1

PROJECT REPORT
(STUDY OF REACTOR PARAMETERS)
For
VOCATIONAL TRAINING
At
PHILLIPS CARBON BLACK LIMITED, DURGAPUR.

Project by:
1>
2>
Chemical
Engineering

WHAT IS CARBON BLACK

Carbon black is a material produced by the incomplete combustion of
heavy petroleum products such as FCC tar, coal tar, ethylene cracking tar.
Carbon Black is used in almost every part of the car, from the engine
compartment to the tyres and the exterior coatings. It is also used to
reinforce rubber. Carbon Black's biggest application is as reinforcing filler in
rubber products.
The most common use (70%) of carbon black is as a pigment and reinforcing
phase in automobile tires. Carbon black also helps conduct heat away from

the tread and belt area of the tire, reducing thermal damage and increasing
tire life.

PRODUCT DESCRIPTION
Carbon Black is composed essentially of elemental carbon in the form of
semispherical,
colloidal particles coalesced into each other and forming mainly particle
aggregates.

These are obtained by partial combustion and thermal decomposition of

highly aromatic
hydrocarbon oils under controlled conditions.
There are many types of Carbon Blacks that differ in the physical-chemical
properties of
the particles.
This wide variety of Carbon Black grades requires different reactor designs
and different
reaction conditions (temperature, residence time, turbulence and
concentration of active
ingredients).

Carbon Black Particle Size Comparison

Mean Diameters

N 110(15 nm)
nm)

N 762 (80 nm)

N 990(280

CARBON black structure comparison

CERTAIN GRADES OF CARBON BLACK

HARD BLACK
N-110, N-115, N-220, N-234, N-219, N-231, N-299, N-330, N-326,
N-347, N-351, N-339, N-375.

SOFT BLACK
N-550, N-660, N-650, N-765, N-762, N-774, N-772.
SPECIAL GRADES
P -435 (plastic grade), N 330B.

Hard Black grade particles are finer and gives higher abrasion
resistance where as soft black grades are coarser and exhibits
better flexibility.
First digit of the number denotes particle size
For 220 grade Carbon Black particle diameter around 20 nm i.e.,
20x10-9m.

MANUFACTURING PROCESS OF CARBON BLACK

Carbon black is produced with the thermal decomposition method or the
partial combustion method using hydrocarbons such as oil or natural gas as
raw
material.
The characteristics of carbon black vary depending on manufacturing

process, and therefore carbon black is classified by manufacturing process.

Carbon black produced with the furnace process, which is the most
commonly used method now, is called furnace black, distinguishing it from
carbon black, which is manufactured with other processes.
Furnace method forms carbon black by blowing petroleum oil or coal oil as
raw material (feedstock oil) into high-temperature gases to combust them
partially. This method is suitable for mass production due to its high yield,
and allows wide control over its properties such as particle size or structure.
This is currently the most common method used for manufacturing carbon
black for various applications from rubber reinforcement to colouring.

NAME: Oil Furnace Process

Used in: tyre/non tyre industry
Plastic grade carbon black
Plastic hose pipe
Plastic pipe
Paints, inks
Engineering components-V belts, conveyor belts
Raw material:
Conversion Oil (Make oil)
Liquid hydrocarbon like lube extract, FCC bottoms from petroleum
refineries (overseas), tar oil from steel plants etc.
Composition:
C content- >90% (higher the better)
H content- (5-7) % (lower the better)
S level- < (1.5 to 2)% (lower the better)
Metal traces- Na, K, Al etc. <10 ppm.

Tar oil testing

-

Moisture content using dean and stark apparatus

Viscosity using a viscometer
Mid boiling range(MBR) by distillation(MBR is inversely proportionally
to BMCI)
BMCI is an indication of the aromaticity of the feed stock

Higher BMCI >> higher aromaticity >> higher carbon content >>
higher YIELD%
However BMCI cannot be increased indiscriminately because higher
hydrocarbons will contain greater number of C-C bonds which would
require a larger amount of activation energy to break down.
Optimum BMCI is in the range 132-135.

Chemistry of the Process

Oils undergo high temperature cracking (incomplete combustion) inside the
reactor in deficiency of oxygen to form Carbon Black. Few gases are also
generated during the reaction. The combustion of gases is called Off-Gas.
It is the process waste gas and is the only by product in the manufacture of
Carbon Black.

Reaction
Oil + Air
CXHY + O2
O2

Carbon Black + Gas

C + CO2 + CO + H2O + CH4 + C2H2 + H2 + N2 +

SO2 is also formed if S is present in the feedstock. The temperature of the

reaction varies from 1300C to 1800C depending on the type and grade of
carbon black produced.

Burning of Oil
CHZ + (1+ z/4) CO2 + (z/2) H2O

Pyrolysis of Oil
CHZ C + (z/2)H2

Side reactions
Carbon CO2 reaction
C + CO2

2CO

Carbon H2O reaction

C + H2O CO + H2
SO2 + 2C COS + CO
2COS + C CS2 + 2CO

PROCESS DESCRIPTION
Supporting feedstock (SFS) fuel is burned in the tangential tunnel of the
reactor (pre combustion chamber) with calculated preheated air, air usually
being 40 to 100 % in excess of the theoretical depending upon the
combustion temperature.

REACTORS

HOW A CAT REACTOR LOOKS FROM INSIDE

(Atomizing air is used in order to atomize the SFS.

Reason: Atomizing results in a volume expansion thereby reducing the oil
density. This provides for a quicker phase change of oil to its vapour state,
thereby reducing the amount of unburnt oil in the reactor.)
In soft black operations no auxiliary fuel is used.
Heated feedstock kept in different storage tanks are transported to the
process by high pressure pumps & fed to the horizontal refractory lined
reactors through burners of special design.
(The make oil is injected radially to get the characteristic star like pattern.
It also helps to utilize the heat obtained from SFS combustion more
efficiently.)
Feedstock undergo cracking inside the reactor at high temperature in
presence of insufficient air( although combustion of the make oil takes place
simultaneously with cracking ) and the resultant smoke of Carbon Black & off
gas is directly quenched with water sprays and passed through heat
exchanger ( Rekuperator ).

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Quenching can be done in 2 ways:

i)
ii)

Radial: Heat is extracted from the entire plane, so reaction stops in

single
step.
Co-current /Counter current: Conical zone is formed and
reaction stops in 2
steps. Temperature
first drops to 1200C and
then
further to 900C.

Radial

Co-current

Rekuperator (air pre heater, APH) , imported from Germany, is the

unique piece of energy saving equipment which helps conserve considerable
quantity of heat energy extracted from hot carbon black smoke stream and
donated to the cold process air to increase its temperature up to 800C.
The smoke stream still retains quite good amount of sensible heat. This heat
is effectively utilized in raising process steam in the waste heat boiler and in
pre heating the reactor feed oil in the pre heater (OPH).
The product stream is further water quenched, if required, before its entry
into the process bag filter at a temperature between 250C to 300C.For
carbon black separation in order to avoid condensation of steam, the process
bag filter ( multimodular type ) is equipped with fibre glass bags. After
separation of carbon black from gases in the filter modules, the fluffy black is
conveyed by cold air stream to the micro pulveriser.
The function of the micro pulveriser is to finely crush down any foreign
material present in the carbon black. The carbon laden air reaches the DBC
(DENSE BAG COLLECTOR) which separates CB from air. Clean air is vented
and the CB thus separated is sent to intermediate storage tank (called dense
tank). CB passes through Rotary feeder to enter the Pelletier unit (the shaft
inside the shell is fitted with radial pins in a double helical arrangement, the
pins extending to a close clearance with the shell, and optimum distance

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between pins and shell being 2.5 mm).A paste of CB is made inside the
pelletiser unit with the help of water and some beading aids like molasses.

Pelletiser shaft with pins

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Inside the pelletiser shell

It is then followed by horizontal rotary dryers heated by waste off gas

burning to produce dry pellet product .Waste off is also utilized in the
captive power plant (cpp) for generation of power.
Wet pellets from the pelletiser are fed by a screw conveyor to the dryer
where the moisture content is reduced to less than 1%(typically 0.5%). The
dryer is a large rotating drum mounted on rollers and rotated at 3 to 4 rpm.
Wet pellets are fed at one end and dry pellets exit at the other. Internal
helical flights attached to the drum shell rapidly move the CB into the heated
section and agitating flights or lugs tumble the CB as it passes through the
heated length. A separate combustion furnace is employed with combustion
gases distributed along the heated length of the drum by a refractory duct.
A purge gas blower pulls a portion of the combustion gas into the drums
through inlets known as snorkels and located near the outlet ends. The
purge gas passes through the drum countercurrent to the CB flow to sweep
out the steam. From the blower the purge gas is routed to vapour bag
collector.
Dryer discharge product is carried via elevator to different final storage
tanks.

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The entire manufacturing process operates and is controlled in a highly

sophisticated room known as the Distributed Control System (DCS).

Material Conveying Equipment

1) Screw Conveyor
Screw conveyors are one of the oldest and simplest methods for moving bulk
materials and consist primarily of a conveyor screw rotating in a stationary
trough, Material placed in the trough is moved along its length by rotation of
the screw which is supported by hanger bearings. Inlets, outlets, gates and
other accessories control the material and its disposition.
The conveyor screw is the rotating portion of a screw conveyor which
imparts smooth and positive motion to the bulk material being conveyed. It
consists of spiral flights mounted on a pipe and is made either right or left
hand to suit the screw rotation and the desired direction of material travel.

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PARTS OF A SCREW CONVEYOR

2) BUCKET ELEVATOR

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A bucket elevator, also called a grain leg, is a mechanism for hauling

flowable bulk materials (most often grain or fertilizer) vertically.
It consists of:
1.
2.
3.
4.

Buckets to contain the material;

A belt to carry the buckets and transmit the pull;
Means to drive the belt;
Accessories for loading the buckets or picking up the material, for
receiving the discharged material, for maintaining the belt tension and
for enclosing and protecting the elevator.

INSIDE A BUCKET ELEVATOR

A bucket elevator can elevate a variety of bulk materials from light to heavy
and from fine to large lumps.

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CERTAIN FLOW MEASURING DEVICES

1) Orifice Plate
With an orifice plate, the fluid flow is measured through the difference in
pressure from the upstream side to the downstream side of a partially
obstructed pipe. The plate obstructing the flow offers a precisely
measured obstruction that narrows the pipe and forces the flowing fluid to
constrict.

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The orifice plates are simple, cheap and can be delivered for almost any
application in any material.
The Turndown Rate for orifice plates is less than 5:1. Their accuracy is
poor at low flow rates. A high accuracy depends on an orifice plate in
good shape, with a sharp edge to the upstream side. Wear reduces the
accuracy.

2) Venturimeter
Due to simplicity and dependability, the Venturimeter is often used in
applications where it's necessary with higher Turndown Rates, or lower
pressure drops, than the orifice plate can provide.
In the Venturimeter the fluid flow rate is measured by reducing the cross
sectional flow area in the flow path, generating a pressure difference.
After the constricted area, the fluid is passes through a pressure recovery
exit section, where up to 80% of the differential pressure generated at the
constricted area, is recovered.

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With proper instrumentation and flow calibrating, the Venturimeter flow

rate can be reduced to about 10% of its full scale range with proper
accuracy. This provides a Turndown Rate 10:1.

3) Mass Flow Meter

A mass flow meter, also known as an inertial flow meter is a device that
measures mass flow rate of a fluid traveling through a tube. The mass
flow rate is the mass of the fluid traveling past a fixed point per unit time.

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The mass flow meter does not measure the volume per unit time (e.g.,
cubic meters per second) passing through the device; it measures the
mass per unit time (e.g., kilograms per second) flowing through the
device. Volumetric flow rate is the mass flow rate divided by the
fluid density. If the density is constant, then the relationship is simple. If
the fluid has varying density, then the relationship is not simple. The
density of the fluid may change with temperature, pressure, or
composition, for example. The fluid may also be a combination of phases
such as a fluid with entrained bubbles.

4) Magnetic Flow Meter

An electromagnetic flowmeter operate on Faraday's law of
electromagnetic induction that states that a voltage will be induced when
a conductor moves through a magnetic field. The liquid serves as the
conductor and the magnetic field is created by energized coils outside the
flow tube.
The voltage produced is directly proportional to the flow rate. Two
electrodes mounted in the pipe wall detect the voltage which is measured
by a secondary element.
Electromagnetic flowmeters can measure difficult and corrosive liquids
and slurries, and they can measure flow in both directions with equal
accuracy.
Electromagnetic flowmeters have relatively high power consumption and
can only be used for electrical conductive fluids as water.

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COMPRESSOR
A gas compressor is a mechanical device that increases the pressure of
a gas by reducing its volume.

Compressors are similar to pumps: both increase the pressure on a fluid and
both can transport the fluid through a pipe. As gases are compressible, the
compressor also reduces the volume of a gas. Liquids are relatively
incompressible; while some can be compressed, the main action of a pump
is to pressurize and transport liquids.

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SEPERATION OF CARBON BLACK FROM SMOKE

PULSE BAG COLLECTOR (PBC)
Pulse bag collectors are also commonly known as baghouse. The filtering
part consists of numerous cylindrical meshes which are covered by silicon
coated fibre glass bags. It is here that the smoke from the reactors is
processed to get the fluffy carbon black. In the Durgapur plant, there are
total of 15 PBCs:
LINE 1 > 6 PBC
LINE 2 > 7 PBC
LINE 3 > 2 PBC
In the PBC, a high pressure blast of air is used to remove dust from the bag.
The smoke laden air enters from the side of the PBC and its entrance is lower
than that of the pulsating air. Carbon black adheres on the surface of the
silicon coated glass fibre bags, while the air moves out from the top and
goes to the CPP. The blast (air at 90 psi) enters the top of the bag tube,
temporarily ceasing the flow of dirty air. The shock of air causes a wave of
expansion to travel down the fabric. The flexing of the bag shatters and
discharges the carbon black. The air burst is about 0.1 second and it takes
about 0.5 seconds for the shock wave to travel down the length of the bag.
Due to its rapid release, the blast of air does not interfere with contaminated
gas flow. Therefore, pulse-jet baghouses can operate continuously and are
not usually compartmentalized. The blast of compressed air must be
powerful enough to ensure that the shock wave will travel the entire length
of the bag and fracture the dust cake.
LINE 1 & LINE 2 PBC CONTAINS 284 BAGS WHILE LINE 3 PBC
CONTAINS 492 BAGS.
Bag filter troubleshooting: In case there is any leakage in the filter bags,
the carbon black might travel upwards with the air instead of sticking to the
sides of the bags. In this case, nitrogen gas purging is carried out. Here,
pressurized nitrogen gas is passed below individual bags and wherever it
reaches the top, indicates a faulty bag. The particular bag is temporarily
closed to prevent any further leakage. The number of faulty bags covered at
a time can range from anything between 6 to 20 or even more.

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INSIDE THE PBC

FUNCTIONING OF THE PBC

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PBC: OUTER & INNER VIEWS

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DISTRIBUTED CONTROL SYSTEM

Distributed Control Systems are used to control the manufacturing process

that are continuous or batch-oriented, such as oil refining, petrochemicals,
food & beverage manufacturing, cement production, steelmaking etc. DCS
are connected to censors and use set point control to control the flow of
material through the plant. The most common example is a set point control
loop consisting of a pressure censor, controller, usually through the aid of a
signal conditioning input device. When the measured variable reaches a
certain point, the controller instructs a valve or actuation device to open or
close until the fluidic flow process reaches the desired set point. Large oil
refineries have many thousands of points and employ very large DCS.
The priority of DCS is to provide superior operator interfacing & real time
process control. The flexibility of implementation of sequential control &
integration among the various types of control is also an additional feature of
DCS. As the nature of the system is distributed so a single failure will not
shut down the whole process.

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Temperature
profile
&
CONVERSION
DURING
MANUFACTURING PROCESS

SENSIBLE
CARBON

HEAT
BLACK

1900C

900C

500C

(i)

1650C
350C
(ii)

1200C
(iii)

(iv)

650C

(v)

Around 100C < 170C

(vi)

(vii)
<

250C
(x)

(i)
(ii)
(iii)
(iv)

(ix)

(viii)

Temperature reached during combustion.

Temperature after cracking of oil has occurred.
Temperature after quenching with water.
Air is heated by passing it through the APH and is sent to the
reactor header at 800C.
(v)
This temperature in the Waste Heat Boiler (WHB) is used to
generate steam. This steam is used for atomizing purposes, flashing
in the APH to prevent CB from sticking to its sides.
(vi) The OPH (oil pre heater) at this temperature pre heats the Make Oil
before sending it to the choke section of the reactor.
(vii) Smoke + flue gases reach the Quench tower for further cooling.
(viii) It is passed through the PBC modules from where fluffy Carbon
Black is obtained.
(ix) Temperature inside the dryer.

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(x)

Product temperature.

AT PCBL, DURGAPUR
Reactors

Carbon Black is being prepared in 2 kinds of reactors namely CAT

(Columbian axial trade) & CARCASS.
CARCASS >>>>>> produces SOFT grade CB.
CAT >>>>>>>>> produces HARD grade CB.
There are 4 CAT reactors namely CAT 1, CAT 2, CAT 4 & CAT 6.
The reactors are divided into 3 lines:
LINE 1 CAT 4 & CAT 6
LINE 2 CAT 1 & CAT 2
LINE 3 CARCASS

UNLOADING

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The oil comes in tanks.

All the seals are checked, serial and batch numbers are matched
according to the document provided.
Visual checking is done by inserting a rod from the tank top and seeing
whether the oil slips from the rod surface or not.
Certain quality tests are done on a sample such as moisture, viscosity.
If all criterias are fulfilled then only will the sample be unloaded.
Unloading is done both by the help of gravity and through pumps.

TANKS
The plant houses a total of 26 tanks.
11 are for CB storage.
Line 1 has 2 tanks, each having 4 compartments with capacity @
125 MT each compartment.
Line 2 & line 3 have 9 tanks, 250 MT each.
v7c1,v7c2,v7c3 are 3 dedicated tanks for line 2.
v7c5, v7c6, v7c7, v7c8, v7c9 are 5 dedicated tanks for line 3.
v7c4 tank can be used for either line but is mostly used for the
softer grade CB.
9 are used to store raw materials such as Tar Oil, CBFS, LDO, IFS.
2 tanks are used to store water
2 are blending tanks.
2 are for high speed diesel.
The tank numbers and their capacities are shown below:

STORAGE
NO.
S-1
S-2
S-3
S-4
S-6
S-8
S-10
S-11

TANK CAPACITY(KL)
1600
1600
800
800
4500
4500
4500

MATERIAL TYPE
Tar Oil
Tar Oil
Water
CBFS-HPL
LDO
IFS
IFS
Water

TYPE
Insulated
Non-insulated
Insulated
Insulated
Non-insulated
Non-insulated

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S-12
S-13
S-16
S-17
S-18

90
90
1600
5000
5000

Blending Tank
Blending Tank
IFS
CBFS-HPL
IFS

TOTAL PLANT AREA

Total plant area is around 31 acres.
5.5 acres dedicated to Captive Power Plant (CPP).
22 acres dedicated to CB manufacturing part.
Rest of 3.5 acres is the extension part.

RAW MATERIAL
CBFS is shipped from USA by ships.
Components of CBFS
Naphthalene
Methylnaphthalene
Biphenyl
Methyl biphenyl
Fluorine
Anthracene
Asphaltenes
Other polycyclics

10 %
20 %
5
5
5
5

%
%
%
%
10 %
40 %

All data are given in %-w/w unless stated otherwise.

It follows the following route: Mundra >> Palej >> Cochin >>
Haldia >> via road tanks to Durgapur.
Coal tar is the higher fraction of petroleum distillation.
Tar Oil is the lower fraction of petroleum distillation.
Feed for the reactor is composed of 80% IFS + 10% each of C.TAR &
T.OIL.
IFS is highly aromatic and is a blend of different oils.
ITO (imported tar oil) from China has a tendency to get cooled very
fast hence creates problems of pitch formation.
55000 cu. Nm/day CBM (coal bed methane) is being supplied while
72000 cu. Nm/day is required for full functionality.
Potassium Nitrate/ Potassium Carbonate (KNO3/K2CO3) and
Molasses are used as
respectively.

reactor additives and pelleting additives

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Potassium Nitrate/ Potassium Carbonate

solution is injected in

CBFS prior to entering the Reactor for Carbon

Raw molasses is injected into a mixing tee with water. This mixed
solution then goes into wet mixer for pelletisation. Molasses increases
the pellet strength of carbon black.

AIR INPUT
Atmospheric air is used as raw material in the reactors.
6 air blowers suck the atmospheric air and provide to the reactors.
4 Hoffmann Blowers + 1 Process air blower (PAB) + 1 Roots blower
(RB).
Hoffmann blowers are named as HB-1, HB-2, HB-3, and HB-4.
Capacity of each HB is 20000 cu. Nm/hr.
HB-1, HB-2, HB-3 + 1 PAB + 1 RB are connected to the high pressure
header which supplies air to all the CAT reactors.
HB-4 is connected to the low pressure header which provides air to
CARCASS.

Process air blower

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PRODUCTION TIME
FOR 1 CYCLE OF PRODUCTION
LINE 1 40 minutes
LINE 2 45 minutes
LINE 3 50 minutes

PACKING
2 kinds of packing material: BULK BAG & PAPER BAG
BULK BAG PROPERTIES
Made of polypropylene and is laminated.
It is meant for wholesale packaging
Weight is 1000 kg.
It is made for those processes where pneumatic conveying is possible
(large scale industries)
There are 2 sizes: (92 x 92 x 230) cu. cm. for domestic purposes.
(102 x 102 x 240) cu. cm for export purposes.
Each bag has a code for e.g.: D120625J
D stands for Durgapur, 120625=yymmdd, J is the machine number.

PAPER BAG PROPERTIES

Made of scrap paper
Meant for small or retail packaging.
Weight is 25 kg.
It has been designed for smaller processes where manual conveying of
material is carried out.
It has only 1 standard size.

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Carbon black quality tests

DBP test (DBP-dibutyl phthalate)

Primary quality control method used to access the structure of carbon

black.

Device used in known as an absorptometer.

20 Gms. Carbon black is taken in an internal mixer consisting of

rotating blades, to which DBP or paraffinic oil is added drop wise
through an automated burette.

DBP is added till the mixture changes from a free flowing powder to a
semi-plastic agglomerate.

70% of the maximum torque that can be developed is set as the end
point.

The process stops when the set torque point has been reached.

Quantity of DBP is noted and calculated as ml of oil/100gm of carbon

black.

Iodine number test (for surface area measurement)

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It measures the amount of iodine which can be adsorbed on the

surface of a given mass of carbon black.

0.50 gm carbon black is treated with 25ml standard iodine solution;

the mixture is shaken and centrifuged.

20 gm of this solution is titrated with 0.0394N sodium thiosulphate

solution and starch solution is added till the solution is transparent.

Amount of thiosulphate solution used is noted which is the S value;

another blank value B, is noted without taking carbon black into the
solution.

Now, the B-S value is noted at the particular strength of thiosulphate

solution and the iodine number is calculated with the help of a chart.

Iodine number is reported as grams of iodine adsorbed per kilogram of

carbon black (g/kg).

Pour density (PD)

The pour density of carbon black is useful for estimating the weight-tovolume relationship for certain applications such as automatic batch
loading systems and for estimating weights of bulk shipments.

A cup of known volume is taken, filled completely and flattened from

top with carbon black.

Its weight is taken and multiplied by 2 to get the Pour density.

Pellet hardness

This method determines the individual crush strength of carbon black

pellets, which may affect the handling properties and possibly the
dispersion of carbon black in rubber compounds.

35

It is measured in an apparatus called Individual Pellet Hardness Tester

(IPHT).

Sample of carbon black is taken and sieved through standard screens

of 12 mesh and 14 mesh.

Fraction retained on 14 mesh is taken and kept on a container in the

IPHT.

All sample details (grade, time taken) are fed into a computer
software.

The machine employs a piston that brings 1 pellet at a time against a

load cell until it breaks it.

Data on 20 such pellets is collected and finally the average value is

taken as the hardness.

Grit testing

This test determines the amount of water wash sieve residue present
in carbon blacks and is important in some molded or extruded
products as it may relate to surface appearance of those products.

100gm sample is taken and put in a conical container below which a

mesh of 325 mesh number is kept.

Water at 30 psi is forced through the sample till residue is left behind
on the mesh.

Mechanical rubbing is done to remove any residual carbon black.

The residue is passed through 100 mesh and then 25 mesh and the
weight retained is noted.

The grit is passed under a magnet to check for any metallic impurities
also.

Presence of grit leads to a non-homogeneous product which might lead

to its failure.

Heat loss

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The heating loss is the weight loss of carbon black upon heating and is
a measure of the amount of moisture and other volatile materials on
the surface of carbon black.

It is calculated in an apparatus known as the moisture balance.

The machine is calibrated after which the sample is distributed evenly

on a pan.

The pan is kept in the apparatus and the sample is heated for around 5
minutes at 30 deg. C. with the help of a bulb.

A pointer on a scale shows the amount of moisture lost.

Toluene discoloration

This method estimates the amount of toluene-soluble discoloring

residues present on the surface of carbon black.

Basically, it measures the degree of unburnt oil in the reactor.

A certain amount of sample is taken in a test tube and toluene is

added as 10 times that quantity.

The solution is passed through a filter paper and the filtrate is taken.

Light of 425 nm wavelength is transmitted through the filtrate in a

spectrophotometer which determines the discoloration of toluene.

Lower the value of % transmittance, greater will be the amount of

residue remaining on carbon black.

Heat Recovery and Tail Gas Utilization

The Carbon Black manufacturing process generates both the sensible heat
energy contained by and the chemical energy in the tail gas. Without a
waste energy recovery strategy, less than 60 percent of the sensible energy

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and only 50 percent of the chemical energy is utilized for the Carbon Black
manufacturing process. Optimizing recovery of these energies make sense in
reducing carbon dioxide emissions, as well as providing additional revenue.
For reducing carbon dioxide gas, it is very important to increase the yield of
Carbon Black from Carbon Black oil by using a well-controlled heat recovery
process and also utilizing tail gas as a fuel for the boilers, dryers and oil
preheaters. Utilization of tail gas thereby reduces the need for fossil fuels,
such as petroleum oil or natural gas.
There are some energy recovery and tail gas utilization facilities in the
process, such as,
Air pre-heaters
Boilers including steam boilers, waste gas boilers and inline boilers
Oil pre-heaters
Dryers
Air Pre heater
Reactors are equipped with air pre heaters which are actually heat recovery
facilities used to exchange heat from the tail gas containing Carbon Black
under high temperature into combustion air for the imperfect combustion of
Carbon Black oil. The simultaneously cooled Tail Gas is then directed to the
next facility. An air pre-heater is usually constructed as a tubular heat
exchanger through which combustion air counter flows to the tail gas.
Combustion air supplied by an air blower is heated up to a range of 500
800 degree C by an air pre-heater.
It is well known that a higher combustion air temperature results in a better
yield of Carbon Black.

Tail Gas Utilization

The imperfect combustion of Carbon Black oil converts half of the
hydrocarbons in oil into Carbon Black and the other half into Tail Gas. The
Carbon Black Industry has developed specific tail gas combustion chambers
so as to supply heat energy to boilers, dryers and oil pre-heaters thereby
eliminating the need for petroleum oil or natural gas.

38

Steam Boiler
Concerning energy supply, the Carbon Black Industry installs special boilers
which generate steam and/or electricity that are consumed during the
manufacturing process. Generally speaking, the tail gas combustion steam
boiler efficiently co-generates both steam and/or electricity that are then
consumed as either heat energy to keep the Carbon Black oil warm, or as
power to drive the motors for the air blowers, the air compressors and the
many pumps. Furthermore, two of these 26 energy products can be
transferred to neighboring industries where possible, and can contribute to
reducing carbon dioxide emissions at neighboring industries.
Oil Pre-Heater
Carbon black oil is highly carbonaceous and needs to be preheated for easy
transportation and atomization in reactors. The smaller the droplets, the
faster they mix with the hot flame in the reactors, the quicker the reaction
time and the better the carbon black yield.
Dryer
The wet pellets have to be dried after leaving the wet pelletizers. This is
done by rotary-kiln dryers using an indirect heating method in order to
remove the water added in wet pelletizers. The heat source for the dryers is
tail gas that is separated from Carbon Black by the main bag filters. This tail
gas is then directed with air into the combustion chamber of the dryer and
generates burnt gas of high temperature, about 800 degree C. Then this
burnt gas enters into the external drum of the dryer and indirectly heats the
Carbon Black which is led to the internal drum of the dryer. Drying efficiency
and Carbon Black transport have both been improved by fitting additional
components such as lifters in the dryers.

39

CAT 1 REACTOR DATA SHEET

CAT 1

(WEDNES
27-06-12 DAY)

GRADE(LINE 2)
N330 B
TIME(A.
MAKE
AIR
SFS(kg/
M.)
OIL(kg/hr)
RATE(Nm3/hr) hr)
10:03
4879.51
11485.44
559.24
4882.7
11490.37
568.82
10:05
4869.66
11486.15
569.04
4840.48
11482.45
571.03
4833.02
11482.27
569.54
4835.99
11538.32
567.41
4852.96
11551.52
566.06
10:10
4869.81
11527.95
565.72
4868.3
11520.43
578.72
4890.78
11501.48
571.07
4901.22
11497.25
567.47
4891.77
11499.8
571.96
10:15
4893.41
11494.52
568.12
4878.88
11486.56
571.32
4901.88
11467
579.95
4891.77
11489.38
572.83
4890.23
11528.25
570.33
10:20
4893.12
11517.83
571.2
4887.46
11515.58
568.95
4884.67
11492.03
572.51
4880.55
11501.77
570.44
4864.77
11501.58
569.98
10:25
4881.23
11494.34
569.4
4873.97
11491.54
571.23
4875.13
11478.21
565.48
4862.57
11483.75
568.44
4853.59
11491.2
577.07
10:30
4861.18
11483.4
573.04
4862.83
11529.02
563.81
4884.41
11577.79
570.81

40

10:35

10:40

10:43
MAX
VALUE
MIN
VALUE
DIFFERE
NCE
AVERAG
E
S.D.

4885.11
4859.32
4870.35
4867.71
4859.21
4860.78
4860.62
4857.97
4835.16
4794.59
4805.61

11531.83
11440.02
11460.89
11481.81
11477.46
11506.89
11502.41
11499.16
11503.61
11525.04
11506.16

572.27
564.72
555.71
560.09
569.43
568.2
572.84
573.2
567.23
570.44
566.13

4901.88

11577.79

579.95

4794.59

11440.02

555.71

107.29

137.77

24.24

4848.235

11508.905

23.48349574

25.03905784

567.83
4.61439
77

CAT 1 TREND
RATE OF CHANGE OF MAKE OIL WITH TIME

41

RATE OF CHANGE OF AIR RATE WITH TIME

RATE OF CHANGE OF SFS WITH TIME

42

CARCASS DATA SHEET

CARCA
SS
(LINE 3)
TIME
(A.M.)
10:06
10:10

10:20

10:30

30-06-12

P435

(SATURDAY
)

TOTAL OIL
TANGENTIA REACTOR
RATE
AXIAL AIR
L AIR
EFFICIENCY
(kg/hr)
(Nm3/hr)
Nm3/hr)
(%)
8661.32
5962.77
10026
54.17127146
8665.36
5965.79
9941.79
54.47315054
8665.66
6040.51
9961.09
54.1549595
8649
6022.86
9970.51
54.07865884
8637.83
6012.12
9938.16
54.1547233
8659.07
6021.12
9952.54
54.20842812
8671.77
5991.67
9946.01
54.41049136
8690.27
6054.53
10027
54.03882591
8703.03
5954.55
10015
54.49765335
8720.17
5963.1
10066
54.40211865
8733.47
5947.61
10023
54.68463634
8526.68
5925.65
9966.64
53.65293485
8701.48
6017.69
9985.44
54.37361316
8701.59
6177.54
9821.25
54.38905067
8670.48
6118.47
9950.43
53.95814275
8656.32
6006.01
9965.38
54.19891443

43

10:40

10:50

11:00
11:04
MAXIMU
M
MINIMU
M
DIFFERE
NCE
AVERAG
E
S.D.

8659.39
8731.26
8729.91
8690.19
8680.7
8704.33
8713.07
8740.22
8741.03
8717.1
8715.62
8713.82
8729.65
8700.1

6011.56
5998.61
5929.27
6019.55
5826.91
5973.65
6042.4
6029.53
5963.78
6002.99
6003.61
6023
5982.43
6044.59

9966.59
9985.74
9948.11
10011
9991.44
10002
10094
10058
10010
9978.64
10027
10022
10006
10051

54.19519782
54.62380391
54.98331589
54.21017994
54.87740504
54.48498183
53.99636846
54.32916054
54.72111172
54.5444989
54.36861105
54.30863197
54.59979498
54.05269394

8741.03

6177.54

10094

54.98331589

8526.68

5826.91

9821.25

53.65293485

214.35

350.63

272.75

1.330381036

8633.855
42.7259379
7

6002.225

9957.625
51.2534770
4

54.31812537

61.2870122

CARCASS TREND
OIL RATE CHANGE WITH TIME

0.286711292

44

TANGENTIAL AIR RATE CHANGE WITH TIME

AIR RATE CHANGE WITH TIME

45

CHANGE OF REACTOR EFFICIENCY WITH TIME

CAT 6 DATA SHEET

46

Reactor_6_
GAS
(LINE 1)
TIME (A.M.)
9:43

9:51

10:01

10.13

10:21

10:31

10:41

10:51

29-0612 FRIDAY
GRADEN374
SFS (CBM)
(Nm3/hr)
642.6
640.2
647.9
645.5
645.8
646.8
643.5
646.2
638.6
640.8
644.9
640.3
642.4
644.2
641.1
639.6
645.3
649.7
649.3
646.7
645.2
643.7
643.5
645.3
639.6
643
639.3
636.4
643.6
643.1
646.7
649.3
642.5
639.2
646.4
641.7

AIR RATE

MAKE OIL

(Nm3/hr)
10520
10498
10514
10553
10517
10500
10450
10443
10494
10497
10619
10495
10502
10505
10477
10499
10497
10532
10518
10486
10519
10485
10457
10521
10495
10461
10518
10460
10483
10542
10514
10490
10436
10442
10572
10497

(kg/hr)
3688.31
3654.16
3728.21
3719.02
3680.94
3720.37
3698.53
3697.66
3687
3719.82
3673.1
3726.97
3649.34
3677
3676.34
3682.3
3679.77
3726.68
3712.23
3685.19
3686.67
3727.34
3721.36
3713.09
3694.14
3722.35
3675.45
3695.11
3727.4
3710.95
3694.38
3707.85
3697.88
3683.32
3750.11
3661.03

47
640
639

10481
10507

3781.44
3741.8

649.7

10619

3781.44

636.4
13.3
643.05
3.31738920
3

10436
183
10527.5
35.8478688
5

3649.34
132.1
3715.39
27.447952
15

10:59
MAXIMUM
VALUE
MINIMUM
VALUE
DIFFERENCE
AVERAGE
S.D.

CAT 6 TRENDS
SFS CHANGE WITH TIME

48

AIR RATE CHANGE WITH TIME

MAKE OIL RATE CHANGE WITH TIME

49

CALCULATION OF CHOKE
VELOCITY
VALUES
G
V
B
P

UNITS

24000

26000

28000

5.2

5.2

5.2

Tf
C
D

1910

1910

1910

10

10

10

Ac
C
V

0.545415

0.545415

0.545415

1469.452

1591.906

1714.36

FULL FORM

ft3 /hr

combustion gas
volume

psig

bustle pressure

sq.ft

flame temperature
equivalent choke
diameter
cross-section area of
choke

ft/sec

choke velocity

ft

NOTE:
>Choke velocity is the rate at which tail gas passes through a given cross sectional ar
region.
>Here combustion gas volume is equal amounts of input air and coal bed methane.

>Bustle pressure is the pressure of the system where air and fuel or oil enters the rea
>Flame temperature is the temperature after fuel
combustion.

50

CAT REACTOR AND VENTURI

REACTION VOLUME CALCULATIONS
DIMENSI
ONS

VALUE

UNIT
S

R1

inches

R2

7.23

inches

L1

12

inches

L2

50

inches

inches

D1

inches

D2

15

inches

FULL FORM
radius for frustum of right cone &
choke region
radius for breeching
region
length for choke
region
length for breeching
region
height for frustum of right
cone
diameter for choke
region
diameter for
breeching region

SECTION 1: FRUSTRUM OF RIGHT CONE(CONVERGING

SECTION)

51

V1

814.2413
35

cubic inches

volume 1

cubic inches

volume 2

cubic inches

volume 3

cubic inches

total
volume=V1+V2+V3

SECTION 2: CHOKE REGION

V2

603.1857
89

SECTION 3: BREECHING
REGION

V3

8835.729
34

TOTAL REACTION VOLUME

10253.15
65
5.933539
62

cubic feet

NOTE:
>The reaction volume is defined as the internal volume of the react
from the oil spray position to the 1st (primary) quench water spray

CALCULATION OF REACTION TIME

VALUES
GV

UNITS

24000

24000

24000

24000

Tf

1910

1910

1910

1910

Tr

1860

1810

1760

1710

RV

5.93354

5.93354

5.93354

5.93354

RT

197.362
9

199.489
7

201.662
8

203.883
7

FULL FORM

(SCFH) tail gas volume

F

F
cubic
feet

flame temperature
back calculated
reaction
temperature
reaction volume

reaction time

52

NOTE
:
>Reaction time is the amount of time it takes from the injection of the oil
to the first cut off spray.

THEORETICAL FLAME TEMPERATURE (SHORT

CUT METHOD)
CBM(Nm3/hr)
Sp.Heat
CBM(kcal/Nm3)
Vair(SCFH)
Tair(deg.C)
Tair(deg.F)
Sp.Heat
air(BTU/cuft/degF)
Heat from

750
8450
13750
760
1400
0.0183
49.03288

53
oil(BTU/cuft)
Heat from
air(BTU/cuft)

201
25.62

Heat Input(BTU/cuft)

74.65288
201

flame temp(degC)

1879.057
64

NOTE:
>Flame temperature is the temperature after fuel
combustion.

YIELD & PRODUCTION CALCUTIONS

GAS COMPOSITION

(% VOL)

CO2

6.48

O2

CO

19.88

CH4

0.4

H2
C2H2

N2

63.76

% C OUT WITH GAS

26.76

operating conditions
CONV.OIL( KG / HR )

5200

SFS( KG / HR )

631

{AIR( NM3 / HR )+ATM AIR}

13100

C CONTENT IN M.O.%

89.34

C CONTENT IN SFS%

89.34

ATOMISING AIR

350

CF in (carbon in from fuel) (lb C/hr)

CO in (carbon in from oil) (lb C/hr)
TC in (total carbon in) (lb C/hr)

563.735
4
4645.68
5209.41
54

54

TC out (total carbon out in gas) (lb C/hr)

2331.98
75

CB (carbon black production) (lb/hr)

2877.42
79

YIELD %( ON M.O.)
YIELD %( ON M.O.+ SFS)

55.3351
52
49.3470
75

NOTE
For TC out
>mol.wt of C=12.011
>% of N2 in flue gas=79
>1 lb=2.2 kg
>379.43 cu. Ft is contained in 1
mol of a gas
>.0268 is to convert cu. Nm to
SCFH

PROBLEMS WITNESSED IN PCBL DURGAPUR

REACTOR: One port valve of the choke section melted and fell off due
to which there was a huge fountain of dangerous sparkles which flew
both horizontally and vertically. Immediately the reactor (CAT 4) was
shut down and steam was passed through all nozzles.

55

REASON: Failure of the port valve due to localized heating resulting in

melting of the metallic components of port valve.
CORRECTIVE MEASURE: The damaged part of the refractory was
recasted with refractory lining and a new port valve was introduced. A
pipe was installed above them which supplied water continuously to
cool the surface.

PELLETISER: The parallel pelletizers in LINE 3 (CARCASS) were not

giving adequate pellet size distribution.

56

REASON: 1 pelletiser (ME 415) was 4 months old while the other (ME
416) was 2 weeks old. The problem was in the ME416 and not in
ME415.
CORRECTIVE MEASURE: - changing the ME416 with new pins
- Some modification in terms of water jet position across the pelletiser
- New jet nozzles to create high pressure water
- High RPM
sorted the problem during the production run of P435. The pellet size
distribution varying from 2 % to 24% was reduced to 2% maximum in
10 mesh retention. (Optimum parameter for pellet size distribution on
page 12, last paragraph).

WAREHOUSE: A visit of the LINE 3 warehouse showed that there was

immense amount of carbon black spillage in the area. Also, packing
and storage being in the same place often led to the packed bags
getting dirty.
The wooden pallets, on which the bags were kept, were broken at
different places. This invited a risk of the paper bags getting damaged
during transportation & loading.

57

CONCLUSION
A study of the reactors involved in the production of carbon black at the
PCBL factory was done. The process of carbon black manufacturing was
understood right from the basic raw material up to the packing and loading
stage.
Different quality tests (online as well as final) pertaining to carbon black
were also seen as well as carried out by hand.
An understanding of the behavioral pattern of the main reactor parameters
was made.
A fair idea was gained regarding the variability of the parameters.
Certain data of main parameters of the reactor were taken for different lines
on a basis of 1 or 2 minutes difference. This gave a micro analysis of the
variability in the parameters as compared to the macro analysis carried out
by the company itself, where data is taken every 2 hours.
Variability analysis of SFS flow in CAT reactor on flame temperature has been
done. It has been observed that for every 1 unit of heat input (BTU/hr), there
is a 20C variability in the flame temperature.
Make oil variability has also been found. It has been understood that Make
Oil variability has a higher impact on Iodine number and lesser impact on
DBP.
Air change has an impact on the combustion ratio.
Only a micro level analysis has been carried out. However on a macro level,
the variability will be minimized.

58

A correlation of process parameter variability with the characteristics of

product can be carried out for better understanding of the process
parameters on product characteristic.
Reactor yield analysis has also been carried out.
The management has collaborated with the consultancy firm Mckinsey for
yield improvement.
The following changes have also been carried out:

Changing the dynamic flow pattern of fuel (either CBM or Oil), based
on computerized fluid dynamics.

Water cooled nozzle spray at Make Oil locations of the choke.