c purge
the thermic fluid with nitrogen gas to remove any oxygen present and
prevent oxidation and also to avoid vaporizing of the thermic fluid by
raising its boiling point by purging with nitrogen.
4. Once the temperature is achieved start the vacuum pump and rotation of
the shaft.
5. Start the flow of feed in to the vertical cylindrical shell where it is heated by
the hot thermic fluid present in the shell side.
6. The lighter components present in the feed such as water boil up and are
condensed by the internal condenser and are further collected as liquid in
the distillate tank.
7. The remaining heavy components are collected in the residue tank.
 27

OBSERVATION:

Thermic fluid temperature: 265 c

Vacuum: 3-4 torr
Shaft rotation speed: 300 rpm

S.NO. Thermic fluid Set point Time Remarks

temperature (c) temperature (c)
1 34 41 10:50 Heater started
2 60 57 11:00
3 73 76 11:10
4 90 91 11:20
5 91 105 11:30
6 103 117 11:40
7 118 131 11:50
8 132 142 12:00
9 142 154 12:10
10 152 169 12:20
11 166 180 12:30
12 180 185 12:40
13 181 192 12:50
14 196 201 13:00 Nitrogen purged
15 219 222 13:20
16 223 222 13:30
17 228 231 13:40
18 231 235 13:50
19 237 238 14:00
20 241 245 14:10
21 246 246 14:20
22 252 256 14:30
23 256 260 14:40
24 258 260 14:50
25 261 265 15:00 Vacuum, shaft
rotation started
26 263 265 15:10 Feed flow
started
27 265 265 15:20
28 264 265 16:05 150 ml distillate
collected
 28

Dt: 30-05-2016

STAGE 4: SOLVEN EXTRACTION:

FEED: distillate from the asphalt removal process containing lube oil fractions,
8.5 L

PROCEDURE:

1. Add N-methyl pyrrolidinone (NMP) to the distillate obtained from

Asphalt removal process in 3:1 ratio.
2. The solution is put in a separating funnel and left undisturbed for
separation to take place in between the two phases.
3. NMP is an aromatic selective solvent which extracts the aromatic
fractions present in the paraffinic lube oil solution.
4. After the separation is completed, two layers can be seen the funnel;
the upper layer contains NMP with the extracted aromatics and the
lower one containing the lube oil.
5. After separation about 35 ml of lube oil has been recovered.

RESULT:
1. At the end of stage 1, no distillate is obtained.
2. At the end of stage 2, 200 ml of distillate containing low boiling
hydrocarbons in the range of diesel is obtained.
3. At the end of stage 3, 150 ml of distillate is obtained, containing base oil
and aromatics and the residue containing asphalt.
4. At the end of stage 4, 30 ml of lube oil is recovered.
 29

BENEFITS OF RE-REFININIG:
1. Reduce dependence on base oil imports saving foreign exchange.
2. Prevent ground water contamination and pollution of surface water.
3. Preserve natural resources like coal and crude oil.
4. Reduce sewage treatment costs.
5. Eliminate improper burning of waste oil as fuel, which generate toxic fumes
and air pollution.
 30

SIEVE ANALYSIS
Dt: 22-05-2016

OBJECTIVE: To separate the various fractions of the given sodium methoxide

powder sample according to their particle sizes using the sieve analysis technique.

DESCRIPTION:
A sieve analysis is a practice or procedure used to assess the particle size
distribution of a granular material.

The size distribution is often of critical importance to the way the material
performs in use. A sieve analysis can be performed on any type of non-organic or
organic granular materials including sands, crushed rock, clays, granite, feldspars,
coal, soil, a wide range of manufactured powders, grain and seeds, down to a
minimum size depending on the exact method.

TYPES OF SIEVES:

1. Woven wire mesh sieves: these sieves are usually have nominal aperture
ranging from 20 micrometers to 3.55 millimeters, with diameters ranging
from 100 to 450 millimeters.
2. Perforated plate sieves: these can have round or square apertures ranging
from 1 mm to 125mm. the diameters of the sieves range from 200 to
450mm.
3. American standard sieves: the nominal aperture of these sieves range from
20 micrometers to 200 millimeters, however these sieves have only 8 and
12 inch diameter sizes.

WORKING:
 31

A typical sieve analysis involves a nested column of sieves with wire mesh cloth
(screen). A representative weighed sample is poured into the top sieve which has
the largest screen openings. Each lower sieve in the column has smaller opening
than the one above. At the base is a round pan, called the receiver.

The column is typically placed in a mechanical shaker. The shaker shakes the
column, usually for some fixed amount of time. After the shaking is complete the
material on each sieve is weighed. The weight of the sample of each sieve is then
divided by the total weight to give a percentage retained on each sieve.

EQUIPMENT: a shaker with a number of sieves having different sizes, weighing

machine

CHEMICAL: 100 gm SMO sample

PROCEDURE:
1. Take the sample of 100 grams of sodium methoxide and place it on the
upper sieve of the mechanical shaker.
2. Set the shaking time to 10 minutes.
3. Switch on the power supply to the shaker.
 32

4. After shaker is stopped, collect the samples from different sieves and weigh
them on the weighing machine.
5. Tabulate the percentage of different size particles retained on each sieve.

OBSERVATIONS:
Weight of SMO sample taken = 100 gm

Tabular form:
S.NO. SIEVE SIZE (m) WEIGHT RETAINED(gm) WEIGHT RETAINED (%)
1 425 11.15 11.15
2 355 02.60 02.60
3 210 18.00 18.00
4 150 28.50 28.50
5 125 16.00 16.00
6 106 02.35 02.35
7 75 05.40 05.40
8 53 07.18 07.18
9 38 01.06 01.06
10 - 00.09 00.09

PRECAUTIONS:
1. The sieves should be free of moisture.
2. The sieves should be arranged in decreasing order of their sizes from top to
bottom.
3. Sample weights should be measured accurately.

RESULT:
The fractions of the given SMO sample retained at different sieves are calculated
and observed that the majority of the particles are having sizes 150 m and more.
 33

DISTILLATION COLUMN DESIGN

BY McCabe-Thiele method

DISTILLATION:
Distillation is a process in which a liquid or vapor mixture of two or more
substances is separated into its component fractions of desired purity, by the
application and removal of heat.

It is a unit operation and the components to be separated depend on the

differences in boiling points of the individual components. Also, depending on the
concentrations of the components present.

Methods of Distillation:

1. Differential or simple Distillation

2. Flash Distillation
3. Rectification or Fractional Distillation

Design and Analysis factors:

Factors that influence the design or analysis of a binary- distillation operation
include:

1. Feed flow rate, composition, temperature, pressure, and phase condition.

2. Desired degree of component separation.
3. Operating pressure (which must be below the critical pressure of the
mixture).
4. Pressure drop, particularly for vacuum operation.
 34

5. Minimum reflux ratio and actual reflux ratio.

6. Minimum number of equilibrium stages and actual number of equilibrium
stages (stage efficiency).
7. Type of condenser
8. Degree of liquid reflux sub cooling
9. Type of reboiler
10.Type of trays or packing
11.Column height
12.Feed-entry stage
13.Column diameter
14.Column internals, and material of construction
15.Heat lability and chemical reactivity of feed components

McCabe-Thiele Method:
It is a graphical method and involves calculation of total number of equilibrium
stages required for a given separation using material balance and equilibrium
relations.

It uses the fact that the composition at each theoretical tray (or equilibrium stage)
is completely determined by the mole fraction of one of the two components and
is based on the assumption of constant molar overflow which requires that:

1. The molar heats of vaporization of the components are equal.

2. For every mole of liquid vaporized, a mole of vapor is condensed.
3. Heat effects such as heats of solution are negligible.

McCabe-Thiele method assumes that the liquid on each tray is in equilibrium with
the vapor phase above each corresponding tray.

The following notations shall be used:

 35

Y: mole fraction of more volatile component in vapor phase

X: mole fraction of more volatile component in liquid phase

V: molar flow rate of vapor, mole/time

L: molar flow rate of liquid, mole/time

F: molar flow rate of feed (vapor or liquid or mixed), mole/time

Steps involved in determining the number of theoretical stages:

1. Analysis of the Rectifying section, and determine the ROL using XD and R.
2. Analysis of the feed section, and determine the feed condition Q.
3. Determination of the feed line (q line) using XF and q.
4. Locate the intersection point between ROL and q-line.
5. Analysis of the stripping section, and determine the SOL using (4) and XB.
6. Draw triangles between the equilibrium curve and ROL, SOL, starting from
the point XD up to the on or crossing of the point XB on the diagonal line.

OPERATING LINE EQUATIONS:

1. ROL:
' (
Yn+1 = Xn + XD
' ( ' (
2. q-line:
)* (
Y=- X+ XF
()* ()*
3. SOL:
+,
Y=- X+ XB
+,) +,)

DESIGN PROBLEM:
A continuous fractionating column is to be designed for separating 10,000 kg per
hour of a liquid mixture containing 40 mole percent methanol and 60 mole
 36

percent in to an overhead product containing 97 mole percent methanol and a

bottom product having 98 mole percent water. A mole reflux ratio of 3 is used.
Calculate (i) moles of overhead product obtained per hour and (ii) number of ideal
plates and location of feed plate if the feed is at its bubble point.

Equilibrium data:

X: 0 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.0

Y: 0 0.417 0.579 0.669 0.729 0.78 0.825 0.871 0.915 0.959 1.0

Where X = mole fraction of methanol in liquid

Y = mole fraction of methanol in vapor

DATA:

Feed rate = 10,000 kg/hr

R=3

q = 1 (feed is at its bubble point)

XF = 0.4

XD = 0.97

XB = 1- 0.98= 0.02

Calculations:

Average molecular weight of feed = o.4 x 32 + 0.6 x 18 = 23.6

Molar flow rate of feed = 10000/23.6 = 423.73 kmol/hr

Overall Material balance:

F=D+B

423.73 = D + B
 37

Component balance for methanol:

F x XF = D x XD + B x XB

423.73 x 0.4 = D x 0.97 + (423.73 D) x 0.02

D = 169.4256 Kmol/hr

B=FD

= 423.73 169.4256

= 254.3044 kmol/hr

ROL:
(
Intercept = XD
' (

(
= x 0.97
- (

=0.2425

q=1

q-Line passes through the point (0.4,0.4) on the diagonal line parallel to the Y-axis
and meet the ROL line at (0.4,0.5425).

ROL, q line are plotted on the Y vs. X graph and SOL line is from the point XB on
the diagonal line through the intersection point of the ROL and q line.
 38

From the above graph we can get the total number of ideal stages = 7 and
the feed is given at 5th stage.
 39

DISTILLATION COLUMN INTERNALS

Distillation columns are made up of several components, each of which is used

either to transfer heat energy or enhance mass transfer. A typical distillation
contains several major components:

1. A vertical shell where the separation of liquid

components is carried out

2. Column internals such as trays/plates /

packings which are used to enhance component
separations

3.A reboiler to provide the necessary

vaporization for the distillation process

4. A condenser to cool and condense the

vapour leaving the top of the column

5. A reflux tank to hold condensed vapour

from top of the column a so that liquid can
be refluxed it back to the column

DISTILLATION COLUMN INTERNALS

Typical internal accessories include trays, packing, liquid distributors,

redistributors, collectors, bed limiters, mist eliminators.

TYPES OF VAPOUR-LIQUID CONTACT EQUIPMENT

 40

I.TRAYS
II.PACKINGS

Trays and packing are installed in the column for efficient vapour liquid contact.

I.TRAYS:
The function of a Tray is to felicitate contact between the vapour phase and liquid
phase, so that mass transfer between the two phases can take place.
The geometry of the tray within the column will affect extent of contact between
vapour and liquid streams.
Each tray is considered as being made up of 3 sectons:
1. Weir
2. Bubbling area
3. Downcomer

Each tray has 2 conduits, one on each side, called downcomers. Liquid falls
through the downcomers by gravity from one tray to the one below it.

A weir on the tray ensures that there is always some liquid (holdup) on the
tray and is designed such that the holdup is at a suitable height, e.g. such
that the bubble caps are covered by liquid.

In bubbling area, vapour-liquid contact takes place.

Being lighter, vapour flows up the column and is forced to pass through the liquid,
via the openings on each tray, forming a foaming, turbulent mixture. During this
foaming process , a high interfacial area for efficient vapour liquid mass transfer is
 41

produced.. The area allowed for the passage of vapour on each tray is called the
active tray area.

1. SIEVE TRAY:

Material of construction: Stainless steel, Duplex, Monel, Titanium, Hastelloy or

any metal or alloy.

Sieve trays are simply metal plates with holes in them. Vapour passes straight
upward through the liquid on the plate. The arrangement, number and size of
the holes are design parameters.

Application:
Low cost, used when high turn down ratios are not required.

2. VALVE TRAYS:

Valve trays contain holes with opening and closing

Valves and have tendency to experience fouling
due to accumulation of material.
 42

a) FIXED VALVE TRAY:

The V-Grid tray technology utilizes a fixed valve and

combines the attributes of sieve and float valve trays.
The tapered, rectangular valves are formed out of the
tray deck and are oriented parallel to the liquid flow,
thus providing unique advantages compared to
traditional sieve trays.

Benefits:
Lower froth height, less entrainment due to lateral vapour release
Increased capacity and improved turn down ratio when compared to
sieve trays
Excellent fouling resistance

b) FLOATING VALVE TRAY

In floating valve trays, perforations are covered by liftable caps. Vapour

flows lifts the caps, thus self creating a flow area for the passage of vapour.
The lifting cap directs the vapour to flow horizontally into the liquid, thus
providing better contact than is possible in sieve trays.
 43

Applications:
Floating valve trays are used in applications where higher turndown
ratios are required.
No liquid flow under the valves
Minimized weeping due to lateral vapour release

c) BUBBLE CAP TRAYS

A bubble cap tray has riser or chimney fitted over each hole, and a cap that
covers the riser. The cap is mounted so that there is a space between riser
and cap to allow the passage of vapour. Vapour rises through the chimney
and is directed downward by the cap, finally discharging through slots in
the cap, and finally bubbling through the liquid on the tray.
 44

Applications:

Used for low liquid loads and higher turn down ratios.

COMPARISION OF BUBBLE CAP, SIEVE, VALVE TRAYS:

Principle factors:
1. Cost:

Bubble caps are appreciably more expensive than sieve or valve trays.
Due to its simple design, sieve trays are normally the cheapest.

2. Operating range:

It refers to the range of vapour and liquid rates over which the tray will
operate satisfactorily.

TURNDOWN RATIO: the ratio of the highest to the lowest flow rate is called
the Turndown ratio.

Bubble cap trays can operate efficiently at very low vapour rates.
Sieve trays cannot operate at very low vapour rates.
Valve trays are intended to give greater flexibility than sieve trays at a
lower cost than bubble cap.
 45

3. PRESSURE DROP:

Sieve tray has lowest pressure drop, followed by valve and bubble caps
giving the highest.

4. MAINTENANCE:

Bubble caps are not suitable for dirty services as they may be susceptible to
plugging.
Sieve trays are easiest to clean.
Valve trays should be considered, if the specified turndown ratio cant be
maintained with sieve trays.

II.PACKINGS:

The type of packing material in industrial use can be distinguished into structured
packing (also called as stacked or arranged) and random packing (also called
dumped).

A good packing material is one that provides a high surface area per volume since
mass transfer takes place between liquid layer forming on the packing element
surface and gas going through the packing elements.

The material of construction must provide a high liquid flow capacity through it to
ensure a uniform liquid layer (good wettability) as well as good resistance to
pressure (high strength).

Pressure drop should be desirably low.

A) STRUCTURED PACKING:

Structured Packings, made from thin-gauge sheets or woven wire mesh to

give a regular pre-formed shape, provide high surface area with high void fraction
to promote efficient vapour-liquid contacting in mass-transfer operations.
 46

Structured packings require much less height of column with lower pressure drop
compared to random packings or trays.

Structured Packings are of three types:

1. Structured packing made of wire mesh
2. Structured packing made of sheet metal
3. Structured grid Packing

WIRE MESH (STRUCTURED PACKING):

Material of Construction: Stainless Steel, Carbon Steel,

Phosphor bronze or any metal/alloy
Sizes: 25mm to 3 m diameter.
Surface area: 500 to 750 m/m.
NTSM: 1 to 4.5
Application:
Typically used for fine chemicals when fouling is not a concern.
Can be used at high vacuum to low pressure.
Good for low pressure drop.
Wire mesh is often used in vacuum distillation where liquid flow rate
is low and minimizing pressure drop is essential.

SHEET METAL (STRUCTURED PACKING):

Material of Construction: Stainless Steel, Duplex, Titanium,

Hastelloy.
Sizes: 50mm to 8 m diameter.
Surface area: 60 to 1000 m/m.
NTSM: 1.2 to 3.5
Application:
Can be used at moderate vacuum to high pressure, low to high liquid
loading.
 47

Can be used at low pressure drop vacuum distillation services to

medium, high pressure drop absorbers.

STRUCTURED GRID PACKING:

Grids are developed for severe services that are susceptible to fouling, erosion,
coking, and high solids content. Grids are installed in rigid modules stacked in
successive layers with a fixed orientation, thus minimizing the overall pressure
drop while simultaneously increasing tower efficiency.

Material of Construction: Stainless Steel, Carbon steel, Duplex, Monel, Hastelloy.

Sheet thickness: 1 to 2 mm.
Application:
Provides extended operations in fouling systems, corrosive environment
and where frequent cleaning is required.

There are two types of structured grid packings:

Corrugated sheet metal
Stamped blades

Corrugated sheet metal:

Corrugated Grid Packing combines the high surface

area of traditional structured packing with the rugged
construction of the common grid configuration, to
provide high heat transfer efficiency, high mechanical
strength and antifouling characteristics in severe
services that are prone to plugging, coking, erosion
and containing solids.

The smooth surface provides low liquid hold up reducing the residence time and
the possibility of coke formation.
 48

APPLICATIONS
Coker fractionators wash section
Atmospheric Crude Unit wash section
Crude Vacuum Unit was section
Reactor Off Gas Scrubbers
Flue Gas Scrubbers

Stamped blades: Bladed grid packing achieves its mass

transfer and heat transfer capability by creating a
tortuous path for vapour and liquid streams.

a) RANDOM PACKING :

Random packings are small objects made from metals, polymers, ceramics
are dumped into the column.

Random packings have low pressure drop when compared to tray columns.

Random packings are made of

Metal
Ceramic
Plastic

Metal: Good wettability and high strength.

Ceramic:
Ceramic elements are used when corrosive chemicals are involved and good
wettability is required.

Plastic:
Usually polypropylene is largely used because of low cost but fail at high
temperature and it also has poor wettability.
 49

Different types of random packings:

Cylindrical rings:

Material of construction: Stainless steel or any metal or alloy.

Bulk density: 200-900 kg/m.
Surface area: 90-600 m/m.
NTSM: 1.5 1.8
Application:
High mechanical strength

P-Rings:

Material of construction: Stainless steel or any metal or alloy.

Bulk density: 220-350kg/m.
Surface area: 120-500 m/m.
NTSM: 1.8-2.2
Application:
Good capacity and lower pressure drop
Higher liquid hold-up and residence time

C-Rings:

Material of construction: Stainless steel or any metal or alloy.

Bulk density: 150-250kg/m.
Surface area: 110-220 m/m.
NTSM: 2.2-2.5
Application:
Good capacity and lower pressure drop
Low liquid hold-up, High throughput, Good liquid
distribution
 50

Saddle-Rings:

Material of construction: Stainless steel or any metal or alloy.

Bulk density: 120-330kg/m.
Surface area: 60-280 m/m.
NTSM: 2.2-2.5
Application:
Good capacity and lower pressure drop
Low liquid hold-up, High throughput

N-Rings:
Material of construction: Stainless steel or any metal or alloy.
Bulk density: 130-180 kg/m.
Surface area: 150-220 m/m.
NTSM: 1.2-2.5
Application:
Very low pressure drop, suits high vacuum conditions, very low-liquid hold-up.

HP-Rings:

Material of construction: Stainless steel or any metal or alloy.

Bulk density: 190-280 kg/m.
Surface area: 90-270 m/m.
NTSM: 1.8-2.2
Application:
Higher capacity and lower pressure drop than pall
rings
Similar efficiency compared to pall rings.
High mechanical strength than pall rings
 51

STRUCTURED PACKING Vs. RANDOM PACKING:

STRUCTURED PACKING RANDOM PACKING

1. More expensive but very
efficient.
2. Useful for times when we dont
have a lot of pressure drop to
play with .e.g ; vacuum service.
3. For fouling liquid, it is
impossible to clean and often
difficult to even get out of the
column.
4. It has more number of stages
per packed height, which
reduces the total height of the
column required, thus reducing
the cost of material in
construction.
Cheap and relatively efficient.
Used if the packing is a consumable/
wearable packing that needs replacing
regularly.
Can be used for fouling liquids.
It is cheaper, but will contain voids
which may reduce structural
performance. Also it has less number
of stages per packed height, thus
increasing the height of the column.

Advantages of structured packing over Random packing:

1. Lower pressure drop
2. Higher efficiency for the same tower height
3. Reduced liquid hold-up
4. Lower resistance to vapour flow and efficient use at available surface area.

Disadvantages:
1. Higher cost
2. Greater sensitivity to maldistribution

LIQUID DISTRIBUTORS AND REDISTRIBUTORS:

Packing whether random or structured, serves the basic purpose of providing

intimate contact between vapour and liquid in mass transfer operations. But for
effective and efficient performance of packing some peripherals are needed.
 52

Liquid distributors serve the purpose of distributing liquid evenly over the
packing.

1. CHANNEL TYPE DISTRIBUTOR

Channel type distributor is one of the regularly used types for structured
packing.

Size: Diameter up to 800mm can be manufactured in single segment and

can be manufactured with top trough up to 2 m diameter in segmented
pattern.

2. BAFFLE TYPE DISTRIBUTOR:

These distributors are provided with holes at certain level on side wall of
the channels and are fitted with baffle plates. This construction helps to
distribute liquid flow evenly, helps to distribute liquid flow evenly, helps to
cover more surface area even for low liquid flow rates.

Size: Available from diameter of 700 mm onwards.

3. SPIRAL TYPE DISTRIBUTOR:

 53

Construction of this distributor resembles the construction of channel

tube type distributor. Channelized construction is applied with holes on the side
wall where it is covered with spiral tube.
Such construction helps to apply for viscous and severely plugging application.

4. CHIMNEY TRAY TYPE DISTRIBUTOR:

Chimney tray distributors are applicable for high liquid loads and higher diameter
columns
Features of this distributor it helps to work as a distributor and re-distributor.

5. SPRAY NOZZLE TYPE DISTRIBUTOR:

The spray nozzle type distributor has cone spray nozzles instead of
distribution holes for homogeneous distribution of liquid.
This type has an advantage that liquids containing solid particles can be
distributed without plugging problems to the nozzles.
The Spray type nozzle distributor consists of a main header and laterals with
downpipes and spray nozzles.
 54

6. PIPE TYPE DISTRIBUTOR:

Pipe type distributors can be efficiently used where vapour flow rate is high as
pipe construction provides large area for vapour flow.

7. SPIDER TYPE DISTRIBUTOR:

It resembles channel type distributor, used when low liquid flow rates are
required. The purpose of this type construction is to cover maximum surface area
even at very low liquid flow rates.
The low liquid load can be possible by spider type tube arrangement at the
bottom.
 55

8. PAN TYPE DISTRIBUTOR:

Pan type distributor provides liquid hold up for very low liquid loads. Vapour
passes through a circular or rectangular gas riser. Distributors can be used even
from as low as 100mm and 800mm column diameter with pan.

Application: These can be largely used in random packings.

9. TROUGH TYPE DISTRIBUTOR:

Trough type distributor can be used for high liquid load and high column
diameter.
Both bottom hole construction and tube construction is possible in trough type
distributor. Top trough distributes the liquid in the bottom channels which equally
distributes the liquid on the surface of the packing.

Application: Can be used for both random and structured packing.

 56

LIQUID COLLECTORS:

1. VANE TYPE COLLECTORS:

Also known as ring type collectors these collectors have lower pressure drop.

2. COLLECTORS WITH SUPPORT GRID:

This is a combination of packing support grid and vane type collector.

3. FLANGED TYPE COLLECTORS:

These are used for comparatively small diameter columns.

4. CHIMNEY TRAY TYPE COLLECTORS:

These are normally used for large diameter columns with high liquid throughput.
 57

PACKING SUPPORTS:

These are used to support the packing placed above them. These should have a
high percentage of open area to allow unrestricted counter flow of liquid and
vapour.

For large and heavy duty column

For large columns and heavy duty distillation columns, the static weight of packed
bed combined with liquid column is quite high. Strong construction of packing
support is needed.

Multi beam support used for random packing.

For random packing which are dumped on the support plate, the weight per unit
cross section area is high. Therefore comparatively stronger construction is
needed.
Random packings use a gas-injection support that provides separate passages for
liquid and vapour flow, so that two phases do not compete for the same opening.
Incorrectly designed gas injection support plates can limit the column capacity
rather than the random packing limiting the column capacity.
 58

Support grid used for structured packing.

Structured packings allow support by a simple open-grid structure.
Very construction is needed to support the structured packing as the weight per
unit cross-section of a structured packing is high.

BED LIMITERS:
Bed limiters are installed directly above a packed bed in a distillation column to
prevent shifting of packing elements under turbulent conditions of vapour and
liquid.
 59

MIST ELIMINATORS:

Mist eliminator which helps n separation of liquid droplets from gas stream which
provide suitable foaming system with higher liquid loading.

1. WIRE TYPE MIST ELIMINATORS

(Knitted mesh type, High efficiency mesh type)

Mesh type devices typically consist of pad of knitted wire supported by a

framework.
They function as a mist eliminator because impingement of liquid droplets
to coalesce and subsequently disengage from wire surface under gravity.
These can be utilized in both horizontal and vertical configuration in
separator.
Offer high gas/liquid separator efficiency, low installed cost and low
pressure drop.
 60

2. VANE TYPE
(Hook type, Pocketed vane type, Plain vane type)
Used when fouling and blockage are possible.
Used where a relatively low efficiency is acceptable.
These kinds of mist eliminators can be used where higher pressure drop is
allowed.
 61

PUSHER CENTRIFUGE
INTRODUCTION:
A pusher centrifuge is a type of filtration technique that offers continuous
operation to de-water and wash materials such as relatively in-compressible feed
solids, free-draining crystalline, polymers and fibrous substances. It consists of a
constant speed rotor and is fixed to one of several baskets. This assembly is
applied with centrifugal force that is generated mechanically for smaller units and
hydraulically for larger units to enable separation.

Pusher centrifuge can be used for a variety of applications. They are typically used
in inorganic industries and later, extensively in chemical industries such as organic
intermediates, plastics, food processing and rocket fuels.

WORKING:
A suspension feed enters the process to undergo pre-acceleration and
distribution. The subsequent processes involve main filtration and intermediate
de-watering, after which the main filtrate is collected. Wash liquid enters the
washing step and final de-watering follows. Wash filtrate is extracted from these
two stages. The final step involves discharge of solids which are then collected as
the finishing product. These process steps take place simultaneously in different
parts of the centrifuge.

It is widely accepted due to its ease of modification, such as gas-tight and

explosion.
 62

OPERATION:
The slurry is feed through a stationary feed pipe at the centerline of the pusher
basket. The slurry is accelerated in the rotating feed funnel and distributed
uniformly at the back of the rotating screen. This feed funnel is anchored to the
pusher plate. The feed funnel gently accelerates the slurry in to the basket speed
in order to form an even cake and minimize particle attrition.

As the pusher plate moves in to its back position, a clean wedge slot screen
surface is exposed. The accelerated slurry is deposited on the wedge slot screen,
and cake is built as the mother liquor drains through the basket. Then, the pusher
plate moves forward and pushes the cake forward, towards the solids discharge
end. During this time, the incoming feed is held in thee feed funnel, until the
pusher plate moves backward and exposes fresh screen for another annular ring
of cake to be built. The reciprocation of the pusher plate causes cake to progress
towards the solids discharge end. The cake, which is under centrifugal force,
becomes drier as it progresses in the basket and ultimately is discharged from the
pusher basket in to the solids discharge housing.
 63

ADVANTAGES:
1. It offers higher processing capacities than batch filtering centrifuges such as
vertical basket and inverting filter.
2. Provides the best washing characteristics of any continuous centrifuge due
to control of retention time and uniform cake.
3. Gentle handling makes pusher better suited for fragile crystals.

LIMITATIONS:
1. Pushers require a constant feed flood due to their continuous nature.
2. Although high capacities may be preferred, this may result in longer
residence time.
3. Typical particle sizes must be at least 150 micrometer and average 200
micrometer.
4. A high viscosity feed lowers throughput.
5. Pushers have a limited liquid filtration capacity and requires fast-draining
materials, since it must form a cake within the period of one stroke.

APPLICATIONS:
1. Production of sodium chloride as common salt.
2. Production of organic intermediates include paraxylene, adipic acid, oxalic
acid caprolectum, nitrocellulose, carboxymethylcellulose, etc.
3. In food processing, pusher centrifugation is used to produce monosodium
glutamate, salt, lysine, and saccharin.
4. In plastic industry, for the production of PVC, polyethylene and a number of
other resins.
5. Individual products include soda ash, sodium carbonate, paraxylene, Adipic
acid, cotton seed delinting.
 64

MIXING TECHNOLOGY

STATIC MIXER:
A static mixer is a precision engineered device for the continuous mixing of fluid
materials. Normally the fluids to be mixed are liquid, but static mixers can also be
used to mix gas streams, disperse gas into liquid or blend immiscible liquids. The
energy needed for mixing comes from a loss in pressure as fluid flows through the
static mixer.

One design of static mixer is the plate-type mixer and another common device
type consists of mixer elements contained in a cylindrical (tube) or squared
housing. Mixer size can vary from about 6 mm to 6 meters diameter.

Typical construction materials for static mixer components included stainless

steel, polypropylene, Teflon, PVDF, PVC, CPVC, and polyacetal.
 65

OPERATION:
In the plate type design, mixing is accomplished through intense turbulence in the
flow.

In the housed-elements design, the static mixer elements, consists of a series of

baffles made of metal or a variety of plastics. Similarly, the mixer housing can be
made of metal or plastic. The housed-elements design incorporates a method for
delivering two streams of fluids into the static mixer. As the streams move
through the mixer, the non-moving elements continuously blend the materials.
Complete mixing depends on many variables including the fluids properties, tube
inner diameter, number of elements and their design. The housed-elements
mixers fixed, typically helical elements can simultaneously produce patterns of
flow division and radial mixing.

FLOW DIVISION:

In laminar flow, a processed material divides at the leading edge of each element
of the mixer and follows the channels created by the element shape. At each
succeeding element, the two channels are divided, resulting in an exponential
 66

increase in stratification. The number of str iations produced is 2n where n is the

striations
number of elements in the mixer.

RADIAL MIXING:

In either turbulent flow or laminar flow, rotational circulation of a processed

material around its own hydraulic center in each channel of the mixer causes
radial mixing
ng of the material. Processed material is intermixed to reduce or
eliminate radial gradients in temperature, velocity and material composition.

APPLICATIONS:
1. In Mixing two-component
component adhesives (e.g., epoxy) and sealants.
2. In Waste water treatment and chemical processing.
3. In bitumen processing and desalting crude oil in the refineries.
4. In polymer industries to facilitate polymerization reactions or for the
admixing of liquid additives.
 67

SHEAR MIXER:
A shear mixer disperses, or transports, one phase or ingredients (liquid, solid, gas)
into a main continuous phase (liquid), with which it would normally be
immiscible. A rotor or impeller, together with a stationary component known as a
stator, or an array of rotors and stators, is used either in a tank containing the
solution to be mixed, or in a pipe through which the solution passes, to create
shear. A high-shear mixer can be used to create emulsions, suspensions, lyosols
(gas dispersed in liquid), and granular products. It is used in the adhesives,
chemical, cosmetic, food, pharmaceuticals, and plastic industries for
emulsification, homogenization, particle size reduction, and dispersion.

PRINCLIPLE OF WORKING:
Fluid undergoes shear when one area of fluid travels with a different velocity
relative to an adjacent area. A high-shear mixer uses a rotating impeller or high-
speed rotor, or a series of such impellers or inline rotors, usually powered by an
electric motor, to work the fluid, creating flow and shear. The tip velocity, or
speed of the fluid at the outside diameter of the rotor, will be higher than the
velocity at the center of the rotor, and it is this velocity difference that creates
shear.

A stationary component may be used in combination with the rotor, and is

referred as the stator. The stator creates a close-clearance gap between the rotor
and itself and forms an extremely high-shear zone for the material as it exits the
 68

rotor. The rotor and stator combined together are often referred to as the mixing
head, or generator.

The mixer has a separate chamber at the bottom through which the mixing
ingredients are drawn in. the high speed rotating head pushes the ingredients
through specially designed perforated head at a very high velocity. This helps the
fluid to break into small particles which flow through the peripheral cavity to the
top. The fluid is kept in suspension in the chamber by rotating blades and flows
out through the top nozzles.

OPERATION:
Shear mixer works on the principle of drawing the materials through the specially
designed mixing head and shearing this through another specially designed
rotating assembly.

The different steps involved in the mixing process are:

Stage 1:

The high-speed rotation of the impeller draws material through the suction of the
mixing vessel.

Stage 2:

Centrifugal force drives material towards the periphery of the impeller where it is
subjected to a milling action in the clearance between the ends of the impeller
blades and the stator head.
 69

Stage 3:

This is followed by intense shearing of the material which is forced, at high

velocity, out through the perforations in the stator head.

Stage 4:

The material expelled from the head flows up at high speed towards the sides of
the mixing vessel. The impellers at the top of the mixing head keep the material in
the suspension.
 70

Equilibrium mixing:

High-shear mixers are used in industry to produce standard mixtures of

ingredients that do not naturally mix. When the total fluid is composed of two or
more liquids, the final result is an emulsion; when composed of a solid and a
liquid, it is termed a suspension and when a gas is dispersed throughout a liquid,
the result is a lyosol. Each class may or may not be homogenized, depending on
the amount of input energy.

To achieve a standard mix, the technique of equilibrium mixing is used. A target

characteristic is identified, such that once the mixed product has acquired that
characteristic, it will not change significantly thereafter, no matter how long the
product is processed. For dispersions, this is the equilibrium particle size. For
emulsions, it is the equilibrium droplet size. The amount of mixing required to
achieve equilibrium mixing is measured in tank turnover- the number of times the
volume of material must pass through the high-shear zone.

APPLICATIONS:
Shear mixers are used throughout the chemical process industries, wherever it is
necessary to produce standardized mixtures of ingredients that do not naturally
mix. These include:

1. Pharmaceuticals, preparation of suspensions and granular products.

2. Paper manufacture, bleaching and preparation of paper pulp.
3. Food preparation, emulsion for condiments, sauces and dressings.
4. Manufacture of cosmetics.
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