In-Plant Training: Aadithiyasekaran G Kaviya S M N Rashmi
In-Plant Training: Aadithiyasekaran G Kaviya S M N Rashmi
In-Plant Training: Aadithiyasekaran G Kaviya S M N Rashmi
In-plant training
(May 14th, 2018 – June 14th, 2018)
AADITHIYASEKARAN G
KAVIYA S M
N RASHMI
(B.TECH CHEMICAL ENGINEERING, AMRITA SCHOOL OF ENGINEERING)
SRF LIMITED – TECHNICAL TEXTILES BUSINESS
We sincerely thank Mr. Ashok Malhotra for his guidance and encouragement in
carrying out this internship work. We also wish to express my gratitude to the
officials and other staff members of SRF Limited who rendered their help during
the period of our work.
TABLE OF CONTENTS
S No. Title Page No.
1. ABOUT SRF LTD 4
2. INTRODUCTION TO THE RAW MATERIAL 65
3. POLYMERIZATION 6-16
3.1 Lactam melting
3.2 Lactam preparation
3.3 Polymerization
3.4 Extraction
3.5 Solid state polymerization (SSP)
3.6 Recovery
4 SPINNING 16-17
4.1 Chip feeding
4.2 Spinning and quenching
4.3 Drawing and take winding
5 TWISTING AND WEAVING 17-18
6 DIPPING 18-20
7 QUALITY ASSURANCE 21-22
8 INDUSTRIAL YARN BUSINESS 23-24
SRF Limited was listed in the 2011 Asia's Best under a Billion lists by Forbes
magazine.
2. INTRODUCTION TO THE RAW
MATERIAL
The initial raw material for the process is Caprolactam (CPL), an organic
compound with the formula of (CH2)5C(O)NH. Caprolactam occurs as white
hygroscopic flakes or a crystal with a distinctive odor and is a lactam (a cyclic
amide) of caproic acid. This is the material used to make nylon-6 chips through the
polymerization process. It is being sourced from CPH, GSFC and Zaklady, BASF
and FACT.
After being pumped from the lactam storage tank (NPL), the virgin lactam is
mixed with DM water, lactam from monomer recovery process and
de-polymerization process, and blended in a static mixer. The whole process of
lactam preparation is maintained under N2 blanketing for inert atmosphere, setting
the flow rate of the N2 at the range of 30-40 litres per minute. The lactam if left
with oxygen will oxidize and will present itself with a yellow tint. Therefore, the
lactam now is deoxidized before being sent to any further process. Now, the lactam
from the mixed pure lactam tank (MPL) is made to pass through series of filters to
remove the impurities. From there the lactam is sent to the de-oxy unit. The
de-oxygenation takes place in an evaporator under vacuum of 500 mmHg. From
now on all the vessels which handle the lactam will be blanketed with nitrogen.
The deoxygenated lactam is pumped from the bottom of the evaporator to the inlet
of first poly through pre-heater by which the temperature is increased nearly to
reaction temperature of 135±5 °C.
3.3 POLYMERIZATION
1. Initiation: The Lactam ring is split open by the free radical of the catalyst.
CO-(CH2)5-NH + H2O COOH-(CH2)5-NH2 (Amino Caproic Acid)
2. Poly-addition
COOH-(CH2)5-NH2 + CO-(CH2)5-NH
(COOH-(CH2)5-NHCO-(CH2)5-NH2)m+1
(Adduct)
3. Poly-condensation
(COOH-(CH2)5-NHCO-(CH2)5-NH2)m+ (COOH-(CH2)5-NHCO-(CH2)5-NH2)n
(-CO-(CH2)5-NHCO-(CH2)5-NH-)m+n+
H2O
The lactam from the pre-heater enters the first poly reactor. The lactam mixture is
heated in the reactor which consists of a jacket containing Dow-therm oil of
temperature 270 °C which is in-turn heated by a Santo-therm re-boiler
[Santo-therm oil] at a temperature of 350 °C. The jacket temperature of this reactor
269-271.5 °C, which is controlled by temperature indicating control system (TICS)
and the jacket pressure is 0.5 kg/cm2, which is controlled by pressure indicating
control system (PICS). An endothermic reaction occurs in the 1st poly reactor. The
water evaporated at the top of the 1st poly is condensed by the condenser. The
condensed water is sent to concentration process for lactam recovery. The lactam
mixture from the 1st poly is supplied to the 2nd poly with help of a gear pump.
3.4 EXTRACTION
This process is used to polymerize the OG chips which are not of adequate degree
of polymerization. The extracted chips which are passed into the centrifuge are
de-hydrated and fed into the mixing tank. The additives A-1 [Potassium bromide]
and A-2 [Potassium iodide] which are used for heat stabilization of tire cord are
added in a powder state. A given amount of the additives are thrown into the
respective preparation tanks which contains a specific amount of DM water. The
solution is agitated by an agitator and dropped by gravity into the additive feed
tank and mixed. The mixed solution is pumped by the additive feed pump and
mixed in the mixing tank once again along with the extracted chips by an agitator.
The un-dried chips are fed to the top of the tower and moved down to the bottom
of the tower continuously being contacted with nitrogen flow of high temperature
in counter. The SSP tower consists of three zones with decreasing diameter. The
upper zone is the pre-drying zone which requires a lot of energy to evaporate water
and large amount of nitrogen is blown. The velocity of nitrogen gas is maintained
below terminal velocity to avoid fluidization of the chips in the tower. The middle
zone is the drying and polymerizing zone. It has high temperature nitrogen with
low dew point to obtain high molecular weight polymer and low water content.
The lower zone is for cooling the FD chips and is transferred to silo.
NITROGEN RECOVERY
SIGNIFICANCE OF N2-
1. Maintaining inert
atmosphere.
The top two nozzles of N2 gas are at temperatures of 164 – 167 °C.
The extracted water from the extracted water receiver is supplied continuously the
1st evaporator. Before passing it into the evaporator, the extracted water is heated
in a pre-heater to match the conditions in the evaporator. The mixture is partially
concentrated and sent to the 2nd evaporator. The concentrated liquid that flows out
of the 2nd evaporator is fixed at a concentration by controlling the vacuum degree
and liquid temperature at around 72 °C. The 1steffect inlet has a concentration level
of 10-12 %, which gets concentrated to 20% and in the 2nd effect it gets further
concentrated to 70-75%. Both the effects are maintained under vacuum to facilitate
flashing. The 1st and 2nd effect is under 450-500 mmHg pressure. The concentrated
solution is called LDL [concentrated lactam through concentration process] is
collected in a concentrated lactam tank and sent to distillation batch wise. A
portion of the evaporated water from the 1st effect is collected through the
thermo-compressor and water from the 2nd effect is collected in the condensate
tank and transferred to extraction process for recycle.
The distillation is used to purify the crude lactam that is LDL, ADL and AEL. The
distillation still is heated up to a temperature of 125 °C. This is when the first
reflux starts. The water vapor in the column starts moving into the vapor column
under a pressure of 560 mmHg. The water vapor is then condensed in a condenser
and goes to the seal pot. This water is then sent to the water storage tank through
the water cut line. Once this is completed the 2nd reflux starts when the distillation
still reaches a temperature of 150 °C. The lactam vapor is sucked by the vapor
column at a pressure of 760 mmHg. The vapor is passed through condenser where
the water is passed on the tube side at a temperature of 50 °C and vapor on the
shell side at 150 °C. The vapor gets condensed to about 70 °C and is passed onto
the seal pot. The lactam mixture is passed through the over flow of the seal pot. A
portion of the distillate (10%-15%) is pumped back into the distillation still as a
reflux. The main distillate of LPL or APL is collected in the LPL or APL receiver
respectively through the LPL or APL main cut. The final product is transferred to
the respective storage tanks through an over flow pipe at the receiver. The LDL or
ADL is supplied batch wise to the distillation still which is maintained under high
pressure and high temperature. The residue of LDL is stored in the IDL receiver
and is used as the liquid input in the de-polymerization reactor. The residue of
ADL is discarded in the residue pit at the bottom of the distillation column.
4 SPINNING
4.1 CHIP FEEDING
Fully dried chips [of melting point-220 °C] are fed to chip receiver silo 1 from FD
silo through powder separator under nitrogen atmosphere and then FD chips are
blended with heat stabilizer additive special mixer (ASM) under nitrogen
atmosphere further the ships are fed to chip receiver silo 3 (batch wise) through
chip receiver silo 2 by gravity. CRS 2 is used to isolate the ambient conditions and
reduce unnecessary system failure. In ASM tank, additive used is CuI (cuprous
iodide). It is used because it acts as a thermo-stabilizer. CuI is added in the ratio of
1:5000 with the fully dried chips. The capacity of CRS 1 is 1.4 tonnes, CRS 2 is
0.8 ton and CRS 3 is 5 tonnes. The CRS 2 and CRS 3 are maintained under
vacuum and nitrogen.
Twisting is done in a 2 steps process. The first one being single ply twisting, in
which the yarn is twisted in its own axis. The bobbin contains a traveler which
rotates at a speed of 6000rpm. The traveler enhances the motion of the twisted yarn
in a to and fro motion. Yarns with different deniers are twisted in the same manner
with their respective operational conditions. The second one is the double ply
twisting. In which, two single ply yarns are twisted using rollers and taken up as a
single yarn. After the winding of double ply yarn, the yarn now is sent to weaving
so that the ability of the fabric to dip and make into cord is improved. In weaving,
the yarn is weaved into a fabric and sent to dipping. The number of bobbins used
for weaving can vary with style's specifications. The fabric consists of two parts
warp and weft. The warp is the nylon fabric from twisting and the weft is the
cotton threads which is interlaced axially with the fabric. Weft binds the fabric.
Polyester can be also used. Cotton is used because it has less strength and
inexpensive. Thus, the weaved fabric is stretched and rolled up in a huge roller and
sent to dipping process.
6 DIPPING
The final stage in tyre cord manufacturing is Dipping. In this process, the twisted
and weaved yarns get dipped into a solution.
The above-mentioned factors are improved using 3 T's [Temperature, Tension, and
Time].
The process starts with the let off roller, from which the fabric from the spindle
passes into the let off accumulator. The let off accumulator accumulates the last
part of the fabric from the roller. Further, the fabric is sent to pull roller stand
(PRS-1A) where the PRS stretches the fabric at a speed of 74 m/min (approx.). The
height of the PRS is 80m throughout the process. After the Stretching by PRS-1A
the fabric is sent to the dip station for the fabric to pick up the adhesive material
which in future will be used to coat the rubber on it. The dip station solution is
RFL (Resorcinol formaldehyde latex), which is prepared batch wise in a separate
tank with two setups. The first is called the resin mixing tank, where the formalin,
resorcinol and DM water is being mixed and is agitated for 5.5hrs at a temperature
of 22-25℃. From there this solution is transferred to the final batch tank or ageing
tank. In this tank, VP latex (Vinyl pyridine) and DM water are added and mixed.
The lifetime of this batch is 72hrs. The output is taken as RFL. When the tyre cords
are layered there is no adhesiveness for the cord to stick on to the rubber.
Therefore, the RFL solution is being applied on the grieve fabric to increase the
adhesiveness with rubber. The Ammonia vapors from the dipped fabric are sucked
by the vacuum column also known as de-webber system. The dipped fabric is sent
to PRS 1-B which rotates at a speed of 75 m/min. Now the fabric undergoes
process two zones (two driers) in series. First drier is the pre-drying zone and it
contains 6 zones of rollers in which the fabric undergoes tension. The temperature
of Drier 1-A is about 135℃. Further, the fabric is dried completely in the Drier 1-B
(6 zones) which is at temperature of 140℃. During this series of drying, the fabric
gains a dip tension of 2%. After drying, the fabric then rolled on PRS-1 which
speeds up to 76m/min. The RFL vapors are sucked by the de-webber system to
maintain the TSC (Total solid content) in RFL which is about 21%. Now, the
fabric is sent to series of driers to enhance the structural properties of the fabric.
The dipped tyre cord sent to Drier-1, which has 4 zones for heating the nylon tyre
cord fabric. This tyre heats up the fabric up to 210℃ with the 4 zoned heating
processes. From there, the fabric is being maintained at a temperature of 210℃.
During this series of drying, the fabric is being stretched under heat to an extent of
8%. Now the fabric is subjected to PRS-3 which the Master PRS which speeds up
to 80m/min. Furthering the fabric to normalize in two driers. Both driers are at
temperature of 210℃ which is maintained to provide the uniformity to the fabric.
During this normalization process, the fabric contracts by -2.5% (relaxation).
Relaxation happens to give the compatibility and dimensional stability over a
period. Then the fabric rolled on PRS-5 which has a speed of 79m/min. The fabric
is then sent to a unit called Flexibliser, which reduces the stiffness gained by the
fabric during dipping. Following the process, the fabric is sent to PRS-6 and wind
up accumulator accumulates the processing fabric and feeds to wind up feed rollers
stand. Then the fabric is winded by surface winder which in turn taken to package.
7 QUALITY ASSURANCE
There are few criteria followed in QA for testing the samples such as
1.Quality plant
2. Specifications
3. Test procedures
4. Record/ Reports
Samples to be tested:
1. Polymerization Process-
Caprolactam, KI, KBr, Ortho Phosphoric acid, KMnO4, Di-Hydraxine
Carbonate, DM Water
2. Dipping-
Resorcinol, Formaldehyde, Latex, Ammonia.
3. Spinning-
Terran, Paraffin Oil, CuI, Nitrating Mixture.
4. IYB-
AB, CuCl2, Magnesium Stearate, Vegetable Oil.
The below listed are few basic tests which are tested in QA.
PMV Test-
This test is applied for Caprolactam. Permanganate value is calculated to
verify the purity of the raw material. In this test 1g of lactam is diluted with
DM water and made up to 100ml. 1 ml of N/100 of potassium
permanganate is added to the made-up solution maintaining the
temperature at 20 ℃. Compare the permanganate colour. Usually, Grade-1
lactam takes 6 to 8 hours of process time.
Oxidation Test-
This test is processed for FD chips.
This test is done to verify whether the FD chips are oxidized to external
factors or not. In this test, take certain amount of FD chips and subject it to
UV light. If the colour observed is pink, the chips are not oxidized, or the
chips emits a glowing colour (Neon tint), then the chips are oxidized to
external atmosphere.
Colour Test-
This test is done through naked human eye.
The industrial yarn business is a sector that deals with yarn production for
applications like, fishing nets, defence applications, jersey & jackets, footwear, bag
handles etc. The yarn produced in this unit, unlike TTYB varies from 100 deniers
to 2500 deniers. Yarn in the range of 100 to 700 deniers is called low denier yarn
and above 700 is called high denier yarn. The FD chips are outsourced from
Gujarat and Russia. The obtained FD chips are fed into the silo in batches of
625kgs. The FD chips are then transferred to the Nauta mixer where 0.3% of AB
(2-mercaptobenzimidazole), 0.15% of SM (magnesium stearate) and 0.015% of
CuCl2 is added in case of high denier requirements. There are six Nauta mixers
and two of them will process for coloured yarn. Similarly, for low deniers, the
composition varies as 0.05% of AB, 0.025% of SM and 0.015% of CuCl2 is added.
This mixture is prepared for one hour and sent to the hopper, from where it is sent
continuously to the extruder. There are six hoppers which get feed from NM batch
wise. Meanwhile, the colour that must be incorporated onto the yarn is obtained
from pigments, which are heated at a moderately high temperature and are added to
the chips just before they are sent to the extruder. There are fifteen extruders in
total. Each extruder gets four positions but three of them gets five positions. Hence
there are sixty-three positions with metering pump. A dowtherm at a temperature
of 280 degree centigrade is provided in the extruder, which is heated with the help
of an electrical heater and in turn melts the lactam. The screw inside the extruder
rotates at 100 rpm and pushes the lactam in the spin pack where the chips are
filtered. The molten polymer is distributed among the four positions with the help
of the gear pump (one for each position) and is passed into the spinneret. The
lactam is heated to a temperature of 330 degree centigrade and passed down as
filaments (6 – 8 DPF) in the respective spinneret according to the denier
requirements. The coloured filaments are passed through separate extruders and
spinnerets that are meant for coloured Yarn only. The filaments from the spinneret
are sent into the quench chamber which blows cool air at a temperature of around
13 – 15 degrees centigrade and partially crystallizes the filaments. The undrawn
yarn spun and quenched are fed into the 1st drawing zone where yarn is applied
with sin finish oil. The finish oil contains 200 litres of DM water, 190ml of OM27
(an anti- bacterial agent) and 46 litres of simmer oil. The filaments dipped in the oil
are stretched i.e. drawn to 5 times its initial length in 2 stages. In the 1st stage it is
drawn by stress induced elongation and in the second by temperature induced
elongation. The yarns are produced as two halves i.e. if you require yarn of 420
deniers, two bobbins of 210 denier each are produced. The stretched yarns from
the 1st stage is taken to the second (as they are unstable) and are slightly twisted to
make the two halves one. The yarn from the two bobbins are taken up in the take
up winder and are heated to a temperature of 180 degree centigrade and slightly
twisted and woven onto to the spindle. This yarn is then sent for sales.