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Internship Report

ICI Soda Ash

Submitted To: Engr. Adnan Sarwar


Submitted By: M. Khubaib Asadi
Reg. No: FA16-CHE-017
Date: 04-09-2019

CHEMICAL ENGINEERING DEPARTMENT


COMSATS University Islamabad,
Lahore Campus

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Abstract

Soda ash is very necessary in the manufacturing of necessary materials such as glass,
paper and detergents. And ICI soda ash khewra plant produces almost 1200 tons of soda ash per
day using Solvay process and then convert a part of this light soda ash into dense ash and also in
refined sodium bicarbonate. In the production process, slat coming from khewra salt mine is used
for brine production. Then brine goes into ammonia absorber where vat liquor is formed which
then goes to mono-carbonating tower, where, by addition of CO2 in vat liquor, (NH3)2CO3 is
formed. The product of MCT is called carbonated vat liquor. Then, the carbonated vat liquor goes
to carbonating tower where CO2 react with carbonated vat liquor and crystals of sodium
bicarbonate are formed. The product of carbonating tower is called magma which is then sent to
rotary drum filter. After filter, cake of sodium bicarbonate is sent to calciner where light soda ash
is formed and sent to Asher house. And the remaining liquid from filter is called feeder liquor.
The feeder liquor is sent to ammonia recovery units consist on a distiller, two prelimers, cassie
cooler etc. The plant also has its own power generation unit where circulation fluidized bed
boilers are used to produce steam which is then used for power generation and also inside the
plant like in prelimers, distillers etc.

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Table of Contents
1. Introduction .........................................................................................................................................................4
2. HSE Training: .....................................................................................................................................................4
3. Raw Materials .....................................................................................................................................................5
4. Basin & Brine purification .................................................................................................................................6
5. Kiln .......................................................................................................................................................................7
6. Absorber ..............................................................................................................................................................7
7. Mono-Carbonating Tower .................................................................................................................................8
8. Carbonating Tower .............................................................................................................................................9
9. Rotary Filter ........................................................................................................................................................9
10. Calciner ......................................................................................................................................................... 10
11. Ammonia Recovery Section ......................................................................................................................... 10
12. Refined Sodium Bicarbonate Plant ............................................................................................................. 11
13. Dense Ash Plant ............................................................................................................................................ 11
14. Main Products ............................................................................................................................................... 11

List of Figures

Figure 1: PFD of Brine Purification Plant .................................................................................................................6


Figure 2:PFD of Kiln ...................................................................................................................................................7
Figure 3: Absorber Tower ..........................................................................................................................................8
Figure 4: Mono-Carbonating Tower PFD .................................................................................................................8
Figure 5: Rotary Filter Flow Diagram .......................................................................................................................9
Figure 6: Calciner PFD ............................................................................................................................................. 10

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1. Introduction
ICI Pakistan Limited’s Soda Ash plant can trace its roots back to 1929, when the
construction of the plant began, and 1944 when soda ash commercial production first commenced.
Through various expansion projects, the plant’s original capacity of 18,000 tons per annum has increased
to 425,000 tons, and by 2020, ICI expect it to become a half million-ton site. The Business diversified its
product range in 1950 and 1995 with the installation of dense ash and refined sodium bicarbonate plants,
respectively.
As production capabilities have evolved, so have the various markets and applications for soda ash. Today,
soda ash consistently ranks as one of the top ten inorganic chemicals produced in the world and is an
essential raw material to a variety of industries.
Soda Ash is used as a builder or filler in the formulation of soaps, detergents, and other cleaning
compounds. In the glass industry it is used to bring down the melting temperature of silica sand (the main
raw material of glass). In the paper industry, soda ash is used in the preparation of the sodium sulphite
buffer liquid used in the pulp manufacturing process. Soda ash even finds an application in the water
treatment segment, by adjusting the pH of water when it is acidic.
ICI Pakistan Limited’s Soda Ash Business caters to approximately 70% of the country’s total requirement
for this commodity. Pakistan’s domestic consumers of soda ash rely upon ICI Pakistan Limited as a trusted
and reliable supplier for high quality soda ash. ICI utilize indigenous raw materials to ensure substantial
foreign exchange savings through import substitution. Soda ash produced at our Khewra plant is now
regularly exported, earning valuable revenue for the national exchequer.
ICI Pakistan Limited has invested heavily in its production facilities and will continue to do so to retain its
competitive advantage. These initiatives include; two additional coal fired boilers; an 18 megawatt (MW)
steam turbine; the expansion of the refined sodium bicarbonate plant to a capacity of 40 kilotons per
annum (KTPA); and the expansion of the dense ash plant to a capacity of 140 KTPA with a further expected
expansion of 70 KTPA in the year 2020.
This report will cover the general process and working of equipment using in each section
of plant:

2. HSE Training:

Health (H), Safety (S) and Environment (E) (together HSE) is a discipline and specialty that studies
and implements practical aspects of environmental protection and safety at work. In simple terms it is
what organizations must do to make sure that their activities do not cause harm to anyone.
Better health at its heart, should have the development of safe, high quality, and environmentally friendly
processes, working practices and systemic activities that prevent or reduce the risk of harm to people in
general, operators, or patients.
From a safety standpoint, it involves creating organized efforts and procedures for identifying workplace
hazards and reducing accidents and exposure to harmful situations and substances. It also includes

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training of personnel in accident prevention, accident response, emergency preparedness, and use of
protective clothing and equipment.
From an environmental standpoint, it involves creating a systematic approach to complying with
environmental regulations, such as managing waste or air emissions all the way to helping sites reduce the
company's carbon footprint.

In the HSE training, we learned about the risks and health hazards, their types and the prevention from
these risks, importance of PPEs. We learned enough about the safety that we were now able to proceed to
the plant for our training.
At ICI Pakistan Limited our HSE&S Policy makes us responsible for:
• Protecting the Health and Safety of employees, contractors, customers and neighbors.
• Maintaining the security of people and assets.
• Protecting the environment. Will work in close cooperation with customers, suppliers and
distributors to;
• Comply with all relevant laws and regulatory requirements.
• Ensure that all activities are conducted in a manner consistent with ICI Pakistan Limited Health,
Safety, Environment and Security Standards and Guidelines.
• Ensure that business activities are conducted to prevent harm to customers, employees,
contractors and public, other stakeholders and the environment.
• Develop, manufacture and market products with full regards of HSE&S aspects, ensure
compliance with the ICI Pakistan Limited Product Stewardship Management System and sell
only those products that can be transported, stored, used disposed off safely.
• Protect people, assets, intellectual property and critical information from accidental or deliberate
harm, damage or loss.
• Openly communicate on the nature of activities, encourage dialogue and report progress on
health, safety and environmental performance.
• Regularly monitor the application of this Policy.

3. Raw Materials
▪ Limestone: -
It is abundantly available from limestone rocks. Small quantities of limestone, known as gorge
stone, are collected from the gorge area. Apart from the gorge area, ICI also owns two quarries, Dandot
and Tobar.

▪ Coke: -
Coke is an expensive raw material used to generate CO2 gas for the process. It is mainly coming
from Poland.

▪ Ammonia: -
Ammonia is obtained from fertilizer plants and it is also recovered from in the distiller.

▪ Salt: -
Salt, NaCl, is found in abundance in the mountain ranges surrounding Khewra. Its main supplier
is Pakistan Mineral Development Corporation.
▪ Others: -
• Water
• Coal

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4. Basin & Brine purification
The basin is the part of plant where the raw brine is made. In basin, there are four stocks which are
used in the formation of brine. First of all, water from water reservoir is showered on piles of salt (coming
from khewra salt mine) and then this salt mixed water goes into sea sump stock by passing through settler
where mud is settled down. From sea sum tank, it is then showered on another pile of salt using pump and
stored in primary stock by passing through settler. And then, it is again showered on slat piles and stored
in dissolving cell by passing through settler and then goes to brine purification section. The raw brine
coming from basin should have a test of almost 105.6mls N/20mls.
Sources of Salt:
• PMDC – Main Mine, Makrach.
• Malik Khadim – Pir Dakhara.
• Punjab Mine – Jotanna, Waralar.
• ICI – Matin.
Types of salts:
• Rock Salt – 95% NaCl
• Potash – 70% NaCl
• Khallar 75-80% NaCl
The salt which is passed for the process
must have 90% NaCl otherwise it is
rejected.

Crude brine coming from basin is not


enough pure for use in the process as it
contains calcium and magnesium salts
and frequently potassium salts, sodium
sulphate and iron compounds. These
impurities are precipitated out of the
brine solution, so they do not scale the
equipment. In brine purification plant,
all the alkaline earth impurities are
removed by milk of lime and soda ash
treatment.
In brine purification plant, Figure 1: PFD of Brine Purification Plant
crude brine is dissolved in a reaction
vessel with milk of lime and then sent to a time vessel so that complete mixing of mol and brine takes
place. And then it is sent towards primary settler for complete settling of red precipitates of magnesium
hydroxide. And then it goes to Ash mixing tank where brine mixes with ash and then goes to final settler
for settling of red and white precipitates of sodium and calcium carbonate respectively. The drain of
reaction vessel, primary settler and final settler goes to a decanter from where some brine is recovered,
and the sludge goes to calcium carbonate plant. (As see in fig.). After brine purification section, the brine
should have a test of almost 104.4 mls N/20mls.

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5. Kiln
The main purpose of kiln is to produce lime which is used to make milk of lime (MOL),
and also kiln produces CO2 which is used in the
process. Inside the kiln, CO2 is produced when coal
combustion takes place and also by decomposition of
limestone. The top product of kiln is almost 42% CO2
and bottom product consist of unburnt limestone, lime
and grit (impurities like sand etc.).
In kiln process, first of all, limestone and coke
are stored in their respective two hopper through
conveyer. In the charging of feed into the kiln, there are
two plate feeder feed the coke in a weight tank and then
wind loss take it from weight tank and feed it into kiln
or in some old kilns, the feed is distributed in kiln by a
Hannon flask and air is fed by forced draft fan. The
exiting kiln gas goes to kiln gas scrubber where it is
scrubbed with water and then sent to plant. And at
bottom of kiln, a rotary lock is used to remove bottom
products of kiln. Rotary lock draws the products on
buckets elevator which then takes the products to Lime
Bunker where it is stored and send to MOL Dissolver
Figure 2:PFD of Kiln
which is a revolving (a little bit inclined for movement
of materials) drum in hot water is showered to dissolve
lime (CaO). There is also a sieve inside MOL Dissolver by which grit and lime passes and goes to next
MOL dissolver and back stone is removes and sent back to limestone stock. And in the next MOL
Dissolver the grit is also removed and sent to dump yard. The remaining lime is then sent to MOL stock
Tank from which it goes to plant where it requires.

6. Absorber
Absorber is a very important unit of plant. The objective of absorber is the absorption of ammonia into
brine as ammonia is act like an intermediate catalyst or an activator in the carbonization of brine in
carbonating tower. In absorber following reactions takes place:
NaCl.H2O + NH3 NaCl.NH4OH
(Brine) (Ammoniated Brine)
Traces of CO2 causes following reaction:
2NH4OH + CO2 (NH4)2CO3 + H2
The combined product of above two reactions is known as Vat Liquor (Green Liquor).

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The absorber has two main portions, the first and the upper portion is usually called as under-vacuum
absorber and also tower washer (as it is using carbonating
tower waste gases in absorption). In this portion, purified
brine is fed from top and tower waste gases are fed from
bottom and absorption takes place. After exit from under-
vacuum absorber, the brine is sent to plate heat exchanger
to lower it temperature as absorption is always favorable
at high pressure and low temperature. Then, the under-
vacuum absorber brine goes to Absorber Proper which is
the second portion of absorber tower. In this portion,
absorption takes place under vacuum. Here, the first three
compartments named as Abs. Vac. Washer are auto
controlled using showering of brine such that no gases
can pass to Abs. Vac. Engine. After these three
compartments, the proper absorber starts. From very
bottom of Absorber Tower, the ammonia coming from
distillers and some makeup ammonia is fed which by
vacuum move upward. The liquor exiting the proper
absorber is called weak liquor and is sent to PHE for
lowering its temperature and then fed it back into
Preliminary Absorber. Preliminary Absorber consists of
only two compartment and the weak liquor is fed and at
its exit we get strong liquor which is commonly called as Figure 3: Absorber Tower
Vat Liquor. The Vat liquor is then sent to Vat liquor
Stock tank. Each absorber has a capacity of almost 350 tons vat liquor per day. And maintenance of
absorber tower mostly takes place after a year during plant partially shut down duration.

7. Mono-Carbonating Tower
The function of mono-carbonating tower is to partially carbonate the ammoniated brine so that NH3
absorbed in the brine is converted to ammonium
carbonate (NH3)2CO3.
Following reaction takes place in mono-carbonating
tower:
2NH4OH + CO2 (NH4)2CO3 + H2O
This is an exothermic reaction and so the heat released,
and temperature of liquor increases from 38 to 50 °C.

The vat liquor from stock is pumped to the top


of mono-carbonating tower. The liquor is evenly
distributed into the tower which contains 2’’ mini
cascade polypropylene rings in random configuration.
The low-pressure blower suck kiln gas, containing 42%
CO2 deliver it into the bottom of the MCT. The unreacted
CO2, some NH3 (flashed off from liquor), and nitrogen Figure 4: Mono-Carbonating Tower PFD
leave MCT from top, and are scrubbed of NH3 in the
MCT- washer by purified brine and sent to tower washer
brine main while the other gases vent from top. The liquid product exiting the MCT from bottom is then
go to reammoniator in which part of distiller gases (mainly consisting NH3) are passed from bottom. This
to absorb more NH3 in the liquor exiting MCT so as to increase it NH3 concentration.

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Following reaction takes place in reammoniator:
NH3 + H2O NH4(OH)

Here NH3 is absorbed in the liquor and unabsorbed gases leave the Reammoniator from top
and join the rest of the gases going to the absorber. The Liquor leaving the Reammoniator is called
Carbonated Vat Liquor (CVL), which then goes to the carbonating Towers.
There should be minimum or no crystallization due to formation of sodium bicarbonate as mono-
carbonating tower washing maintenance is difficult and is usually done annually.

8. Carbonating Tower
The carbonating tower is a very main unit as here the carbonization of CVL is completed by further
absorption of carbon dioxide to produce sodium bicarbonate, NaHCO3. In the carbonating tower, the
primary source of CO2 is kiln gas 42% CO2, and the secondary source is the strong gas coming from
calciner, 92-96% CO2
In the carbonating tower, CO2 is fed from bottom and middle by blower and the CVL is from top
of tower. The reaction inside the tower is exothermic, due to which, it is important to control the
temperature of liquor properly so that proper sodium bicarbonate crystal growth can occur, maximum
CO2 is absorbed and also ammonia retained in solution. Following reaction occur mainly in tower:
(NH4)2CO3 + CO2 + H2O 2NaHCO3 + 2NH4Cl
When the CVL is initially carbonated it has a high affinity for carbon dioxide and so the lower strength
kiln gas is used to control the temperature of liquor. However, as the reaction proceeds, higher strength
gas is required and a mixture of two sources of CO2 is used, making a CO2 concentration of 70%. The
final temperature of liquor is important to make sure that the maximum quantity of sodium bicarbonate
has been precipitated. The temperature is maintained using an intricate water circulation system with the
help of shell and tube heat exchanger. The top, middle and draw temperatures are 60, 40 and 25 °C.

The bottom product of tower is called magma which contain solid sodium bicarbonate in
suspension, which is then sent to the rotary filter. Due to the deposition of sodium bicarbonate,
ammonium carbonate and ammonium bicarbonate on the inside of towers a cleaning routine is carried out
every 72 hrs., during which ammoniated Vat Liquor is circulated in the towers to dissolve the scale.

9. Rotary Filter
The magma from carbonating tower then goes to rotary filter. The purpose of rotary filter is to
separate the crystals of sodium bicarbonate from mother
liquor and also minimize moisture and chloride content in the
cake of sodium bicarbonate. The filter is a horizontally
revolving drum. The surface of drum is porous for suction
and blowing. A trough is fitted at 75% height of drum for
washing cake with wash water to remove the chloride
content as otherwise it will contaminate the final product.
There are press rulers on both sides of filter drum which
press the cake and water is removed from the cake. At the
bottom of drum, vacuum suction is used to suck cake on the
surface of drum leaving the mother liquor and then water is
showered for washing. And after that press rollers squeeze
out the water. After this, a fixed blade is used to scrape off Figure 5: Rotary Filter Flow Diagram
the cake and then this cake is sent to calciner. And the

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remaining liquor is then sent toward distillers where it is known as feeder liquor and ammonia is
recovered from it.

10. Calciner
Here the calcination of sodium bicarbonate cake is done to turn it into light soda ash.
The main objective of calciner is to make saleable grade soda
ash and to recover maximum strong gas (92-96% CO2). In the
calciner, the decomposition of sodium bicarbonate takes
place, by which CO2 and water is produced. As shown in
equation: (Heat)
2NaHCO3 Na2CO3(s) + CO2(g) +
H2O(g)
At calciner, the bicarb cake first goes to a double shaft
mixer with the help of star feeder. In the double shaft mixer, a
quantity of dry is also fed to reduce the mixer motor load and
this ash is called as return ash. After mixing, it goes to a
rotating drum in which it is heated with steam tubes. Here the
solid soda ash moves forward and exit from calciner at almost
200-210 C and its some amount is used as return ash and other
is sent to Asher house for packing or other purposes. The Figure 6: Calciner PFD
gases leave from the opposite side of ash exit and move
through a gas riser and go into a cyclone where particles of ash and bicarb are settle down and send back
to mixer while the gases are then go to wash box for washing and then used in the plant as strong gas.

11. Ammonia Recovery Section


Ammonia recovery section consists of two prelimers, one distiller, a Cassie Cooler,
DBO vessel and a flash vessel. As ammonia is a very hazardous and expensive gas and that’s why it is
desired to recover maximum ammonia from the feeder liquor.
In the ammonia recovery section, feeder liquor coming from rotary filter goes to Cassie Cooler
where it is preheated to almost 75 C and then it goes to distiller heater section where maximum free
ammonia is removes. In this section, gases move upward from bottom and feeder liquor moves downward
in ceramic rings packing. And it is required to maintain a temperature of almost 101C on gases entrance
in heater section. The feeder liquor leaving the distiller heater section is then fed to prelimers 1 where
MOL is introduced and also IP steam is fed from bottom.
In prelimers following reaction takes place:
2NH4Cl + Heat(Steam) + Ca(OH)2 2NH3 + 2H2O + CaCl2
After overflow from prelimers-1 , feeder liquor goes to the prelimers-2 where only IP steam is
introduces from bottom. In prelimers, fixed ammonia is mainly removed and the recovered ammonia from
both prelimers is sent to gases compartment. The feeder liquor exiting prelimers-2 is then fed to
distillation section of distiller. In the distillation section LP steam is used for heating purposes. After
distillation section the remaining liquid is sent to Flash vessel where by flashing some of the ammonia is
also recovered and then it is sent to DBO vessel from more ammonia and then it is send to lime beds. The
gases exiting from the top distiller column, are fed to Cassie cooler to cool down and send to absorber.

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12. Refined Sodium Bicarbonate Plant
Refined sodium bicarbonate, commonly known as baking soda, is widely used in industry.
The Chemical Formula is NaHCO3. Basic ingredients for the manufacture of refined bicarb are soda ash
and carbon dioxide

Reaction include:
Na2CO3 + H2O + CO2 → 2NaHCO3

Here, Mother liquor dissolves LSA and is sent to the feed filter where it is filtered using a sand
filter. There are three sand filters and their combined capacity is 400m3/hr. CaCl2 is dosed in it before
sending it to the filter.
The feed is then sent to the saturator where hot kiln gas is pumped from the bottom by FD fan and
converts LSA to Sodium Bicarbonate. The gas is sucked from the top by suction fan.
The magma produced is sent to the magma tank and from there it is pumped to the centrifuge decanters.
The cake and mother liquor are separated using a filter cloth and the mother liquor is sent back to the
dissolver where LSA is dissolved.
The cake is removed by a knife and sent to the drying tube where the rest of the moisture is removed.
After that, it is sent to a cyclone where its impact is lowered, and smooth flow is maintained. It then
moves to the storage silos where RSB is packed in bags.
About 250kg of RSB is produced per hour.

13. Dense Ash Plant


The purpose of this plant is to convert light ash into dense ash
Reactions Include:
Na2CO3 + H2O → Na2CO3.H2O + Heat
(Monohydrate sodium carbonate)
Na2CO3.H2O + Heat → Na2CO3 + H2O

The first reaction takes place in Monohydrate mixer. Light ash is brought to the
mixer via conveyor but only 60% of it is fed into the mixer with soda liquor being sprayed on it. The
remainder of the 40% of light ash is fed into monohydrate mixer at a position further down the mixer.
Sodium carbonate Monohydrate crystals come out of the mixer and are fed into return ash mixer where it
is mixed with hot return ash. A vibratory screen then separates the ash and feeds it to the fluidized bed.
Hot air is used to fluidize the crystals and provide heat. The second reaction takes place here where our
desired product is separate out.

14. Main Products


• Light Soda Ash.
• Dense Soda Ash.
• Sodium Bicarbonate.

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