MANUFACTURING OF LINEAR LOW

DENSITY POLYETHYLENE (LLDPE)

(960 TPD)


PROJECT REPORT

SESSION 2012-2013



Submitted to Panjab University, Chandigarh
In Partial fulfillment of the requirement
For the degree of

BACHELOR OF ENGINEERING (CHEMICAL)
2013



PROJECT GUIDE:
Dr. SUKHMEHAR SINGH



SUBMITTED BY:
BHAGWAT BHARDWAJ
ROLL NO. CH-9217



DR. S. S. BHATNAGAR UNIVERSITY INSTITUTE OF
CHEMICAL ENGINEERING & TECHNOLOGY
PANJAB UNIVERSITY, CHANDIGARH


MANUFACTURING OF LINEAR LOW DENSITY POLYETHYLENE
(LLDPE)
(960 TPD)


Linear low-density polyethylene (LLDPE) is a substantially linear
polyethylene, with significant numbers of short branches, commonly made by
copolymerization of ethylene with longer-chain olefins. Linear low-density
polyethylene differs structurally from conventional low-density polyethylene
because of the absence of long chain branching. The linearity of LLDPE results
from the different manufacturing processes of LLDPE and LDPE. In general,
LLDPE is produced at lower temperatures and pressures by copolymerization
of ethylene and such higher alpha olefins as butene, hexene, or octene. The
copolymerization process produces an LLDPE polymer that has a narrower
molecular weight distribution than conventional LDPE and in combination with
the linear structure, significantly different rheological properties.
Production and properties
The production of LLDPE is initiated by transition metal catalysts, particularly
Ziegler or Philips type of catalyst. The actual polymerization process can be
done in either solution phase or gas phase reactors. Usually, octene is the
copolymer in solution phase while butene and hexene are copolymerized with
ethylene in a gas phase reactor. The LLDPE resin produced in a gas phase
reactor is in granular form and may be sold as granules or processed into
pellets. LLDPE has higher tensile strength and higher impact and puncture
resistance than LDPE. It is very flexible and elongates under stress. It can be
used to make thinner films, with better environmental stress cracking
resistance. It has good resistance to chemicals and to ultraviolet radiation. It has
good electrical properties. However it is not as easy to process as LDPE, has
lower gloss, and narrower range for heat sealing.
Processing
LDPE and LLDPE have unique theoretical or melt flow properties. LLDPE is
less shear sensitive because of its narrower molecular weight distribution and
shorter chain branching. During a shearing process, such as extrusion, LLDPE
remains more viscous and, therefore, harder to process than an LDPE of
equivalent melt index. The lower shear sensitivity of LLDPE allows for a faster
stress relaxation of the polymer chains during extrusion, and, therefore, the
physical properties are susceptible to changes in blow-up ratios. In melt
extension, LLDPE has lower viscosity at all strain rates. This means it will not
strain harden the way LDPE does when elongated. As the deformation rate of
the polyethylene increases, LDPE demonstrates a dramatic rise in viscosity
because of chain entanglement. This phenomena is not observed with LLDPE
because of the lack of long-chain branching in LLDPE allows the chains to
slide by one another upon elongation without becoming entangled. This
characteristic is important for film applications because LLDPE films can be
down gauged easily while maintaining high strength and toughness. The
rheological properties of LLDPE are summarized as "stiff in shear" and "soft in
extension". It is not taken in most curbside pickups in communities. LLDPE
can be recycled though into other things like trash can liners, lumber,
landscaping ties, floor tiles, compost bins, and shipping envelopes.
Process types :-
1) Slurry process: - it is also called basells hastalen slurry process. It
consists of two continuous stirred tank reactors operated in parallel or in
series according to the grade of polymer required. The process is
designed to produce uni or bimodal polymer using Ziegler Natta
catalyst. The polymer is produced at relatively low temperature ( 70 -
110
o
C ) and low pressure ( 1 - 5 MPa ) in a saturated hydrocarbon
medium. The polymer form suspension or mobile slurry. The reaction
medium is removed and polymer is separated from the hydrocarbon inert
diluents. The obtained powder is mixed with stabilizers and generally
extruded into pellets.
2) Gas phase process: - In this process the catalyst and the co-monomer
are fed to a slurry stirred reactor in which pre polymerization occur. Pre
polymerization under mild conditions help to prevent hot spots or it will
hinder the process. The polymer is transferred to a dryer where hot
nitrogen evaporates the solvent. Then the polymer powder acts as a
catalyst for the main polymerization reactor and is fed continuously to
the fluidized bed reactor.
The fluidization reactor comprises of two main parts
- Cylindrical part
- Disengagement part
The cylindrical part is equipped with gas distribution in order to fluidize
the content of the bed.
The disengagement reduces the velocity of flowing gas and constantly
disengages the polymer particle from output gas.
Finally, the gases are compressed and returned to bottom of the reactor
ethylene, butene, or hexane, H
2
as a chain terminator and N
2
as an inert
gas is introduced at different points to assure perfect mixing and prevent
condensation which could damage the blades of the compressor.
The circulating gas fluidizes the bed and removes the heat of the
reaction.

Comparison of Gas phase process and slurry process :-
- In slurry process due to use of solvent, same additional
equipments is required like solvent stores , purifiers etc. therefore
gas phase processes are
- More compact - simpler - have lower cost - environmental impact is less
- In gas process, it creates no wall sheeting or fouling due to the
ployethenes solubilities in solvent medium which is the main
problem in slurry process.
- In slurry process there are some useful points like
- Mild operating conditions
- Ease of heat removal
- Ease of processing
- high monomer conversions
- In gas phase process, production of more off spec polymer during
grade change especially changing from 1 catalyst to another catalyst
type.
- In gas phase process, agglomeration and lump due to poor heat
removal from growing polymer practices leading to the formation of
hot spots followed by sintering of the polymer.
- In gas phase process, disintegration of growing polymer particle
due to undesirable stress leading to the formation of fines. Increasing
the fines content in the gas phase reactor is catastrophic for all gas
phase plants, leading a loss of homogeneity of fluidization and
eventually leading to the blockage of subsequent process unit.
- In gas phase process, electrostatic charge leading to agglomerate
formation are wall sheeting especially near the inclined part of the
disengagement zone of gas phase reactor.
- Slurry reactors have a very efficient heat removal and wide co
monomer range but the product range is limited due to solubility of the
produced polymer.

Application
LLDPE has penetrated almost all traditional markets for polyethylene, it is used
for plastic bags and sheets (where it allows using lower thickness than
comparable LDPE), plastic wrap, stretch wrap, pouches, toys, covers, lids,
pipes, buckets and containers, covering of cables, geomembranes, and mainly
flexible tubing. In 2009 the world market for LLDPE reached a volume of
almost 24 billion US-Dollars (17 billion Euro).
[1]
LLDPE manufactured using
metallocene catalysts is labeled mLLDPE.
Physical Properties
Table-1
Property Value
Density 0.92 g/cm
Surface hardness SD48
Tensile strength 20 MPa
Flexural modulus 0.35 GPa
Notched izod 1.06+ kJ/m
Linear expansion 2010
5
/C
Elongation at break 500%
Strain at yield 20%
Max. operating temp. 50 C
Water absorption 0.01%
Oxygen index 17%
Flammability UL94 HB
Volume resistivity 10
16
cm
Dielectric strength 25 MV/m
Dissipation factor
1 kHz
909090
Dielectric constant
1 kHz
2.3
HDT @ 0.45 MPa 45 C
HDT @ 1.80 MPa 37 C
Material drying NA
Melting Temp. Range 120 to 160 C
Mould Shrinkage 3%
Mould temp. range
20 to 60 C




GRADE
PROPERTIES
FEATURES APPLICATION
M.I. DENSITY (gm/cm)
STRESS
EXPONENT
COLOUR
W50A009 0.7 - 1.0 0.950 - 0.954 1.45 - 1.55 >50
Excellent
processability with
optimum balance of
tape strength and
elongation.
Stretched tape for woven
fabric, jumbo bag,
tarpaulin.
I60A080 7.5 - 9.0 0.957 - 0.960 1.2 - 1.25 >60
Excellent
processability with
optimum balance of
mechanical
properties & low
degree of warpage.
General purpose, multi
purpose, vegetable crates
etc.
I60U080 7.5 - 9.0 0.957 - 0.960 1.2 - 1.25 >60
UV stabilized,
excellent
processability with
optimum balance of
mechanical
properties & low
degree of warpage.
Soft drink crates,
Vegetable crates, milk
crates etc.
I50A180 19 - 23 0.950 - 0.954 1.2 - 1.3 >55
Excellent
processability with
optimum balance of
mechanical
properties & low
degree of warpage.
Household containers like
bucket, mug etc.
S56A010 0.7 - 1.0 0.950 - 0.954 1.45 - 1.55 >50
Excellent
extrudability, and
good balance
between liner
strength and knot
strength.
Low denier application like
fishing net, mosquito net
etc.
E45A003 0.5 -0.7 0.943 - 0.946 2.0 - 2.1 >50
conform to DOT
specifications for
JFC.
Telecommunication for
sheathing.
P41A004 0.39 - 0.43 0.938 - 0.941 1.70 - 1.90 >45
Excellent
processability,
ESCR, carbon black
dispersion, abrasion
resistance. tape
strength and
elongation.
Coating on steel pipes
used for gas
transportation.
C43D006 0.64-0.75 0.945 - 0.948 2.0 - 2.1 >55
conform to DOT
specifications for
JFC.
Base resin for cable
insulation applications.





























RESIN
TYPE
GRADE M.I.
DENSITY
(gm/cm)
STRESS
EXPONENT
COLOUR FEATURES APPLICATION
FILM
F20S009
0.8 -
1.1
0.918 -
0.921
1.25 - 1.35 <0
Excellent
processability, with
optimum balance
between
mechanical &
optical properties.
Low gel count,
resistance to
leakage & pinholes,
excellent sealing
characteristics.
General purpose
film, liquid
packaging film,
lamination film. F20S020
1.8 -
2.1
0.918 -
0.921
1.25 - 1.35 <0
E20AN009
0.8 -
1.1
0.918 -
0.921
1.25 - 1.35 <0 Non slip film.
Lamination, cling
film
FILM-
OCTENE
O20S009
0.8 -
1.1
0.918 -
0.921
1.25 - 1.35 <0 Octene film grade.

INJECTION
MOULDING
I24A530
50 -
60
0.922 -
0.927
1.25 - 1.35 >50
Excellent gloss &
high flow.
Caps and closures,
shopping baskets,
master batch.
EXTRUSION
COATING
E36A060
6.0 -
8.0
0.920 -
0.923
1.2 - 1.3 >45
Excellent
processability.
Extrusion coating
on HDPE woven
fabrics.
ROTO
MOULDING
R35A042
4.0 -
5.0
0.933 -
0.939
1.2 - 1.32 >40
Excellent
processability&
impact strength.
Outdoor storage
tanks, toys.
RAW MATERIALS AND SUPPLY

Monomer: Ethylene (C
2
H
4
) from natural gas after recovery of C
3
and C
4

gases.

Comonomer: butane- I

Solvent : cyclohexane C
6
H
12
ethylene is highly soluble in cyclohexane most
of C
6
H
12
is recovered from operation but make up is required.

Catalyst: a mixture of Titanium tetrachloride ( TiCl
4
) and Vanadium
Oxytrichloride ( VOCl
3
)

Chain transfer and terminating agent: hydrogen ( H
2
)

Catalyst deactivators: Pentadione
Pelargonic acid ( C
8
H
17
COOH )
Purification medium: molecular sieves
Silica gel
Activated alumina

Polymer additives: antioxidants and UV stabilizers.



Process block diagram





STRIPPING &
BLENDING
BAGGING
FINISHED PRODUCT
OFF GASES & GREASE
TO VAPOURIZER
EXTRUSION &
PELLETIZATION
ADDITIVES
POLYMER
SEPERATION
SOLUTION
ADSORBER
POLYMERIZATION
CATALYST
PREPERATION
ALUMINA
SPENT ALUMINA
PURIFICATION
MONOMER
SOLVENT
SOLVENT
RECOVERY
MONOMER
SOLVENT
MAKEUP SOLVENT
ETHYLENE
PROCESS DESCRIPTION

- REACTION AREA
The process solvent, cyclohexane through purifiers (35
o
C & 4 kg/cm
2
) is
combined with co-monomers Butene-1 / Octene-1, & pumped to
absorber cooler, ethylene from Outside Battery Limits after passing
through purifiers is dissolved at absorber cooler in cyclohexane +
butene-1 stream to form reactor feed solution.

This solution stream is pumped by reactor feed pump (45
o
C & 170
kg/cm
2
) is tempered to achieve reaction feed temperature & then solution
is catalytically reacted to produce poly-ethylene in solution.

The reaction area includes two main reactors : a pipe reactor & a stirred
autoclave reactor (250
o
C & 155 kg/cm
2
) & finally a trimmer reactor
(270-300
o
C). The combination of reactor will be used as per grade
requirement. The catalyst causes ethylene & co-monomers to polymerize
exothermically (93-95% conversion). Hydrogen is used as chain
terminator injected in solution before entering the reactor.

The liquid stream leaving the reactor contains polyethylene
(approx.20%) dissolved in cyclohexane together with un-reacted
ethylene and butene-1. Deactivator is then added to terminate the
reaction & solution is passed through solution pre-heater (295-310
o
C),
then second deactivator is added to promote efficient catalyst removal in
solution adsorber (295-310
o
C/115 kg/cm
2
).

After catalyst removal in solution adsorber, the solution is then
depressurized in stages intermediate pressure separation (IPS), low
pressure separation (LPS) causing cyclohexane, ethylene and butene to
flash off & sent flashed vapours to recycle area. The molten polymer
containing residual amounts of hydrocarbon is sent to finishing area.

- RECYCLE AREA
The area consists of intermediate & low pressure vapor recovery system
& five distillation column systems (Low Boiler column, High Boiler
column, RB (grease) column, FE (ethylene) column & CM (butene)
column).

Vapor Recovery:
(a) Intermediate pressure vapor recovery: The vapor stream from the IPS
contains cyclohexane, the untreated ethylene, co-monomers, grease &
small quantities of reaction by-products.This overhead vapor & the
intermittent hot solvent flow used for flushing the solution adsorber
are combined and sent to the recycle area for purification.
(b) Low pressure vapor recovery: Cyclohexane vapors from two stages of
LPS passes through knock out pot is condensed and collected in LPS
hold up tank. From LPS hold up tank it is pumped to LB column
through LB feed heaters.

- DISTILLATION AREA
The distillation section of the recycle area separates all of the light &
heavy components from the reaction area and facilitates purging of
impurities. It consists of five distillation column systems:
(a) Low boiler (LB) column:
To separate low boilers (ethylene and butene-1/butene-2). The
overhead stream contain ethylene, butene-1 & butene-2 are condensed
& sent to FE column via FE column feed dryers. Bottom is sent to HB
column.
(b) High boiler (HB) column:
To separate cyclohexane & high boilers. The overhead vapor (99.9%
cyclohexane) is condensed & this is recycled to reaction area. HB
bottom contains high boiler (grease) is fed to RB column.
(c) Grease (RB) column:
To concentrate high boiler (grease). Overhead vapor is condensed &
returned back to HB column bottom sump. Bottom contains high
boilers is purged to Dowtherm vaporizer where it is used as fuel. RB
column acts as an extended stripping section of the HB column.
(d) Ethylene (FE) column:
To separate unreacted ethylene & butene-1/butene-2. Overhead vapor
condensed using propylene as refrigerant in overhead condenser.
Ethylene recovered from overhead is recycled to outside battery
limits. Bottom is fed to CM column.
(e) Butene (CM) column:
To concentrate butene-1 in the overhead for recycle to reaction area.
Column concentrates butene-2 in the bottom which is sent to outside
battery limits.
- FINISHING AREA
The polymer separated from the solvent & other components in the
reaction area is further purified & processed into finished product.
Main extruder:
Molten polymer from LPS-2 is fed to main extruder, which is driven by
(variable frequency drive) motor. Polymer enters the rotating extruder
screw. The screw forces the molten polymer through the die plate of
under-water pelletizer.

In NOVA Sclairtech polyethylene technology extruder feed is melt
polymer so power consumption in comparison to other technologies is
lower.

Satellite extruder:
To add solid additive in main extruder.

Under-water pelletizer:
Consists of die plate & a melt cutter. The molten polymer comes out
through the die plate of under-water pelletizer. The melt cutter then
chops the extrudate into pellets. The water/pellet slurry from the
pelletizer flows into the delumper.

Delumper/Dewatering Classifier:
The water/pellet slurry from the pelletizer flows into the delumper. Any
oversize lumps are rejected & any fines & undersize pellets are
separated.

Stripper:
Resin product leaving the pelletizer contains approx. 2.5% (wt.) volatile
hydrocarbons, which must be reduced to 500ppm (max.). Volatile
hydrocarbons trapped within the product pellets removed in stripper,
where they are stripped by counter-current flow of desuperheater steam.

Spin Dryer:
The stripped resin pellets flow out of stripper mixed with transport water
& conveyed to spin dryer to dry down the product pellets. From spin
dryer the dried product pellets are conveyed through pneumatic
conveying system to bagging silos.





Liquid & solid additive:
Additives enhance the quality & range of applications for which
polyethylene can be used. Additives used are as follows:-

Additive Type Feed-in
Antioxidants Liquid IPS tail by dosing pump
Slipping agent Liquid Main extruder by pump
UVS Liquid IPS tail by pump
Polymer processing aid Dry Main extruder by satellite
extruder
Anti -block Dry Main extruder by satellite
extruder
























MATERIAL
BALANCE

MATERIAL BALANCE

AIM: To design a polyethylene plant of capacity 960 TPD(tonnes per day).

1.Estimation of feed to LLDPE plant
Capacity per hour = 960/24 tonnes per hour
= 40 tonnes per hour (TPH)
LLDPE produced =40 TPH
Assuming losses :
- Polymer loss in bagging area = 0.24 TPH(0.60% of LLDPE produced)
- Polymer loss in stripper = 0.04 TPH(0.10%)
- Polymer loss in extruder = 0.27 TPH(0.675%)
- Polymer loss as grease = 8.84 TPH(22.10%)
Total loss = 9.39 TPH
Amount of ethylene reacted (according to losses) =9.39 TPH

Assuming 95 % conversion of ethylene to polythene:
- Therefore the amount of ethylene fed to LLDPE plant
= (40 + 9.39)/.95
= 51.98 TPH
- Amount of ethylene unreacted = 51.98-(40+9.39) =2.59 TPH

2.Absorber:

- In absorber 21% by weight ethylene is dissolved in cyclohexane.
- Ethylene feed, (B) = 38.98 TPH
- Solution (cyclohexane + ethylene), (C) = 51.98/0.21 = 247.52 TPH

- Solvent (cyclohexane) feed , (A) = 247.52 * 0.79 = 195.54 TPH
Material balance across absorber :
Figure-1
C
B
A
ABSORBER
COOLER
A+B = C
195.54 + 51.98 = 247.52
247.52 = 247.52
Input = Output

3.Reactor:
(Assuming 95 % conversion of ethylene to polyethylene)
Reaction
nC
2
H
4
(C
2
H
4
)
n
ethylene polyethylene


Figure-2


Input:
- Ethylene, (A) =51.98 TPH
- Cyclohexane, (B) =195.54 TPH

Output:
- Product (LLDPE + Grease) = 0.95 * 51.98 = 49.38 TPH
- Unreacted ethylene (D) = 51.98 - 49.38 TPH
= 2.60 TPH
Cyclohexane , (E) = 195.54 TPH
Grease, (F) = 8.84 TPH
LLDPE, (G) = Product Grease
= 49.38 - 8.84 TPH
= 40.54 TPH
- Material balance:
Input = Output
c
A
B
D,E,F,G
A+B = D+E+F+G
51.98 + 195.54 = 2.60 + 195.54 + 8.84 + 40.54
247.52 = 247.52
Input = Output

4.Intermediate Pressure Separator :
- IPS gives out 50:50 of polyethylene & cyclohexane.
Input A:
LLDPE = 40.54 TPH
Unreacted ethylene = 2.60 TPH
Grease = 8.84 TPH
Cyclohexane = 195.54 TPH

Figure-3

Output B:
LLDPE = 40.54 TPH
Cyclohexane = 40.54 TPH
Grease = 3.47 TPH {Assumption: Grease removed in
Overheads is 61%approx.)


Overheads C:
Cyclohexane = 155 TPH
Unreacted ethylene = 2.60 TPH
Grease = 5.37 TPH { 8.84 - 3.47 }
Material balance:
A = B+C
195.54 + 40.54 + 2.60 + 8.84 = 40.54 +40.54 + 2.60 + 155 + 3.47 + 5.37
A B
C
IPS
247.52 = 247.52
Input = Output

5.Low Pressure System - I
It gives Output B in which cyclohexane is 5% of (cyclohexane +
LLDPE) in Product stream B.
Input A:
It is output of IPS.
LLDPE = 40.54 TPH
Cyclohexane = 40.54 TPH
Grease = 3.47 TPH

Figure-4
Output B:
Cyclohexane = 40.54/0.95 * 0.05
= 2.13 TPH
Grease = 1.09 TPH(Assumption: Grease removed in
Overheads(C) =69% approx..)
LLDPE = 40.54 TPH

Overheads (C):
Cyclohexane = 40.54 - 2.13
= 38.41 TPH
Grease = 3.47-1.09=2.38 TPH

Material balance:
A = B+C
40.54 + 40.54 + 3.47 = 2.13 + 1.09 + 40.54+ 38.41 + 2.38
84.55 = 84.55
A B
C
LPS-I
Input = Output

6.Low Pressure System II
It gives Output B in which cyclohexane is 2% of (cyclohexane +
LLDPE) in product stream B.
Input A:
It is the output of LPS-I.
LLDPE = 40.54 TPH
Cyclohexane = 2.13 TPH
Grease = 1.09 TPH

Figure-5

Output B:
Cyclohexane = 2.13/0.98 * 0.02
= 0.04 TPH
LLDPE = 40.54 TPH

Overheads C:
Cyclohexane = 2.13 0.04
= 2.09 TPH
Grease = 1.09 TPH
Material balance:
A=B+C
40.54 + 2.13 + 1.09 = 0.04 + 40.54+ 2.09 + 1.09
43.76 = 43.76
Input = Output

7.Extruder
A B
C
LPS-II
Output B of LPS-II is the input of Extruder.
Input A:
LLDPE = 40.54 TPH
Cyclohexane = 0.04 TPH

Figure-6

Polymer loss(Accumulation) = 0.27 TPH
Output B:
LLDPE = 40.27 TPH
Cyclohexane =0.04 TPH
Material balance:
A= B + Accumulation
40.54 + 0.04 = 40.27+0.04+0.27
40.58 = 40.58
Input = Output

8.Stripper

In the stripper, the stream D contains 99.9% of the polymer entering the
stripper.
Input A:
It is output of Extruder.
LLDPE = 40.27 TPH
Cyclohexane = 0.04 TPH
Input C:
Steam = 3.46 TPH(Assumption)
EXTRUDER
A
B

Figure-7
Output D:
LLDPE = 0.999*40.27=40.23 TPH

Output B:
Cyclohexane = 0.04 TPH
LLDPE = 0.04 TPH
Steam = 3.46 TPH
Material balance:
A + C = B + D
40.27 + 0.04 + 3.46 = 0.04 + 3.46 + 0.04 + 40.23
43.77 = 43.77
Input = Output
9.Bagging
Stripper stream D is going to bagging area.
Polymer loss in bagging area = 0.24 TPH
LLDPE input to bagging area = 40.23 TPH
LLDPE produced per hour = 40.23-0.24=40 Tonnes

10.Distillation:

A
B
C
D
STRIPPER

Figure-8

Feed F:
Feed has cyclohexane ,grease,& ethylene.
Cyclohexane = from ( IPS overheads+ LPS-I overheads+ LPS-II
overheads+ Stripper Stream B)
= 155 + 38.41 + 2.09 + .04
= 195.54 TPH
Ethylene = 2.60 TPH (from IPS overheads)
Grease = 8.84 TPH (from IPS overheads ,LPS-I overheads,&
LPS-II overheads)
Total = 206.98 TPH
Ethylene = 2.60 TPH
Cyclohexane + Grease = 204.38 TPH
Wt fraction of ethylene = .013
Wt fraction of cyclohexane + grease = .987

Distillate
Wt fraction of ethylene in distillate = .99
Wt fraction of cyclohexane + grease in distillate = .01

Residue
Wt fraction of ethylene in residue = .005
Wt fraction of cyclohexane + grease in residue = .995

F
D
W
D
I
S
T
I
L
L
A
T
I
O
N
Overall material balance:
F = D + W
206.98 = D + W

Ethylene balance:
X
F
F = X
D
D + X
W
W,
Here, X
F
, X
D
, & X
w
are the mole fractions of ethylene in feed, distillate
& residue respectively.
2.60 = ((206.98 - W)*.99) + (W*.005)
W = 205.39 TPH
D = 1.59 TPH
Distillate
Cyclohexane + grease in distillate = D*(1-X
D
) TPH
= 1.59 * .01 TPH
= .0159 TPH
Ethylene in distillate = D*(X
D
) TPH
= 1.59 * .99 TPH
= 1.5741 TPH

Residue
Cyclohexane + grease in residue = W*(1-X
W
) TPH
= 205.39 * .995 TPH
= 204.363 TPH
Ethylene in residue = W*(X
W
) TPH
= 205.39 * .005 TPH
= 1.027 TPH

Overall Material balance:
F = D + W
206.98 = 1.59 + 205.39
206.98 = 206.98

ENERGY
BALANCE

ENERGY BALANCE


Figure-9
1. Energy balance across Reactor feed heater

Figure-10
Input A:
Mass flow rate of cyclohexane = 195.54 * 10
3
kg/hr
Mass flow rate of ethylene = 51.98 * 10
3
kg/hr
Average Specific heat capacity of cyclohexane(90
o
C) = 2.235
K kg
kJ

Average Specific heat capacity of ethylene(90
o
C) = 0.74
K kg
kJ

- Energy in + Q
from steam
= Energy out
HX
B
150
0
c
A
30
0
C
150
o
C
270
o
C
30
o
C
295
o
C
50
o
C
50
o
C

80.7
o
C
237
o
C
285
o
C
170
o
C
- Q
steam
= Energy out Energy in
= Mass flow rate
cyclohexane
* C
p cyclohexane
* (T) + Mass flow
rate
ethylene
*C
p ethylene
*(T)
= (195.54*2.2325*1000*(150-30)) +
(51.98*0.74*1000*(150-30))
= 5,70,59,652
hr
KJ

2. Energy balance across Reactor


Figure-11
- Energy Balance
Enthalpy Inlet Stream + Heat Generation due to
polymerization(Exothermic Reaction) = Enthalpy outlet stream
- Heat of Reaction = 22380 kcal of heat per kmol of monomer
reacted.
- Taking 25
O
C as reference temperature for enthalpy calculations
and also assuming temperature of reactor between 250-280
O
C for
C
p
calculations.
- Average value of C
p cyclohexane
(210
O
C) = 2.89 kJ/kg K
- C
p ethylene
(input stream at 90
O
C) = .74 kJ/kg K
- C
p ethylene
(output stream at 150
O
C) = .78 kJ/kg K
- C
p LLDPE
(270
O
C) = 5.60 kJ/kg K
- Neglecting grease in the output stream of reactor, we have:-
(m*C
P cyclo
*(T-150)) - (m
ethyl.
*C
P ethyl.
*(150-25))
input
+ (m
ethyl
C
P ethyl
(T-25))
output
+

m
LLDPE
C
P

LLDPE
(T-25) = Heat Generation
{ (195.54*2.89*(T-150))
cy
- (51.98*.74*(150-25))
ethyl input
+

40.54*5.60*(T-25) + (2.60*.78*(T-25))
output ethylene
} = 136092.780
565.12*(T-150) 4808.15 + 227.02*(T-25) + 2.028(T-25) = 136092.780
T = 270
O
C

3. Energy balance across Solution Adsorber Pre-heater


Figure-12
- Energy in + Q
from steam
= Energy out
- Mass flow rate of cyclohexane = 195.54 * 10
3
kg/hr
- Mass flow rate of ethylene = 2.60 * 10
3
kg/hr
- Mass flow rate of LLDPE = 40.54 * 10
3
kg/hr
- C
p cyclohexane
(280
O
C Mean temperature) = 2.90 kJ/kg K
- C
p LLDPE
(280
O
C) = 5.60 kJ/kg K
- C
p ethylene
(280
O
C) = .79 kJ/kg K
HX
B
295
0
c
A
270
0
C
Q
steam
= (m
Ethylene
C
P Ethylene
+ m
Cyclohexane
C
P Cyclohexane
+
m
LLDPE
C
LLDPE
)*(T)
= (2.60*0.79

+ 40.54*5.60

+ 195.54*2.90)*10
3
*25
= 19903.60 * 10
3

hr
kJ

4.Energy balance across Extruder

Figure-13
Inlet A:
Mass flow rate of LLDPE = 40.54 * 10
3
kg/hr
Mass flow rate of Cyclohexane = 0.04 * 10
3
kg/hr
- Energy in Energy out = Q
lost

- C
p LLDPE
(170
O
C) = 5.60 kJ/kg K
- C
p cyclohexane
(170
O
C) = 2.81 kJ/kg K
Q
lost
= m
LLDPE
*C
p LLDPE
*(235) + m
cyclohexane
*C
p cyclohexane
*(235)
= (40.54 * 1000 * 5.60 + 0.04* 1000 * 2.81) * (235)
= 53377.05 * 10
3

hr
kJ

5.Energy balance across Distillation Column
EXTRUDER
A
B
50
0
C 285
0
C

Figure-14
Feed has Cyclohexane, grease and ethylene and entering at 170
o
C
- Cyclohexane = 195.54 TPH
- Ethylene = 2.60 TPH
- Grease = 8.84 TPH
- Cp of cyclohexane at 170
o
C = 2.81
C kg
kJ
o

- Cp of ethylene at 170
o
C(liquid state, absorbed in cyclohexane)
= 0.78
C kg
kJ
o

- Weight fraction of ethylene in feed = .013
- Weight fraction of cyclohexane + grease in feed = .987
- Cp of feed = (2.81*.987) + (.780.013) = 2.78

Distillate is leaving at 80.7
o
C
- Weight fraction of ethylene in distillate = .99
- Weight fraction of cyclohexane + grease in distillate = .01
- C
p
cyclohexane at distillate temperature = 2.0 kJ/kg K
- C
p
ethylene at distillate temperature = 1.5 kJ/kg K
- C
p
of distillate = (2.00.01) + (1.500.99)
= 1.505
K kg
kJ

Residue is leaving at 237
o
C
- Weight fraction of ethylene in residue = .005
- Weight fraction of cyclohexane + grease in residue = .995
F
170
o
C
D
80 . 7
0
C
W
237
o
C
1.8MPa
100
o
C
- C
p
cyclohexane at residue temperature = 2.90 kJ/kg K
- C
p
ethylene at residue temperature = 0.80 kJ/kg K
- Cp of residue = (.995*2.90)+(0.80*.005)
= 2.89
K kg
kJ

Neglecting Grease and assuming binary distillation,we have:-
Referring T-x-y diagrams of cyclohexane & ethylene at 1.8 MPa, we infer that :
- Feed is in liquid state at 170
o
C & 1.8 MPa.
- Residue is also in liquid state at the given residue conditions.
- While distillate after partial condensing at very high pressure is in vapour
state.
- Partial condensed liquid is sent as Reflux in the Distillation column.
Enthalpy of distillate:
- Reference temperature for enthalpy calculations = 25
o
C
= m
distillate
Cp
distillate
T

+ m
cyclohexane
L
cyclohexane

Here ,
m
distillate
= mass flow rate of distillate
Cp
distillate
= specific heat capacity of distillate
T

= temperature difference
L
cyclohexane
= latent heat of vaporization of cyclohexane

- Latent heat of vaporization of cyclohexane = 440
kg
kJ

Enthalpy of distillate = { (1.59*1.505*(80.7-25)) + (.0159*440)} * 10
3

= 140.28 * 10
3
kJ/hr
Enthalpy of residue:
- Taking T
r
= 25
o
C,
= m
residue
Cp
residue
T

+ m
cyclohexane
* L
cyclohexane
= { (204.363*440) + (205.39*2.89*(237-25)) } * 1000
hr
kJ

= 215758.065 * 10
3

hr
kJ

Enthalpy of feed:
- Taking reference temperature for enthalpy calculations 25
o
C, we have :-
= m
feed
Cp
feed
T

+ m
cyclohexane
L
cyclohexane
= { (206.98*2.78*(170-25)) + (195.54*440) } * 10
3

hr
kJ

= 169471.238 * 10
3

hr
kJ


- Distillate = 1.59 TPH
- Assuming reflux ratio = 2.5
- Mass flow rate into condenser = D(1 + R)
= 1.59*3.5
= 5.565 TPH
- Now Q
c
( Condenser load ) is equal to heat required to decrease the
temperature of distillate from 100
0
C to 80
0
C and the latent heat of
condensation of cyclohexane vapours.

Q
c
= { (5.565*1.505*(100-80.7)) + (0.05565*440) } * 10
3

hr
kJ

= 186.130 * 10
3

hr
kJ


Now Overall Energy balance:
Q
B
= WH
W
+ DH
D
+ Q
C
- FH
F

Here,
H
W
,

H
D
,

& H
F
are the enthalpies of Residue, Distillate & Feed respectively.
= ((205.39*215758.065 +1.59*140.28 + 186.130) (206.98*169471.238))
* 10
3
kJ/hr
= 9237801.304 * 10
3

hr
kJ

= 2566.056 * 10
3
kJ/sec
6.Steam requirement in Reactor feed heater
- Steam condenses at 201.4
0
C & 16 bar.
- Latent heat of condensation of steam at the process conditions
= 1933.20 kJ/kg
Q
steam
= mass flow rate of steam(m) * L (Steam is condensed to preheat the
feed in heater )

m*L = 57059652
m * 1933.2 = 57059652
m = 29515.65 kg/hr

7.Steam requirement in Solution Adsorber Pre-heater

C
p
of steam at 473 K = 2.10
kgK
kJ

C
p
= C
1
+ C
2
T+ C
3
T
2
+ C
4
T
3
+ C
5
T
4

Where
C
1
= .336 * 10
5

C
2
= -.2699 * 10
5
C
3
= 2.61* 10
3

C
4
= -.0890 * 10
5

C
5
= 1169
And T = temp in K
Suppose steam inlet and outlet temperature as 300
0
C and 220
0
C
Average C
p
of steam = 2.10
kgK
kJ

- Q
steam
= 2.10 * m
steam
* (300-220)
- m = 19903.60*1000/(2.10*80)
Mass flow rate of steam = 118473.81 kg/hr




















EQUIPMENT
DESIGN

1. Reactor design


Figure-15
Inlet Stream of Reactor:
- It consists of solution of 21%(by wt.)ethylene absorbed in cyclohexane.
- Volume of solution = Volume of Solvent(because a gas is dissolved in
liquid)
- Solvent mass flow rate= 195.54 TPH=195.54*10^3 kg/hr
Density of solvent(cyclohexane) at temp 270
0
C = 779 kg / m
3
Volumetric flow rate of feed = 195.54* 10
3
/ 779
= 251.01 m
3
/hr
Reaction of Process

n(C
2
H
4
) (C
2
H
4
)
n

C
2
H
4
(C
2
H
4
)
n
- According to literature, under conditions 270
0
C and 15.20MPa in an
autoclave Mixed Flow Reactor and polymerization in solution phase,
polymerization kinetics comes out to be of first order with respect to
monomer and catalyst concentration appears in the rate constant.
- Taking 1
st
order reaction we have:
c
Vo
CA0
CA

Design equation for MFR (Mix flow reactor) / CSTR:

= Hold up time
C
A0
= Initial conc. of ethylene in inlet
C
A
=Final conc. of ethylene in outlet
V= Volume of reactor
V
0
=Volumetric flow rate of feed

-r
A
=Rate of reaction
k=Rate constant
= Expansion coefficient

-r
A
= KC
A
(1
st
order reaction)
k= 25.62 hr
-1
( from manual )
(for liquid phase reaction)


For X
A
= 0.95,
V=

*
779
10 * 195.54
3

= 186.15 m
3

Calculation for Agitator power & Agitator dimension.

Figure-16

- Taking turbine as agitator for the system
- Now Correlation between agitator & tank dimensions for turbine are :-
- , , = , ,
, h=D
t
, E=D
a

- Industrial paddle agitators turn at speeds between 20 and 150 rpm.
- Assuming the speed of 210 rpm= 3.5 rps.
- Volume of MFR = 186.15m
3

-
4
H D
2
t
H
= 186.15 m
3

-
4
4.0D * D
t
2
t
H
= 186.15 m
3

- D
t
= 3.89 m

D
a
=
3
t
D
= 1.30 m
L = .25 * D
a
= .325 m
h = D
t
= 3.89 m
H = 4.0 * D
t
= 15.56 m
E

= D
a
= 1.30 m
J

=
12
t
D
= .320 m
W

=
5
t
D
= .260 m
N = 3.50 rps

Where,
D
t
= Diameter of tank
D
a
= Diameter of shaft / impeller
L

= Length of blades
h

= Height of baffles
H

= Height of tank
E

= Height of impeller
J

= Clearance
W

= Width of baffle
N

= Speed of impeller

cyc
(viscosity of cyclohexane at 270
0
C) = 6.926 * 10
-3

Poise

ethyl
(viscosity of ethylene at 270
0
C) = 1.472 * 10
-4

Poise
(avg viscosity of solution at 270
0
C) = .4 * 10
-4

Poise

cyc
(viscosity of cyclohexane at 270
0
C) = 779 Kg/m
3

ethyl
(viscosity of ethylene at 270
0
C) = .802 Kg/m
3

(avg viscosity of solution at 270
0
C) = (
a
M
a
+
b
M
b
)/ M
a
+ M
b

= [(779*78) + (.802*28)]/(78+28)
= 573.40 Kg/m
3


Reynolds Number of solution = (D
a
2
*N*)/
= 1.30
2
* 3.50 * 573.40 / (.4 * 10
-3
)
= 84.80 * 10
6


Power number = 5.00 (for disc mounted flat blade turbine from Coulson &
Richardson vol-6, fig.10.59)

P = 5.00 * D
5
* N
3
*
= 5.00* (1.30)
5
* (3.50)
3
* 573.40
= 456.40 kW
Paddle = 5 (Using 5 paddles at equal lengths of the MFR for effective mixing)
Total shaft power of the agitator = 5 456.40 = 2282 kW

Mechanical design of reactor :-
A CSTR is preferred usually under following circumstances
- Liquid phase reaction
- Low pressure reaction
- Intense agitation is required
- Large residence time
- Better temperature control required
- Less cost
Reason to choose CSTR :-
- Mixing of two liquid phase reactant
- High mass and heat transfer efficiency required
- Reactant are in liquid phase and homogenous.

Mechanical design includes
- Thickness of shell
- Impeller design
- Diameter of impeller
- Material of construction
- Insulation of selection

- Dished bottom reactor requires less power than flat one hence dished
bottom is chosen.

Impeller selected is a pitched blade turbine 45
0
because
- The weighted viscosity of reaction mixture is .4 * 10
-4
poise which lies
in the range of turbine.
- Efficient turbulent flow impeller for blending such liquids.
- Combined axial and radial flows are achieved
- Low cost
- Wide application range.



- N = 3.50 rps(speed of agitator),

- D
a
=
3
t
D
= 1.27 m
- L = .25 * D
a
= .317 m
- h = D
t
= 4.09 m
- H = 4.0 * D
t
= 9.914 m
- E

= D
a
= 1.273 m
- J

=
12
t
D
= .317 m
- W

=
5
t
D
= .2543 m


Where,
D
t
= Diameter of tank
D
a
= Diameter of shaft / impeller
L

= Length of blades
h

= Height of baffles
H

= Height of tank
E

= Height of impeller
J

= Clearance
W

= Width of baffle
N

= Speed of impeller

Shell thickness :-
Diameter of shell = 3.89 m
Operating pressure = 15.20 MPa
Design pressure = 1.2 * 15.20 MPa(factor of safety=1.2)
= 18.24 MPa

Working or operating temperature = 270
0
C
Design temperature =1.2* 270
0
C
= 324
0
C
Material selection
For reactor :-
- Carbon Steel Type 310
Its composition is:-
- Cr = 24-26 % , Ni = 19-22.9 % , C = 0.25 %
Advantages:-
High Strength & Resistant to scaling at high temperatures
This alloy shows increased resistance to high temperature corrosion
For blades :-
- Carbon Steel Type 410
Its compostion is:-
- Cr= 11.5-13.5 % , C= 0.15 %
Advantages:-
Lowest cost general purpose Stainless Steel
Widely used where corrosion is not severe
For baffles
- Carbon Steel Type 405
Its composition is:-
- Cr= 11.5-14.5 % , C = 0.08 % , Al = 0.1 -0.3 %
Advantages:-
Good Weld ability and cladding properties
Version of type 410 with limited hardenability but improved weldability
Baflle spacing
Baffle Spacing is calculated from the following formula
- Baffle spacing = x
4
t
D
= 3.14 x
4
89 . 3
= 3.054m
Baffle spacing = 3.054 m
Width of Baffle ==
12
t
D
= 0.324 m
Width of Baffle = 0.324 m
Distance from Bottom =
2
t
D
=
2
89 . 3
= 1.945 m

Minimum practical wall thickness

There will be wall minimum wall thickness required to ensure that any vessel is
sufficiently rigid to withstand its own weight and any incidental loads. As a
general guide , the wall thickness of any vessel should not be less than the
values given below ; the values include a corrosion allowance of 2 mm
For cylindrical Tanks , wall thickness is given by
- t =
p 0.6 - E * S
r * P
j
i
+ Cc
Where,
P= Internal pressure
Ri = internal radius
Ej = Efficiency of Joint = 0.85
S = Maximum allowable working stress = 360000 Kpa
Cc = 4 x 10-3
t= wall thickness (m)
t =
6 3
6
10 x x18.24 0.6 - 0.85 x 10 x 360000
1.945 x 10 x 18.24
+ 4 x 10
-3

= .124 m
= 12.40 cm
Then outer Diameter of Shell:-
- Do = Di + 2t
= 3.89 + 2 x .124
Do = 4.138 m
Heads & closures
The ends of cylindrical vessel are closed by Heads of various shapes. The
principal types used are
1) Flat plates & formed Flat Heads
2) Hemispherical Heads
3) Ellipsoidal Heads
4) Torrispherical Heads

Flat plates are used as covers for Man ways and as the channel covers of Heat
Exchangers. Formed Flat End, known as Flange only ends , are
manufactured by turning over a flange with a small radius on flat plate. The
corner radius reduces the abrupt change of shape, at the junction with the
cylindrical section; which reduces the local stresses to some extent .
Flange only heads are the cheapest type of formed head to manufacture, but
their use is limited to low pressure & small diameter vessels.
Standard Torrispherical Heads (Dished Heads) are the most commonly used
end closure for vessels up to operating pressure of 15 bars. They can be used
for higher pressures, but above 10 bars, their cost should be compared with that
of an equivalent ellipsoidal head.
Above 15 bars, an ellipsoidal Head will usually prove to be the most
economical enclosure t o use.
A hemispherical head has the strongest shape; capable of resisting about twice
the pressure of a torrispherical head of same thickness. The cost of forming a
hemispherical head will, however, be higher than that for a shallow,
torispherical head. Hemispherical heads are used for high pressures.
So, according to our requirement, hemispherical head is the best choice.
Hemispherical head design
D = 2H
D = Diameter of reactor
D = 3.89 m
H = 1.945 m
Material and conditions:-
SA 240/340 steel
S = 360000 kPa allowable stress
E = 1 (head longitudinal joint efficiency)
Internal pressure(design) = 18.24 MPa
Corrosion correction factor = .201 mm
t
req
=


+ corrosion factor
= 49.721 mm
= 4.9 cm
Where,
L=(Do-2*t)/2
Vessel supports
The Method used to support a vessel will depend on the size, location, shape ,
weight of Vessel , temperature , pressure , interval & external fittings .
Skirt supports are used for tall, Vertical Columns.
Brackets or Legs are used for all types of vessel. Supports must be designed to
carry the weight of the vessel and contents and any superimposed loads, such as
Wind loads.
Supports will impose Localized Loads on the vessel wall and the design must
be checked to ensure that the resulting stress concentrations are below the
maximum allowable design stress.
The Bracket construction permits support of the cylinder without fixing the
supports to the shell.
So, selected support is bracket support , supported from steel work.

Types of flange & selection
Several different types of flange are used for various applications. The principal
types used in process industries are
1) Welding Neck Flanges
2) Slip-on Flanges Hub & Plate types
3) Lap Joint Flanges
4) Screwed Flanges
5) Blank or Blind Flanges
Welding Neck Flanges are suitable for extreme service conditions; where the
flange is likely to be subjected to temperature, shear & vibration loads.
So, the selected flange is welding neck Flange
Gaskets
Gaskets are used to make a leak- tight joint between two surfaces. They are
made from semi- plastic materials.
The gasket factor m is the ratio of the pressure under the operating conditions
to the internal pressure in vessel or pipe.
The internal pressure will force the flanges apart, so the pressure on the gasket
under operating conditions will be lower than the initial tightening up pressure.

The gasket factor gives the minimum pressure that must be maintained on the
gasket to ensure a satisfactory seal.
The following factors must be considered when selecting a gasket material
1) The process conditions, pressure, temperature, corrosive nature of
process fluid.
2) Whether repeated assembly & disassembly of joit is required
3) The type of Flange & Flange face.





2. Reactor feed heater design



Steam in(201.4C,16bar) Steam out(16bar, 201.4C)


P.S.out(150C,17.42MPa) Process stream in(30C,17.6MPa)



Reactor feed heater is a condenser which is exchanging heat by condensing
saturated steam on shell side to heat up the process stream.
From Energy Balance,
- Q (heat duty) = 57059652 kJ/hr
Process stream is taken on tube side and steam is at shell side as steam will
condense on outer surface of tubes.
Steam inlet temp = 201.4
0
C
Steam outlet temp = 201.4
0
C
T
c1
= Process stream Inlet temp = 30
0
C
T
c2
= Process stream Outlet temp = 150
0
C

Now, Q
C
= 57059652
hr
kJ

To find LMTD:
LMTD =
|
.
|

\
|

150 4 . 201
30 4 . 201
ln
) 150 4 . 201 ( ) 30 4 . 201 (
= 99.63C
For Condenser, No correction factor (F
T
) is required. F
T
= 1.


To calculate heat transfer area:
Since cold fluid is majorly cyclohexane(organic solvent) + ethylene and
hot fluid is steam. From Coulson & Richardson Vol.6, Overall heat
transfer coefficients table, we have the range 500-1000 W/ m
2
K
Assuming U = 800 W/m
2
K
- Q = UA (LMTD) A=198.86 m
2



CONDENSER
To calculate number of tubes:
N
t
=
L d
A
o t

Assume O.D. of tube = 20 mm, I.D. = 16 mm and length, L = 4.88 m
Material of tubes Carbon Steel,
Allowing for tube sheet thickness and taking L = 4.83m.
N
t
=
) 83 . 4 (
1000
20

198.86
|
.
|

\
|
t
= 656.30 = 656 tubes approx.
As the shell-side fluid is steam which is relatively clean:-
Using the triangular pitch, P
t
= 1.25d
o
= 0.025 m

Using exchanger with one shell side and two tube side passes.
K
1
= 0.249 ; n
1
= 2.207
Now, bundle diameter, D
b
= d
o
1
1
t
n
1
K
N
|
.
|

\
|
= .71 m
Using split ring floating head, from fig. 12.10 (RC-vol 6), clearance = 64 mm
D
S
D
b
= 0.064m D
S
= 0.773 m

TUBE-SIDE HEAT TRANSFER CO-EFFICIENT:
Mean Process Stream temperature =
2
150 30 +
= 90
0
C
Cross sectional Area of single tube, A
t
=
4
t
(d
i
)
2
= 2.01 10
-4
m
2

No. of tubes per pass, n =
2
656
= 328
Tube flow area = n * A
t
= 328 * 2.01 * 10
-4

= 0.066 m
2

Process stream mass velocity =
area flow tube
m
.
=
.066 * 3600
1000 * 52 . 247

= 1041.75
s m
kg
2
.

Density of process stream at 90
0
C = 729.93
3
.
m
kg

(solution) at process stream mean temperature = 540*10
-6
Pa.s
C
p
= 2.119kJ/kg.K ; k = 0.112 W/m.K
Solution linear velocity =
93 . 729
75 . 1041
= 1.43 m/sec.
Reynolds no. (Re) =

=
6
10 * 540
016 . * 43 . 1 * 93 . 729

= 30927.40
Prandtl no. (Pr) = C
p
/k =
112 .
10 * 119 . 2 * 10 * 540
3 6
= 10.22
Re implies turbulent flow and for turbulent flow,we have

14 . 0 .33 0.8
) / ( Pr * Re * 0.023
w
i
k
Dh
=

Neglecting /
w
term as assuming viscosity is a weak function of temperature.

D
Pr * Re * 0.023 * k
h
.33 0.8
i
=
.016
10.22 * 30927.40 * 0.023 * .112
h
.33 0.8
i
= = 1355.87 W/m
2
C

SHELL-SIDE HEAT TRANSFER CO-EFFICIENT:
h
o
= 0.95 k
L
3
1

g ) (
(

h L
V L L

(N
r
)
(-1/6)

where,
h
o
= mean condensation film coefficient W/m
2
C
k
L
= condensate thermal conductivity W/m C

l
= condensate density Kg/m
3

v
= vapor density Kg/m
3

L
= condensate viscosity Ns/m
2

h
= tube loading = condensate flow per unit length kg/m.s
Amount of condensate: L * m Q
.
=

L
Q
m
.
=

1933.2 * 3600
10 * 57059652
m
3
.
= = 8.20 Kg/s
L = latent heat of vaporization of water at 201.4C & 16 bar = 1933.20kJ/kg
k
L
= 0.58 W/mC

l
= 862.813 kg/m
3

V
= 7.42 kg/m
3

L
= .452 mPas

h
=
l
m
* n
t
.
=
4.83 * 656
20 . 8
= .00259 kg/m.s
Average no.of tubes in vertical tube row, N
r
=2/3*
t
b
P
D
=2/3*
25
709.52
= 18.91
h
o
= 0.95 k
L
3
1

g ) (
(

h L
V L L

(N
r
)
(-1/6)
= 2645.96 W/m
2
C


























OVER-ALL HEAT TRANSFER CO-EFFICIENT:

Outside and inside Fouling/dirt co-efficients are 5000 W/m
2
C and 3000
W/m
2
C and thermal conductivity of steel = 50 W/mC.

( )
i i
o
id i
o
W
i
o
o
Od o o h
1
.
d
d
h
1
.
d
d
k 2
d
d
ln d
h
1
h
1
U
1
+ + + + =

( )
.
3000
1
87 . 1355
1
16
20
50 x 2
16
20
ln 0.02
5000
1
2645.96
1
|
.
|

\
|
+ + + + =
= .00123

U
o
= 809.78 W/m
2
C
This is close to the assumed value.
TUBE-SIDE PRESSURE DROP:
kPa 17.07
2
1.43 * 729.93
* 2.5)
.016
4.83
* 10 * 3.7 * (8 * 2
2
* ) 2.5
L
* j * (8 * N P
2
3 -
2
f p
=
+ =
+ = A
v
i
D

This value of pressure drop is permissible.
Here, N
p
= no. of tube passes ; j
f
is evaluated from the graph between j
f
and Re
(Coulson & Richardson Vol.6)

SHELL-SIDE PRESSURE DROP:
Mass flow rate of steam = 8.20kg/s
A
S
=
t
b S o t
p
l D ) d (p
= 0.023 m
2
Mass flow rate =
.023
8.20
= 356.52
sec m
kg
2

Equivalent diameter, d
e
= ) d 917 . 0 p (
d
1.10
2
o
2
t
o
= 0.0144 m
Re = 356.52*14.4*10
-3
/.452*10
-3
= 113580
From fig. 12.24 (RC vol 6), j
f
= 2.2 * 10
-2
P
S
=
2
1

(
(

2 d
L
j 8
2
e
F
v
v

=
2
1

(
(

2
41 . * 813 . 862
*
.0144
4.83
* .022 * 8
2

= 2.14 kPa(Quite negligible)


CHOOSING BAFFLE SPACING:
25% baffle cut is chosen
So baffle spacing =
5
s
D
= .155 m
















COST ESTIMATION
FIXED AND WORKING CAPITAL:
Fixed capital is the total cost of the plant ready for start-up. It is the cost
paid to the contractors.
It includes the cost of :
1. Design, and other engineering and construction supervision.
2. All items of equipment and their installation.
3. All piping, instrumentation and control systems.
4. Buildings and structures.
5. Auxiliary facilities, such as utilities, land and civil engineering work.
It is a once-only cost that is not recovered at the end of the project life,
other than the scrap value.
WORKING CAPITAL:
Working capital is the additional investment needed, over and above the
fixed capital, to start the plant up and operate it to the point when income
is earned.
It includes the cost of :
1. Start-up.
2. Initial catalyst charges.
3. Raw materials and intermediates in the process.
4. Finished product inventories.
5. Funds to cover outstanding accounts from customers.
Most of the working capital is recovered at the end of the project. The
total investment needed for a project is the sum of the fixed and working
capital.
For a petrochemical plant working capital can be assumed safely to 15%
of the fixed capital.
ESTIMATION OF PURCHASED EQUIPMENT COSTS:-
For Shell & tube heat exchangers
Purchased cost = (Bare cost) * Type factor * Pressure factor
For horizontal & Vertical pressure vessels
Purchased cost = (Bare cost) * Material factor * Pressure factor
For Distillation Column
Installed cost = Cost * Material factor
For purchase cost of miscellaneous equipments

C
e
= CS
n

Where,
C
e
=Purchasing equipment cost ,$ (from table 6.2, RC-6,page no. 259)
C =Cost constant (from table 6.2, RC-6,page no. 259)
S =Characteristic size parameter (from table 6.2, RC-6,page no. 259)
n= Index for that type of equipment (from table 6.2, RC-6,page no. 259)

1. Compressors
Power = 1500 kW(power consumption of 5 compressors)
C
e
= 91000 (1500)
0.8
= $ 31616544.29

2. Reactors
Capacity, MFR=186.15 m
3


C
e
= 115000 (186.15)
0.45
C
e
=$ 1208192.703


3. Storage Tanks
Horizontal floating roof type tanks(Stainless Steel) 2 tanks
Capacity = 1600 m
3

C
e
= 13050 (1600)
0.55

= $ 754877.50

4. Absorption column
Bare vessel cost = $ 210,000
Material factor = 1
Pressure factor =1.1
Vessel cost = 1.1 * 1 * 210000 = $ 231000
Packed cost ( stainless steel) = $ 7500 / m
3

Vol. of packing = 3.14 /4 * 21
2
= 346.185 m
3

Cost of column packing = 7500 * 346.185=$ 2596388
Total cost of column = $ 2827388
5. Reboilers
Reboilers - 2
Bare cost = $ 600,000
Type factor = 0.8
Pressure factor = 1
Purchased cost = $ 600,000 * 0.8 * 1
= $480,000

6. Condenser cost
Condenser Units - 4
Bare cost = $ 447,058
Type factor = 0.85
Pressure factor =1.1
Purchased cost = 447,058 * 0.85 * 1.1
= $418,000
7. IPS cost
Material factor =1, carbon steel
Pressure factor = 1.4
Diameter = 2.50 m
Height = 8 m
Bare cost =$ 640,000
Purchased cost =$ 640,000 * 1 * 1.4
= $ 896,000
8. LPS
Diameter = 1.50 m
Height = 6 m
Material factor = 1
Pressure factor = 1.2
Bare cost = $ 720,000
Purchased cost = 1.2 * 1 *720,000 =$ 864,000

9. Extruder
Barrel diameter = 2 m
Length = 10 m
Material factor =1
Pressure factor =2.2

Purchased cost = 2.2 * 1 * 560,000
= $ 1,232,000

10. Stripper
diameter = 4.00 m
height = 10 m
Material factor = 1
Pressure factor = 1
Bare cost = $ 560,000
Purchased cost = 1 * 1 * 560,000
= $ 560,000

11. Distillation column cost
Total Cost = $550,000

12. Other equipments
drier = $ 88208.536
filter = $ 310676.32


PCE = cost of (compressor + reboiler + absorber + condenser + extruder
+ IPS + LPS + stripper + storage tanks + distillation column + other
miscellaneous equipments)

PCE = $ 41805887


Physical plant cost (PPC):
PPC is calculated from table 6.1 ,RC-6,page no. 252 .

C
f
= f
L
* C
e

C
f
= fixed capital cost
f
L
= the lang factor which depends on the type of process.
C
e
= the total delivered cost of all the equipment items.


Process plant cost = PCE * 3.40
= $ 41805887 * 3.4
= $ 142,140,015
Fixed capital = 1.45 * PPC
= 1.45 * 142,140,015
= $ 206, 103,022
Working Capital Cost = 15% of fixed capital cost
= .15 * 206103022
= $ 30915453
Total Investment Cost = Fixed capital cost + Working capital cost
= $ 237018475.70
ESTIMATION OF OPERATING COSTS
The cost of producing a chemical product will include the items listed below.
They are divided into two groups.
1. Fixed operating costs: costs that do not vary with production rate. These are
the bills that have to be paid whatever the quantity produced.
2. Variable operating costs: costs that are dependent on the amount of product
produced.
Fixed costs
1. Maintenance (labour and materials).
2. Operating labour.
3. Laboratory costs.
4. Supervision.
5. Plant overheads.
6. Capital charges.
7. Rates (and any other local taxes).
8. Insurance.
9. Licence fees and royalty payments.
Variable costs
1. Raw materials.
2. Miscellaneous operating materials.
3. Utilities (Services).
4. Shipping and packaging.

Variable cost estimation

Operating cost Assumed %
Raw material cost 25% of TPC = 0.25y
Operating labour 15% of TPC = 0.15y
Supervisory/Clerical
labour
20% of operating
labour
=0 .20*0.15y
Utilities 15% of TPC = 0.15y
Maintenance and repair 10% of FCI = $ 20610302
Operating supplies 15% of M & R = $ 3091545
Lab charges 23% of operating
labour
= 0.23*0.15y
Royalties & Insurance 2% of FCI = $ 4122060.44
Fixed charges 11% of TPC = .11y
Plant overhead charges

Miscellaneous charges
Administrative Expenses

Distribution & marketing
expenses

60% of Operating
labour
10% of M & R
25% of operating
labour
5% 0f TPC
= 0.60*0.15y

= $ 2061030.20
= 0.25*.15y

= .05y
Total

= 29884937.64 + 0 .902y









Total production cost, y = 0.902y + 29884937.64
TPC(y) = $ 304,948,343.30
Now, these costs are of year 2004, Using chemical engineering plant cost
index (CEPCI) 2012, we have costs in 2012 :-
Index in 2004 = 444.2
Index in 2012 = 575.4
Total production cost in 2012 = TPC in 2004 *



= 304948343.30 *



= $ 393383362.90
= Rs. 2.08 * 10
10

= Rs. 2080 crores
Total Investment cost in 2012 = TIC in 2004 * 575.4/444.2
= $ 305753833.70
= Rs. 1.62 * 10
10

= Rs. 1620 crores


PROFIT ESTIMATION
Current market selling price of LLDPE = Rs. 78.97/kg
Annual Production of LLDPE = 350 kT
Total income(on annual basis) = 350*10
6
*78.97
= Rs. 2760 crores
Gross Earning = Income - TPC
= Rs. 680 crores
Tax payments = 40% of gross earning
= .40 * .68 * 10
10
= Rs. 272 crores
Net profit= Rs. 408 crores
Depreciation = 10% of fixed capital cost = Rs. 1092346017


Payout period =
on depreciati after tax profit Net
Cost Investment Total
+

=
1092346017 10 * 408
10 * 1.62
7
10

= 3.13 years
Rate of return = 100 *
Cost Investment Total
after tax profit Net

= 100 *
10 * 1.62
4080000000
10
= 25.18%




















UTILITIES
The word "Utilities" is now generally used for the ancillary services needed in
the operation of any production process. These services will normally be
supplied from a central site facility; and will include:
1. Electricity.
2. Steam, for process heating.
3. Cooling water.
4. Water for general use.
5. Demineralised water.
6. Compressed air.
7. Inert-gas supplies.
8. Refrigeration.
9. Effluent disposal facilities
ELECTRICITY.
Power is required for chemical process, motor, lightening, pumps, compressor,
& other general & mechanical purposes. It may be purchased from local supply
authority or generated at plant by steam turbine, generator.
STEAM
The steam for process heating is usually generated in water tube boilers; using
the most economical fuel available. The process temperatures required can
usually be obtained with low-pressure steam, typically 2.5 bar (25 psig), and
steam is distributed at a relatively low mains pressure, typically around 8 bar
(100 psig).
COMBINED HEAT AND POWER (CO-GENERATION)
The energy costs on a large site can be reduced if the electrical power required
is generated on site and the exhaust steam from the turbines used for process
heating. The overall thermal efficiency of such systems can be in the range 70
to 80 per cent; compared with the 30 to 40 per cent obtained from a
conventional power station, where the heat in the exhaust steam is wasted in the
condenser. Whether a combined heat and power system scheme is worth
considering for a particular site will depend on the size of the site, the cost of
fuel, the balance between the power and heating demands; and particularly on
the availability of, and cost of, standby supplies and the price paid for any
surplus power electricity generated. On any site it is always worth while
considering driving large compressors or pumps with steam turbines and using
the exhaust steam for local process heating.
COOLING WATER

Natural and forced-draft cooling towers are generally used to provide the
cooling water required on a site; unless water can be drawn from a convenient
river or lake in sufficient quantity. Sea water, or brackish water, can be used at
coastal sites, but if used directly will necessitate the use of more expensive
materials of construction for heat exchangers.
WATER FOR GENERAL USE
The water required for general purposes on a site will usually be taken from the
local mains supply, unless a cheaper source of suitable quality water is
available from a river, lake or well.
COMPRESSED AIR
Compressed air will be needed for general use, and for the pneumatic
controllers that are usually used for chemical process plant control. Air is
normally distributed at a mains pressure of 6 bar (100 psig). Rotary and
reciprocating single-stage or two-stage compressors are used. Instrument air
must be dry and clean (free from oil).
INERT GASES
Where large quantities of inert gas are required for the inert blanketing of tanks
and for purging this will usually be supplied from a central facility. Nitrogen is
normally used, and is manufactured on site in an air liquefaction plant, or
purchased as liquid in tankers.
EFFLUENT DISPOSAL
Facilities will be required at all sites for the disposal of waste materials without
creating a public nuisance.



INSTRUMENT AND PROCESS CONTROL
Instrumentation is the most important factor in ensuring safety and smooth
working of the plant. A separate control room is provided in modern plants
where on panels indicators and recorders are present.
Instruments are used in the industry to measure process variables such as
temperature, pressure, density, level specific heat, conductivity, humidity, flow
rate, chemical composition etc.
The primary objectives of the designer when specifying instrumentation and
control schemes are:
1. Safe plant operation:
(a) To keep the process variables within known safe operating limits.
(b) To detect dangerous situations as they develop and to provide alarms
and automatic shut-down systems.
(c) To provide interlocks and alarms to prevent dangerous operating
procedures.
2. Production rate:
To achieve the design product output.
3. Product quality:
To maintain the product composition within the specified quality
standards.
4. Cost:
To operate at the lowest production cost, commensurate with the other
objectives.
These are not separate objectives and must be considered together.

TEMPERATURE CONTROL / MEASUREMENTS:
Various instruments are used for eg.
1. Thermocouple
2. Resistance Thermometers
3. Thermostats
4. Mercury in Glass Thermometers.
Controllers are used to maintain temperature within specified limits. Every
temperature control problems is essential one. The temperature lay involved in
the measurement of this variable is an important factor. Thermal element is
usually placed in a well to protect it and allow servicing of element without
interrupting the process. The location of the temperature element often has as
much to do with the efficiency element often as other parts of the control loops.
Temperature bulb should always be located at point where the coefficient of
heat transfer will be as large as possible e.g. if vapors and liquid are at same
temperature, then bulb should be kept in liquid because of high heat transfer
coefficients.
PRESSURE CONTROL / MEASUREMENTS
It is quite necessary for most system handling vapours of gas. It can be
measured by using pressure gauges.
Self operated pressure regulation is often used in pressure control. It is
installed directly in the line the control sensing apparatus is paced about 10
diameters from the unit. This location eliminates erroneous pressure caused by
turbulence. Sudden change in velocity, shock and vibrations difficulties often
occur when self operated regulation are used with liquids.
LEVEL CONTROL / MEASUREMENT
The measurement of level can be defined as the determination of location of
interface with respect to a fixed plane. The main objective of a level control
system is to maintain the level of the liquid in a tank at the Act point value. The
different is pressure transmitter senses the pressure difference / a function of
liquid level in the tank) and gives out an electrical signal, which after signal
conditioning is given to the P.I.D. controller. The controller compares the
measured variables with the set point and depending upon the error, gives an
output to the control valve. The control value, in turn controls the flow. Due to
the control of flow, the level is controlled to its set point.
FLOW CONTROL / MEASUREMENTS
It is defined as volume per unit time at specific temperature and pressure
conditions. It is generally measured by positive displacement of rate meters.
CONDENSER CONTROL
Temperature control is unlikely to be effective for condensers, unless the liquid
stream is sub-cooled. Pressure control is often used, or control can be based on
the outlet coolant temperature.
DISTILLATION COLUMN CONTROL
The primary objective of distillation column control is to maintain the specified
composition of the top and bottom products, and any side streams; correcting
for the effects of disturbances in:
1. Feed flow-rate, composition and temperature.
2. Steam supply pressure.
3. Cooling water pressure and header temperature.
4. Ambient conditions, which cause changes in internal reflux.
The compositions are controlled by regulating reflux flow and boil-up. The
column overall material balance must also be controlled; distillation columns
have little surge capacity (hold-up) and the flow of distillate and bottom
product (and side-streams) must match the feed flows. The feed flow-rate is
often set by the level controller on a preceding column. It can be independently
controlled if the column is fed from a storage or surge tank. Feed temperature is
not normally controlled, unless a feed pre heater is used. Temperature is often
used as an indication of composition. The temperature sensor should be located
at the position in the column where the rate of change of temperature with
change in composition of the key component is a maximum.
Near the top and bottom of the column the change is usually small. With multi
component systems, temperature is not a unique function of composition. Top
temperatures are usually controlled by varying the reflux ratio, and bottom
temperatures by varying the boil-up rate. If reliable on-line analyzers are
available they can be incorporated in the control loop, but more complex
control equipment will be needed.

PID LEGENDS:
Instrument locally mounted Process connecting
lines
Instrument at control center Orifice for flow
meas.
Instrument transmitting Electric lines
Control valve pneumatic Pneumetic lines
Controller self contained Capillary lines


FIRST LETTER SECOND LETTER THIRD
LETTER
D- Density A-Alarm A-Alarm
F-Flow C-Control C-Control
H-Hand activated E-Element V-Valve
L-Level G-Glass
M-Moisture I-Indicating
P-pressure R-Recorder
T-Temperature S-Safety weir



PID OF DISTILLATION COLUMN

Temperature Control Composition Control (R controlled and bottom
product as fixed ratio of feed flow)

Composition Control (Top product controlled by feed)


PID OF REACTOR



INSTRUCTIONS FOR OPERATION
Before starting, always make sure that the followings:
- No visible damage is evident in the system.
- All electrical switches are turned off.
- All water valves are closed.
- All valves are tightly closed.

Start up procedure.
- Check the level in the tank.
- Switch on the main supply.
- Turn on the main pump.
- Open valve for pump.
- Start mechanical pump.
- Open the steam valve.
- Check the flow, temperature& pressure during the operation.

System shut down.
- Reduce the flow of the feed & steam.
- Reduce all flow rates & wait for pasture to drop.
- Turn off the pump.
- When the flow slow down close the valve tightly to avoid cavitations.
- Disconnect the packing line.

GENERAL SITE CONSIDERATIONS
PLANT LOCATION AND SITE SELECTION
The location of the plant can have a crucial effect on the profitability of a
project, and the scope for future expansion. Many factors must be considered
when selecting a suitable site. The principal factors to consider are:
1. Location, with respect to the marketing area.
2. Raw material supply.
3. Transport facilities.
4. Availability of labor.
5. Availability of utilities: water, fuel, power.
6. Availability of suitable land.
7. Environmental impact, and effluent disposal.
8. Local community considerations.
9. Climate.
10. Political and strategic considerations.

Marketing area
For materials that are produced in bulk quantities; such as cement, mineral
acids, and fertilizers, where the cost of the product per tonne is relatively low
and the cost of transport a significant fraction of the sales price, the plant
should be located close to the primary market. This consideration will be less
important for low volume production, high-priced products; such as
Pharmaceuticals. In an international market, there may be an advantage to be
gained by locating the plant within an area with preferential tariff agreements;
such as the European Community (EC).
Raw materials
The availability and price of suitable raw materials will often determine the site
location. Plants producing bulk chemicals are best located close to the source of
the major raw material; where this is also close to the marketing area.
Transport
The transport of materials and products to and from the plant will be an
overriding consideration in site selection. If practicable, a site should be
selected that is close to at least two major forms of transport: road, rail,
waterway (canal or river), or a sea port. Road transport is being increasingly
used, and is suitable for local distribution from a central warehouse. Rail
transport will be cheaper for the long-distance transport of bulk chemicals. Air
transport is convenient and efficient for the movement of personnel and
essential equipment and supplies, and the proximity of the site to a major
airport should be considered.
Availability of labour
Labour will be needed for construction of the plant and its operation. Skilled
construction workers will usually be brought in from outside the site area, but
there should be an adequate pool of unskilled labour available locally; and
labour suitable for training to operate the plant. Skilled tradesmen will be
needed for plant maintenance. Local trade union customs and restrictive
practices will have to be considered when assessing the availability and
suitability of the local labour for recruitment and training.
Utilities (services)
Chemical processes invariably require large quantities of water for cooling and
general process use, and the plant must be located near a source of water of
suitable quality. Process water may be drawn from a river, from wells, or
purchased from a local authority. At some sites, the cooling water required can
be taken from a river or lake, or from the sea; at other locations cooling towers
will be needed. Electrical power will be needed at all sites. A competitively
priced fuel must be available on site for steam and power generation.
Environmental impact, and effluent disposal
All industrial processes produce waste products, and full consideration must be
given to the difficulties and cost of their disposal. The disposal of toxic and
harmful effluents will be covered by local regulations, and the appropriate
authorities must be consulted during the initial site survey to determine the
standards that must be met. An environmental impact assessment should be
made for each new project, or major modification or addition to an existing
process.
Local community considerations
The proposed plant must fit in with and be acceptable to the local community.
Full consideration must be given to the safe location of the plant so that it does
not impose a significant additional risk to the community.On a new site, the
local community must be able to provide adequate facilities for the plant
personnel: schools, banks, housing, and recreational and cultural facilities.
Land (site considerations)
Sufficient suitable land must be available for the proposed plant and for future
expansion. The land should ideally be flat, well drained and have suitable load-
bearing characteristics. A full site evaluation should be made to determine the
need for piling or other special foundations.
Climate
Adverse climatic conditions at a site will increase costs. Abnormally low
temperatures will require the provision of additional insulation and special
heating for equipment and pipe runs. Stronger structures will be needed at
locations subject to high winds (cyclone/hurricane areas) or earthquakes.
Political and strategic considerations
Capital grants, tax concessions, and other inducements are often given by
governments to direct new investment to preferred locations; such as areas of
high unemployment. The availability of such grants can be the overriding
consideration in site selection.


SITE LAYOUT

The process units and ancillary buildings should be laid out to give the most
economical flow of materials and personnel around the site. Hazardous
processes must be located at a safe distance from other buildings. Consideration
must also be given to the future expansion of the site. The ancillary buildings
and services required on a site, in addition to the main processing units
(buildings), will include:
1. Storages for raw materials and products: tank farms and warehouses.
2. Maintenance workshops.
3. Stores, for maintenance and operating supplies.
4. Laboratories for process control.
5. Fire stations and other emergency services.
6. Utilities: steam boilers, compressed air, power generation, refrigeration,
transformer stations.
7. Effluent disposal plant.
8. Offices for general administration.
9. Canteens and other amenity buildings, such as medical centres.
10. Car parks.

When roughing out the preliminary site layout, the process units will normally
be sited first and arranged to give a smooth flow of materials through the
various processing steps, from raw material to final product storage. Process
units are normally spaced at least 30 m apart; greater spacing may be needed
for hazardous processes. The location of the principal ancillary buildings
should then be decided. They should be arranged so as to minimise the time
spent by personnel in travelling between buildings. Administration offices and
laboratories, in which a relatively large number of people will be working,
should be located well away from potentially hazardous processes. Control
rooms will normally be located adjacent to the processing units, but with
potentially hazardous processes may have to be sited at a safer distance. The
sitting of the main process units will determine the layout of the plant roads,
pipe alleys and drains. Access roads will be needed to each building for
construction, and for operation and maintenance.
Utility buildings should be sited to give the most economical run of pipes to
and from the process units. Cooling towers should be sited so that under the
prevailing wind the plume of condensate spray drifts away from the plant area
and adjacent properties. The main storage areas should be placed between the
loading and unloading facilities and the process units they serve. Storage tanks
containing hazardous materials should be sited at least 70 m (200 ft) from the
site boundary.


A TYPICAL PLANT LAYOUT:-






COMMISSIONING, START-UP AND SHUT DOWN
COLUMN COMMISSIONING:
It refers to the process of preparing the column for operation. The main
objectives are:
1) Clear the system of undesirable materials.
2) Test the column and rectify potential problems.
3) Take preventive actions against performance deterioration.
Most commissioning operations are performed using readily available liquids
and gases, such as air, nitrogen, steam, water or oil. An important thing to note
is that the column and associated equipments are seldom designed to cater
specifically to commissioning operations. Therefore, they must be tailored to
suit the limitations of the available system.
START-UP:
The following steps are observed:
1. Commissioning
2. Pressure-up
3. Column heating (and/or cooling)
4. Introduction to feed
5. Introducing heating and cooling sources
6. Bring to desired operating conditions

SHUT DOWN:
1. Reducing column/unit rates.
2. Shutting down heating/cooling surfaces.
3. Stopping feed
4. Draining liquid
5. Cooling/heating the column/unit
6. Bringing the unit to atmospheric pressure
7. Eliminating undesirable materials
8. Preparing to opening to atmosphere

VARIOUS COMMISSIONING ACTIVITIES

1. LINE BLOWING:
A common pre-start up practice is to pressurize the column with air or
nitrogen. The unit then serves as vapour reservoir for blowing lines
connected to the unit to remove construction debris.

2. PRESSURIZING OR DEPRESSURIZING:
Pressurizing or depressurizing is performed during commissioning, start-ups
and shut-downs. They are used to check the columns for pressure retention
and leaks. Remove air or inert gas prior to start-up, free the column of gas
(e.g. hydrocarbon) at shut-downs or prepare the column for entry by
personnel for inspection of the column internals. Location and set pressure
of relief valves and/or bursting disks as well as major vents should be
checked.

3. PURGING:
A column needs to be purged with an inert gas prior to start-up to remove
air if it is used for separating combustible materials. The inert gas can then
be purged with process gas. The reverse steps are performed at shut-down.
Drain and vent valves must be opened intermittently so that no dead pockets
are left unpurged.

4 . STEAMING:
A unit may be steamed during commissioning to drive the air out heat the
column up, clear blockages or leak test the unit. Problem associated with it
could be creation of vacuum, water hammer, overheating etc. Steaming is
done before purging.

5. LEAK TESTING:
After purging and before introducing the process gas column is leak tested.
The most common technique is pressurizing the unit up with inert gas
(liquid N2) with all vents and drain closed.

6. WASHING:
Washing is done during start up and shut down for one or more of the
following reasons
- To remove scale, mud etc.
- To coo, the column
- To dissolve or carry away sticky deposits. Water should be drained out
after washing.

7. DRY OUT :
Water should be drained out after washing. To remove water from the
column dry out can be done using hot water or liquid.

8. BLINDING AND UNBLINDING:
Blinds and /or slip plates (spades) are usually installed in all lines which
leave or enter a unit in order to positively eliminate leakage of materials into
the unit when air is introduced. During start up, the plates are removed. The
sequence of blinding and unblinding must be carefully prepared / planned
prior to start up or shut down. A checklist of all blinds should be made.
Blinds be properly tagged, and tag ID must be reflected on checklist.


MAINTENANCE AND SAFTEY MEASURES:-
Safety and Loss Prevention
Any organization has a legal and moral obligation to safeguard the health and
welfare of its employees and the general public. Safety is also good business;
the good management practices needed to ensure safe operation will also
ensure efficient operation. The term "loss prevention" is an insurance term, the
loss being the financial loss caused by an accident. This loss will not only be
the cost of replacing damaged plant and third party claims, but also the loss of
earnings from lost production and lost sales opportunity. All manufacturing
processes are to some extent hazardous, but in chemical processes there are
additional, special, hazards associated with the chemicals used and the process
conditions. The designer must be aware of these hazards, and ensure, through
the application of sound engineering practice, that the risks are reduced to
acceptable levels.
Safety and loss prevention in process design can be considered under the
following broad headings:
1. Identification and assessment of the hazards.
2. Control of the hazards: for example, by containment of flammable and toxic
materials.
3. Control of the process: Prevention of hazardous deviations in process
variables (pressure, temperature, flow), by provision of automatic control
systems, interlocks, alarms, trips; together with good operating practices and
management.
4. Limitation of the loss. The damage and injury caused if an incident occurs:
pressure relief, plant layout, provision of fire-fighting equipment. In this
chapter the discussion of safety in process design will of necessity be limited.
INTRINSIC AND EXTRINSIC SAFETY
Processes can be divided into those that are intrinsically safe, and those for
which the safety has to be engineered in. An intrinsically safe process is one in
which safe operation is inherent in the nature of the process; a process which
causes no danger, or negligible danger, under all foreseeable circumstances (all
possible deviations from the design operating conditions). Clearly, the designer
should always select a process that is inherently safe whenever it is practical,
and economic, to do so. However, most chemical manufacturing processes are,
to a greater or lesser extent, inherently unsafe, and dangerous situations can
develop if the process conditions deviate from the design values. The safe
operation of such processes depends on the design and provision of engineered
safety devices, and on good operating practices, to prevent a dangerous
situation developing, and to minimize the consequences of any incident that
arises from the failure of these safeguards.
The term "engineered safety" covers the provision in the design of control
systems, alarms, trips, pressure-relief devices, automatic shut-down systems,
duplication of key equipment services; and fire-fighting equipment, sprinkler
systems and blast walls, to contain any fire or explosion.

THE HAZARDS
Toxicity
Most of the materials used in the manufacture of chemicals are poisonous, to
some extent. The potential hazard will depend on the inherent toxicity of the
material and the frequency and duration of any exposure. It is usual to
distinguish between the short-term effects (acute) and the long-term effects
(chronic). The permissible limits and the precautions to be taken to ensure the
limits are met will be very different for these two classes of toxic materials.
Industrial hygiene is as much a matter of good operating practice and control as
of good design.
Control of substances hazardous to health
The employer is required to carry out an assessment to evaluate the risk to
health, and establish what precautions are needed to protect employees. A
written record of the assessment would be kept, and details made available to
employees. The designer will be concerned more with the preventative aspects
of the use of hazardous substances. Points to consider are:
1. Substitution: of the processing route with one using less hazardous
material, Or substitution of toxic process materials with non-toxic, or
less toxic materials.
2. Containment: sound design of equipment and piping, to avoid leaks. For
example, specifying welded joints in preference to gasketed flanged joints
(liable to leak).
3. Ventilation: use open structures, or provide adequate ventilation systems.
4. Disposal: provision of effective vent stacks to disperse material vented from
pressure relief devices; or use vent scrubbers.
5. Emergency equipment: escape routes, rescue equipment, respirators, safety
showers, eye baths.
In addition, good plant operating practice would include:
1. Written instruction in the use of the hazardous substances and the risks
involved,
2. Adequate training of personnel.
3. Provision of protective clothing.
4. Good housekeeping and personal hygiene.
5. Monitoring of the environment to check exposure levels. Consider the
installation of permanent instruments fitted with alarms.
6. Regular medical check-ups on employees, to check for the chronic effects of
toxic materials.
Explosions
An explosion is the sudden, catastrophic, release of energy, causing a pressure
wave (blast wave). An explosion can occur without fire, such as the failure
through over-pressure of a steam boiler or an air receiver. When discussing the
explosion of a flammable mixture it is necessary to distinguish between
detonation and deflagration. If a mixture detonates the reaction zone propagates
at supersonic velocity (approximately 300 m/s) and the principal heating
mechanism in the mixture is shock compression. In a deflagration the
combustion process is the same as in the normal burning of a gas mixture; the
combustion zone propagates at subsonic velocity, and the pressure build-up is
slow. Whether detonation or deflagration occurs in a gas-air mixture depends
on a number of factors; including the concentration of the mixture and the
source of ignition. Unless confined or ignited by a high-intensity source (a
detonator) most materials will not detonate. However, the pressure wave (blast
wave) caused by a deflagration can still cause considerable damage.

Sources of ignition
Though precautions are normally taken to eliminate sources of ignition on
chemical plants, it is best to work on the principle that a leak of flammable
material will ultimately find an ignition source.
Electrical equipment
The sparking of electrical equipment, such as motors, is a major potential
source of ignition, and flame proof equipment is normally specified.
Electrically operated instruments, controllers and computer systems are also
potential sources of ignition of flammable mixtures.
Static electricity
The movement of any non-conducting material, powder, liquid or gas, can
generate static electricity, producing sparks. Precautions must be taken to
ensure that all piping is properly earthed (grounded) and that electrical
continuity is maintained around flanges. Escaping steam, or other vapours and
gases, can generate a static charge. Gases (CO
2
) escaping from a ruptured
vessel can self-ignite from a static spark.

Process flames
Open flames from process furnaces and incinerators are obvious sources of
ignition and must be sited well away from plant containing flammable
materials.
Miscellaneous sources
It is the usual practice on plants handling flammable materials to control the
entry on to the site of obvious sources of ignition; such as matches, cigarette
lighters and battery-operated equipment. The use of portable electrical
equipment, welding, spark-producing tools and the movement of petrol-driven
vehicles would also be subject to strict control Exhaust gases from diesel
engines are also a potential source of ignition.
Pressure
Over-pressure, a pressure exceeding the system design pressure, is one of the
most serious hazards in chemical plant operation. Failure of a vessel, or the
associated piping, can precipitate a sequence of events that culminate in a
disaster. Pressure vessels are invariably fitted with some form of pressure-relief
device, set at the design pressure, so that (in theory) potential over-pressure is
relieved in a controlled manner.
Temperature deviations
Excessively high temperature, over and above that for which the equipment
was designed, can cause structural failure and initiate a disaster. High
temperatures can arise from loss of control of reactors and heaters; and,
externally, from open fires. In the design of processes where high temperatures
are a hazard, protection against high temperatures is provided by:
1. Provision of high-temperature alarms and interlocks to shut down reactor
feeds, or heating systems, if the temperature exceeds critical limits.
2. Provision of emergency cooling systems for reactors, where heat continues
to be
generated after shut-down; for instance, in some polymerization systems,
3. Structural design of equipment to withstand the worst possible temperature
excursion.
4. The selection of intrinsically safe heating systems for hazardous materials.
Steam, and other vapour heating systems, is intrinsically safe; as the
temperature cannot exceed the saturation temperature at the supply pressure.
Other heating systems rely on control of the heating rate to limit the maximum
process temperature. Electrical heating systems can be particularly hazardous.

Fire protection
To protect against structural failure, water-deluge systems are usually installed
to keep vessels and structural steelwork cool in a fire. The lower section of
structural steel columns are also often lagged with concrete or other suitable
materials.
Noise
Excessive noise is a hazard to health and safety. Long exposure to high noise
levels can cause permanent damage to hearing. At lower levels, noise is a
distraction and causes fatigue.
The basic safety and fire protective measures that should be included in all
chemical process designs are listed below:-
1. Adequate, and secure, water supplies for fire fighting.
2. Correct structural design of vessels, piping, steel work.
3. Pressure-relief devices.
4. Corrosion-resistant materials, and/or adequate corrosion allowances.
5. Segregation of reactive materials.
6. Earthing of electrical equipment.
7. Safe location of auxiliary electrical equipment, transformers, switches gear.
8. Provision of back-up utility supplies and services.
9. Compliance with national codes and standards.
10. Fail-safe instrumentation.
11. Provision for access of emergency vehicles and the evacuation of
personnel.
12. Adequate drainage for spills and fire-fighting water.
13. Insulation of hot surfaces.
14. No glass equipment used for flammable or hazardous materials, unless no
suitable alternative is available.
15. Adequate separation of hazardous equipment.
16. Protection of pipe racks and cable trays from fire.
17. Provision of block valves on lines to main processing areas,
18. Protection of fired equipment (heaters, furnaces) against accidental
explosion and fire.
19. Safe design and location of control rooms.

SAFETY CHECK LISTS
Check lists are useful aids to memory. A check list that has been drawn up by
experienced engineers can be a useful guide for the less experienced. A short
safety check list, covering the main items which should be considered in
process design, is given below.
Design safety check list
Materials
(a) Flash-point
(c) Auto ignition temperature
(d) Composition
(e) Stability (shock sensitive?)
(g) Corrosion
(h) Physical properties (unusual?)
(i) heat of combustion/reaction
Process
1. Fermenter:
(a) Exothermicheat of reaction
(b) Temperature controlemergency systems
(d) Effect of contamination
(e) Effect of unusual concentrations (including catalyst)
(f) Corrosion
2. Pressure systems
(a) Need?
(b) Design to current codes (BS 5500)
(c) Materials of constructionadequate?
(d) Pressure reliefadequate?
(e) Safe venting systems
(f) Flame arresters
SAFETY AND LOSS PREVENTION
Control systems
(a) Fail safe
(b) Back-up power supplies
(c) High/low alarms and trips on critical variables
(i) Temperature
(ii) Pressure
(iii) Flow
(iv) Level
(v) Composition
(d) Back-up/duplicate systems on critical variables
(e) Remote operation of valves
(f) Block valves on critical lines
(g) Excess-flow valves
(h) Interlock systems to prevent mis-operation
(i) Automatic shut-down systems
Storages
(a) Limit quantity
(b) Inert purging/blanketing
(c) Floating roof tanks
(f) Earthing
(g) Ignition sourcesvehicles
General
(a) Compliance with electrical codes
(b) Adequate lighting
(c) Lightning protection
(d) Sewers and drains adequate, flame traps
(e) Dust-explosion hazards
(f) Build-up of dangerous impuritiespurges
(g) Plant layout
(h) Separation of units
(ii) Access
(iii) Sitting of control rooms and offices
(iv) Services
(i) Safety showers, eye baths
Fire protection
(a) Emergency water supplies
(b) Fire mains and hydrants
(c) Foam systems
(d) Sprinklers and deluge systems
(e) Insulation and protection of structures
(f) Access to buildings
(g) Fire-fighting equipment

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Sinnot, R.K, Coulson and Richardsons Chemical Engineering, vol-6,
Fourth edition, 2005
Trrybal, Robert E., Mass transfer Operations, Third edition, 1981
Perry, Robert H, Green, Don W., Chemical Engineers Handbook, 1999
Chattopadhyay, P Unit Opeartions of Chemical Engineering, vol-1,
2003
McCabe, Warren L, Smith, Julian C, Harriott Peter Unit Operations Of
Chemical Engineering, Sixth edition, 2001
Process biotechnology fundamentals
Eckman, Donald P., Industrial Instrumentation, 1991
Hesse, Herman C., Rushton, J.Henry, Process Equipment Design,
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