Professional Documents
Culture Documents
TITANIUM
PRODUCTS Ltd
Kochuveli Thiruvananthapuram
Pin: 695021
Report
on
Inplant Training
Submitted by
Mahendran S
Rohan Baby Mathews
Rohan Stephen Luke
Sarun Jolak George
CERTIFICATE
1. Mahendran S
2. Rohan Baby Mathews
3. Rohan Stephen Luke
4. Sarun Jolak George
INTRODUCTION
Travancore Titanium products is one of the main major titanium
dioxide producing industry in India from the abundant minerals like
ilmenite occurring in beach sands Manavalakurichi of Tamil Nadu and
Chavara in Kollam district.
TTP is one of the profitably running public sector units managed by the
government of Kerala. At present this plant has a capacity of 45 tonnes
per day.
TTP Ltd was set up in 1951 in collaboration with the British Titanium
Products Ltd(now Tioxide), with technology from national Lead(NL),
USA. Before 1951, the beach sand containing rare earth minerals was
being exported to Europe. The unit was promoted by the princely
administration of Travancore, in technical collaboration with the British
Titanium Products Ltd. Sree Chithra Thirunal Balaramavarma Maharaja
of Travancore and his Diwan, Sir C P Ramaswamy Iyer gave the
inspiration for starting the venture.
TITANIUM DIOXIDE
PLANT
Production Of Titanium Dioxide
Titanium Dioxide is mainly produced from the raw material
illmenite, which is a complex compound of oxides of titanium and
iron.
Process
The two mai processes for the separation TiO2 from Ilmenite are
1. Sulphate process
2. Chloride process
Raw Materials
The major raw materials used are
1. ilmenite
2. Sulphuric Acid
3. Scrap Iron
4. Glyceryl Mono Stearate
5. Aluminium Dust
6. Pottasium Sulphate(K2SO4)
7. Mono Ammonium Phosphate
Process Description
1. Grinding
2. Digestion
3. Clarification
4. Concentration
5. Precipitation
6. Post precipitation filtration
7. Pre precipitation filtration
8. Leaching
9. Post Leaching filtration
10. Treatment
11. De watering filtration
12. Calcination
13. Pulverization
14. Packing
Grinding
Ilmelite is brought to this section from godown using the belt conveyor.
The purpose of grinding is to reduce the size and hence to increase the
surface area of the ore to achieve maximum reaction efficiency.Here
the equipment used for grinding is a ball mill.
1. Ball mill
2. Rotary classifier
3. Mill fan
4. Double cone classifier
5. Cyclone separator
6. Viscobeth
7. Ductings
8. Dampers
9. Vent Pipe
Working
The material is fed into the ball mill from silo using constant weight
feeder. By the action of the fan the ground product along with the air is
sucked into rotary classifier, where the coarser particles are sent back
to the mill for regrinding. Then the air product mixture is sucked into
the double cone classifier, where the oversize is separated and sent
back to the mill. The air leaving the double cone classifier with the
required size particles reaches the cyclone separator where a whirling
action prevails. The product is separated and sent into a bunker
through an air locked rotary valve connected at the bottom of the
cyclone separator
By the action of the mill fan, air is discharged into the ball mill, at the
same time air leaving the cyclone separator is sucked by the fan. Air
from atmosphere enters at certain regons of the ductings, so suction
increases over discharge which may imbalance the whole system.
Inorder to prevent this condition, extra air is removed through a vent
pipe to the atmosphere.
Digestion
Digestion is the second section in the manufacture of TiO2 pigment.
1. Reaction
2. Baking
3. Dissolution
4. Reduction
5. Final Adjustment
The consistent unit to the digester are trident and service line, sturm
box with the strainer bottom ‘T’, service ‘T’, stand pipe and fume
cupboard with exist stack. The three arms of the trident are connected
with compressor air line, water line and stream line, and the common
service line from the trident enters at the bottom of the digester
through the service ‘T’, and bottom ‘T’. The other lines entering
through the top digester cover are the ground ilmenite, weak liquor
and cutting water inlet lines.
Clarification
The crude liquor is sent to a settler which is the equipment used for
settling operation. Reduced liquor contains unreacted ilmenite, residue
due to scrap iron and finely divided colloidal particles which are to be
removed
Settling Operation
Here the feed is fed into the settler through a feed well, so that it will
not spread at the top but reaches the centre. The temperature inside
the settler is minium 600C. An organic flocculent is used which causes
agglomeration and hence faster settling of particles. Clear overflow is
obtained from the top through pipes connected around the settler. The
rakes rotating at a speed of 1/13 rpm, gently agigate the sludge and
move it to the centre of the tank.
The sludge from the settler is withdrawn through the bottom valve and
sent to the sludge dilution tanks. After specified quantity is withdrawn
it is diluted to the required specific gravity and pumped to sludge
settlers. Weak liquor overflow from the sludge settlers is collected in
weal liquor storage tanks.
Concentration
The overflow from the settler has a concentration of 140 gpl. The
purpose of the concentration is to increase the concentration of the
liquor by evaporating the water content and hence to increase the
content of solids in the liquor per litre.
Working
The liquor from the concentration feed tank is fed to the overhead tank
from where it is fed to the preheater. Preheater is a shell and tube type
Heat Exchanger. There are 22 tubes inside the preheater. The tubes
and shell are made of electrolytic copper. The liquor from the
preheater is fed to the bottom of the bottom of the concentrator. The
concentrator has 32 tubes inside it which works independently. The
tube side is made of electrolytic copper and the shell side is made of
mild steel which has insulations to prevent heat loss. The shell side is
fed with fed with steam.
The liquor when passes through the tube side gets the water content
reduced by evaporation. The concentrated liquor and vapour are sent
to the vapour separator. The liquor at the bottom of the vapour
separator is collected into the discharge lute. The vapour is sent to the
preheater.
Precipitation
Titanium Dioxide is separated from the concentrated liquor by
precipitation. Precipation is effected through thermal hydrolysis.
Maximum precipitation takes place at a temperature of 110 0C. The
tank is made up of mild steel which has a brick lining inside made up of
acid and heat resistant bricks which prevents heat loss and also
protects mild steel. There is a rubber lining outside. The concentrated
liquor at a temperature of 900C is fed into the tank. Nuclei is charged
and kept for three hours. Steam is injected and cutting water is added.
This brings about precipitation by thermal hydrolysis. Temperature
raises to about 1100C and the tank is sealed with steam and is
maintained for 3 hours. Then it is left there for about 2 1/2 hours of
cooling.
Filtration
Here rotary drum filter is used. It is a continuous vacuum filter. Here is
liquor is sucked through a moving septum to deposit a cake of solids.
The cake is moved of the filtering zone washed, sucked dry and
dislodged from the septum, which then reenters the slurry to pickup
another load of solids. Some part of the septum is in the filtering zone
always, part is in the washing zone and part is being relieved of solids,
so that the discharge of both solids and liquids from the filter is
uninterrupted.
At the top of the drum water is constantly sprayed which washes the
pulp when it comes in the washing zone. The water and the dissolved
ferrous sulphate is sucked into the tubes. As the drum rotates, when it
comes down vacuum is released at some region and so slurry is
released.
There are 16 tubes inside which are connected to a single tube lead
which leads to a catch pot. The fumes from the catch pot are sent to a
water scrubber. The cleaned gas is sent to a common line, which is
connected to a vacuum pump. The catch pot and the scrubber are
water sealed.
Size
Length - 16 inch
Diameter – 08 inch
The pulp is diluted and is sent to the repulping tank. The repulped
mass is sent to the preleaching filters.
Treatment
In treatment section specific amount of potassium sulphate solution
and mono ammonium phosphate are added and K2SO4 is also added to
improve the tone, texture, PH and quality. Mono Ammonium Phosphate
is added to impart antirutile properties. No. of treatment tank in one
stream is two.
Dewatering Filter
The pulp is again filtered to remove the water present. In the
dewatering filter the vacuum is adjusted in such a way that to get a
solid of 37% in the pulp
Calcination
It is the process of slow heating of the pulp, which takes hours, to
reach the other end of the calciner. Calciner is a long inclined rotary
kiln, cylindrical rotating at a speed of 1/17 rpm. Its inclination is
towards the furnace end. Two numbers of calciners are available here.
They have a capacity of 30 tonnes per day.
Pulverisation
TiO2 obtained after cooling is in the form of granules. This is transferred
using belt conveyors to bucket elevator which inturn lifts the product
and dumps into a silo having a capacity of 40 tonnes. The particle size
is reduced in a Bradely Pulverizer Mill.
Packing
A weighing machine is kept below the bunker. TiO2 is filled into plastic
sacks kept over the weighing machine. 25 Kg is fed in each sack and
sacks are tied. This is then sent into the market.
SULPHURIC ACID
PLANT
Production of Sulphuric Acid
Introduction
Sulphuric Acid is a main raw material for the production of Titanium
Dioxide pigment in Titanium Travancore Products Limited. During the
expansion in 1965 a sulphuric acid plant with 50 tonns per day
capacity was also started. In 1996 a new sulphric acid plant was
commissioned with Double contact double Absorption process with a
capacity of 350 tonns per day.
Equipments
The main equipments used are
1. M.G. Filter (multi grade filter)
2. SAC unit (Strong Acid Cation unit )
3. DE gas sump
4. SBA unit
5. Mixed bed
6. D.M. Storage Tank
SAC unit
This contains a Zeocarbon resin which produces hydrogen. Chlorides of
Magnesium, calcium etc is removed in this unit. Oxides of carbon and
sulphur is converted to carbonic acid and sulphuric acid etc. water
leaving from this section has a ph of 2.5-4 and regeneration resins is
done using sulphuric acid.
De-Gaser sump
Water from SAC unit is sent here to remove the carbonic acid. Water is
sprayed to sump from top and air is supplied using a fan. The acid is
converted to co2 and h2o and co2 is sent to atmosphere.
Mixed Bed
Water from the SBA unit has low acidity and high alkalinity is not best
for steam production and so the water is demineralised using a mixed
bed.
It has two resins with the same principle of SBA and SAC units.
1.Melting Pit
2.Burner
S+O2->SO2
The molten sulphur reacted with compressed air gives sulphur di oxide
gas. A furnace is used for burning molten sulphur and compressed air.
The furnace is a horizontal, cylindrical vessel with two sulphur guns.
The length of the furnace is 7m and diameter is 4m. The furnace is
made up of carbon steel,acid proof bricks and fire resistant bricks.
Molten Sulphur is pumped from a storage tank through heated lines
and sprayed in to the furnace using burners. Dry air from air drying
tower is introduced into the furnace. The temperature of furnace is
kept at about 950-10200c, otherwise leakage of sulphur takes place .
The conversion is exactly 10.5% by mole so2
3.Convertor
The chemical conversion of sulphur dioxide to sulphur trioxide is
designed to maximize the conversion by taking into consideration that
1. Equilibrium is an inverse function of temperature and a direct
function of the oxygen to the sulphur dioxide ratio
2. Rate of reaction is a direct function of temperature.
3. Gas composition and amount of catalyst affect the rate of
conversion and the kinetics of the reaction.
4. Removal of sulphur dioxide formed allows more sulphur dioxide
to be converted.
The commercialization of these basic condition makes possible high
overall conversion by using a multipass convertor.
A four pass convertor is used for conversion in the sulphuric acid plant.
It has 4 beds of ring and start type materials coated with vanadium
pentoxide catalyst for better conversion. The conversion takes place in
two stages.
Stage-1
Sulphur dioxide gas from the mixing chambers is given to the 1st
layer of the 4 pass convertor. The conversion reaction is 2SO2+O2-
>2SO3. This reaction is highly exothermic. Thus the temperature
increases to 6000c. if this conversion stream is directly given to the 2nd
layer of the convertor then the catalytic bed may be spoiled. In order
to avoid that condition the outlet from the first layer is given to a super
heater.
Super Heater
The gaseous stream from the first stage of the convertor is given to
the tube side of the superheater and stream is passed through the
shell side. Then the temperature is reduced to 425oC. The outlet of the
superheater is givan to the second bed of the convertor where 28% of
conversion of SO2 to SO3 takes place. The conversion raises the
temperature of gas to 520oC. For cooling this gas before it is given to
the third layer a hot heat exchanger is used.
Economiser-1
For the further reduction of the temperature to 1800C an economizer is
used. In the economizer gas is flowing through the tube side and water
is flowing through the shell side. Thus the temperature is reduced to
180oC.
Stage-2
The unabsorbed SO3 gas from the interpass absorption tower is given
to the 4th bed of the catalytic convertor which is at a temperature of
4300c and 5.75% conversion of so2 to so3 takes place in the second
stage and temperature is increased due to exothermic reaction.
Economiser-2
It is similar to that of economizer-1 and having so3 gas in the tube side
and water in the shell side. Reduction of temperature takes place and
the outlet from economizer-2 has a temp of 180 0c. The outlet gas is
absorbed in final absorption tower.
Air circuit
Air for sulphur burner is supplied by electric blower is used. During the
starting of the acid plant and power filure condition electric blower is
used. All the other time steam turbine blower is used.
Air from the athmosphere is sucked through a filter for removing dust
and compresed by turbine driven air blower and it is given to air drying
tower to remove entire atmospheric oxygen. During is done with the
help of sulphuric acid. The dry air given to the burner for burning of
molten sulphur.
Precommissioning of plant
Before the plant is made ready for commissioning, it is necessary that
individual sections of the plant are checked and necessary test carried
out on the equipment to ensure their smooth functioning during
commissioning and normal running of the plant.
Preheating
The main step in precommissioning activities for first start is drying of
bricks in sulphur furnace, startup furnace and convertor. Drying of
brickwork shall be carried out by wood firing is sulphur furnace startup
furnace and convertor.
Sulphur circuit
1. For first startup clean all sulphur pits. Flush all the steam coils by
steam to remove any dirt and scale etc.
2. Fill sulphur melter with sulphur through the belt conveyor. Once
substantial amount of sulphur is added to melter, start steam in
melter coils and check for proper operation of traps. Allow the
sulphur to melt and gradually go on adding solid sulphur till level
of liquid sulphur is above the agitator level.
3. Now start the sulphur agitator, check the amperage of agitator
motor, also check for any vibration on sound and start feeding
sulphur gradually and continuously at maximum possible rate
without any lump formation in sulphur pool.
4. Add lime accordingly to neutralize acidity. After sometime
sulphur will overflow to dirty sulphur pit.
5. At this time start steam flow through coils in dirty sulphur pit.
When liquid sulphur level comes to agitator level and check for
smooth operation.
6. Open steam in dirty sulphur jacketed pipe and heat the same.
Once sufficient amount of liquid sulphur is filled in dirty pit, start
sulphur pump to recirculate sulphur. Once smoother operation of
dirty sulphur pump is established transfer the sulphur to precoat
pit and fill the same.
7. Add filter aid and start the agitator in precoat pit. Now system is
ready for precoat operation of sulphur filter. Start steam in all
jacketed pipes and in jackets of sulphur filter.
8. For filling the sulphur filter, first start steam in jacket and ensure
that all are well heated. Ensure that lid flanges are tightened
properly. Open the vent/overflow valve and start precoat sulphur
oump. Keep sulphur valve position in suitable open/close
position. Once sulphur starts overflowing close vent valve and
allow the sulphur to recirculate in precoat pit.
9. Once the precoat cycle is over filter cycle can be started. Adjust
the valves so that low from duty sulphur pump goes to filter and
then to clean sulphur. If found in limits continue the filteration
cycle. In case of ash being excessively check for possibility of
improper precoat or damaged filter leaves.
10. Once the filteration cycle is over as indicated by reduced
sulphur flow in filter outlet, prepare to open and clean the
sulphur filter.
11. Keep clean sulphur tank sufficiently full well before
scheduled date of sulphur firing. Take a trial of clean sulphur
pump amd circulate sulphur in all relevant pipelines.
Normal Operation
Sulphur Section
1. Check the ash content in sulphur once in a shift. Higher ash
content may be due to improper precoat or damage to the
screen. Take the corrective action accordingly.
2. Choking of filter as indicated by reducing in sulphur flow
indicates filteration cycle. At such time arrange for cleaning
sulphur filter.
3. Analysis ash content and acidity of dirty sulohur feed to filter.
This will ensure corrosion free operation and help in anticipating
filteration cycle.
4. Incase filter aid contains chlorides wash the same thoroughly
before feeding to filler to avoid corrosion
Gas circuit
1. Analyse so2 at convertor inlet regularly. Plant is designed to
operate at 10.5% so2 convertor inlet.
2. Convertor 2nd bed inlet temperature can be controlled by
operation of super heater bypass valves.
3. Inlet temperature of 3rd pass is controlled by hot heat exchanged
tube side bypass valve.
Acid Circuit
1. Amperage of circulation pump should be noted regularly.
2. Acid samples should be analysed once a day check operation of
analyser.
3. Level indicator readings should be checked frequently by manuel
level measurement.
4. Observe flow of acid in tower distributor once a day through
sight glasses.
Boiler circuit
1. Check boiler feed water sample and boiler blow down sample
once a day. Any abnormality observed it should be corrected
immediately in water treatment, chemical closing or blow down
frequency.
2. Ensure that steam flow is deaerator is maintained and BFW is at
a temperature of 100-1050c.
3. Safety valves should be checked regularly to ensure safety of
high pressure equipment.
4. Level gauges should be drained and checked once a shift.
5. In no case boiler water level should be allowed to go below
normal level
6. While operating boiler feed water pump, corresponding
recirculation line valve should be kept open.
Shutdowns
In any shutdown, the first thing to turn off is the sulohur feed. For hot
shutdowns, the blower should be turned off immediately after the
sulphur is turned off. For shutdowns, those are expected to last more
than 5-10 min, the acid cooling water should be turned off. Do not stop
the circulation of acid over the towers unless it is necessary to do so.
When possible increase catalyst temperature a few degrees before
shutdown. These will simplify the subsequent start up. Make sure that
dilution water is cut off.
Before shutting down for a prolonged period allow the strength of the
process acid run up to 0.1-0.2% above normal operating strength. This
will serve as a buffer against the small decreases in strength normally
observed during a prolonged shutdown. Then stop dilution water.
Turnoff the sulphur feed, and reduce the dry airflow to about 50% of
design. Cool all catalyst leads with air to about 50 0c at a rate not
greater in the boiler approaches atmospheric temperature, the vent
valve on the steam drum must be opened to prevent formation of
vacuum inside boiler. If the boiler is to be entered during shutdown,
cool raw water may be used as feed water after all steam generation
has stopped, and the circulation. A boiler should not be drained until it
is cooled throughout.
Temperature and conversions in each stage of the 4-
pass convertor
Location Temperature Equivalent
0
c conversion
Gas entering 1st pass 430
Gas leaving 1st pass 600
Rise in temperature 170 60%
TOTAL 99.75%
Conclusion
Travancore Titanium Products Ltd is one of the profit
gaining public sector units. The major asset of this
company is skilled staff. Moreover the efficient
management of the resources have helped them to
overcome the slump in the sales over the last few
years.