Internship Report
Internship Report
1. Introduction……………………………………………………………….…..…1
2. Products…………………………….………………………………………..…..2
5. Quality control……………………………………………….…………….….…9
9. Boiler………………………………………………………………………..….23
11. Nomenclature…………………………………………………………………32
COMPANY INTRODUCTION
Pharmagen Limited is a Pakistani incorporated, Public Limited (non quoted) Company, which
was established in 1990 for undertaking pharmaceutical business and over the years it has
become the leading producer of APIs (Active Pharmaceutical Ingredients) in
Pakistan. Pharmagen group is a dynamic organization that has been providing quality services
and products for healthcare and pharma sector.
Excellent state-of-the-art production facilities at its manufacturing site near Lahore namely:
Other Objectives
Occupational health and safety law
Pharmagen OH&S objectives
Noise Control residual current device(RCD)
Personel protective equipment (PPE)
Failure to abide by the signage
Blue sinage in the work place
Emergency procedures
Avoid aggravating the fire by using unsuitable extinguishers
Do not waste time salvage any of your possessions.
Fire extinguishers:
Dry chemical (wood, paper, plastic,flammable)
Water , AFFF (wood , Paper , Plastic)
Carbon dioxide , Haltron.
Incident report is very important regarding safety point of view because it will provide picture of
the whole scenario. there are two types of incident:
1- Near Miss
2- Accidents
Near miss are those incidents in which actually no damage occur but there was possibility to
cause serious damage.
Accidents are those incidents in which loss of life or property takes place.
UV radiation is most intense during the middle of the day between 10am until 3pm from
September to April. Only 10 to 15 minutes for skin damage to occur.
Nodular melanoma
Thermal discomfort.
Hydrant line
Hydrant pillar
Monitor
Fire hose
Pumps of 40hp and 60hp
Pressure is 5 to 6 bar.
50 ft 50 ft
1. Smothering.
2. Cooling.
3. Starvation.
Types of nozzles:
1. Jet nozzle.
2. Multipurpose nozzle.
Mechanical foam
Sand pite.
Mechanical foam .
Protean+ water.
Centrifugal pump is used because in this system pump keeps running continuously.
If PD pump is used then it keeps applying pressure which should effect the piston.
Contractual activities.
Revision history.
Bill for vehicle fare.
Bill for daily wages labour.
Labour hiring approval form.
Employees facilities.
Furniture fixture.
Handling of communication services.
Handling of company uniform & shoes at factory.
Recreational activities & external visits.
Polices for employers.
Roaster.
Visitors entry.
√ n+1
“n” is the no. of containers .
For example no. of drums are 64 then
= √ 64+1
=8+1=9
So samples are collected from 9 containers.
In material testing following steps are involved and then documentation is done. Finished
product testing is done in which sample of finished product are tested and if they are clear then
passed.
Task performed by quality control:
Swab test
HPLC test
Purchase department report, Manufacturer report, Standard testing report and Sample testing
report
Specific no. is given to the specific batch
Appearance of the material is checked according to the specification given to the analysts.
Some of the abbreviations used there:
MSA (material sample advice)
RSD (relative standard deviation)
MSDS of finished product
1. MC 1.33 39
2 MIBK 0.8 117-118
3. PA 0.905 165
4. IPA 0.786 82.5
5. Methanol 0.785 65
6. Acetone 0.79 56
7. n-Butanol 0.81 121-122
8. EA 0.897 77.1
9. TEA 0.725 89.5
EQUIPMENT
Reactor
Pumps
Distillation Column
Receivers
Spent Tank
Reflux Drum
Decanter
Condenser
Ball Valve
Butterfly valves
Safety valves(Relive valves )
Thermocouple
AUXILIARIES
This is the list of auxiliaries used at solvent recovery
Steam
H 2 SO 4
HCl
Cooling Water
Tab Water
Chilled Water
Caustic
Electricity
Compressed air
BY PRODUCT
It is the main by product of solvent recovery
PRODUCTS
These are the products recovered at solvent recovery
MC recd
MIBK recd
IPA recd
PA recd
Methanol recd
Acetone recd
n- butanol recd
ea recd
tea recd
SPENT
Spent is the chemical used in the production unit and can be recovered at solvent recovery.
Reactors
CR -8 7000L
CR-9 4600L
CR -10 7000L
CR -11 7000L
Recivers
R -1 2600L
R -2 2600L
R-3 2600L
Decantor 150L
BD -1
Solvent Recovery
R -6 (reactor)
TEA vessel
BD -2
Solvent recovery
At CR -8
Recovered(means which is gathered from the spent and then passes through the solvent recovery
plant and used again in the plant).
Recovery of MC:
1. Ensure that still empty and receivers are also clean and empty.
2. Vent value over CW and CHW feed and return lines of main and backing condenser.
3. Charge 7000L spent MC from MC over ground (OG) tank to still using transfer pump.
4. Apply steam (approx pressure =05-1.0kg/cm 2) to the jacket of still and distill off all MC
through decanter, reflux pot and collect in relevant receivers.
5. Adjust value in the decanter to drain upper water layer to disposal and collect denser
Methylene.
6. MC layer in the receiver through reflux pot.
7. Transfer the residue from still to effluent pit.
8. Recharge all distilled MC collected in stop No. 4 to still, heat the batch for 2nd distillation.
9. Complete azeotropic drying, when moisture drops less than 0.5% start collecting MC in
receivers at the rate of 200L/hr till column temp 60°C.
Note: Maintain half level in the reflux pot during fraction.
10. Start recording the control parameter in the relevant log sheet.
11. When column top temperature exceeds 60°C, wt off steam supply to jacket of still.
12. Transfer the residue to effluent pit-3 and wash still with plenty of water.
13. Close value on CW and CHW feed and return lines of main and backing condenser
respectively.
14. Sampling advice sheet of MC to Quality control lab.
15. MC passed by QC should be drum up or transfer to the OG tank.
Methanol and Acetone are recovered similar to the process mention above.
Note: This is the general procedure for MC recovery. Can vary to certain extent.
Dimensions of the shell and tube side fluid connections are defined
Calculation of expansion joint dimensions(to compensate for shell and tube side differential
expansion due to temperature difference).
Calculation of tube
Cold Fluid:
Methanol [shell side]
Inlet temperature=20°C=68F
Outlet temperature=64°C=147.2F
Cp =1.61KJ/kgF
Hot fluid:
Water [tube side]
Inlet temperature=100°C=212F
Outlet temperature=x=?
Cp= 1.890KJ/Kg K
Heat load
Heat load = mCp∆T
=161*79=12719KW
FindingT 2
Q1=Q2
12719=80*1.890(212-x)
12719=151.2(212-x)
84.12=212-x
X=212-84.12
X=127.88F
∆Tlm:
( Ti−t 2 )−(T 2−t 1)
∆Tlm= (T 1−t 2)
ln
(T 2−t 1)
( 212−147.2 )−(128−68)
∆Tlm= (212−147.2)
ln
(128−68)
( 65 )−(60)
∆Tlm= ( 65)
ln
( 60)
5
∆Tlm=
ln 1.083
5
∆Tlm=
0.077
∆ Tlm =65F
correction factor:
Ft=1
U=2000W/m2F
Provisional area
3
12719∗10
A=
65∗2000
12719∗103
A=
130000
A=0.0978*103
A=98m2
L=4.83m
Area 98
Number of tubes= =
Area of one tube 0.303
=323.43
Triangular pitch=1.25
1
323.43 2.207
Bundle diameter Db=20[ ]
0.249
Db=514.98mm
Clearance diameter=59mm
=574mm
=170F
3.14
Tube cross sectional area = *162
4
=201mm2
=32562*10−6
=32562/106
=0.032562m2
=0.683kg/sm2
Specification of water:
Density of water=1000kg/s
Viscosity of gasoline=0.000282kg/ms
Thermal conductivity=0.6W/mF
h idi µ 0.14
= j h ℜ Pr 0.33( )
kf µw
−3 −3
1000∗6.83∗10 ∗16∗10
Re=ƿudi/µ=
0.28∗10−3
1.890∗10−3∗0.28∗10−3
Pr=Cpu/kf=
0.6
=0.88*10−6
L 4.83∗103
=
di 16
=0.301*103
From[12]
j h =¿ 2.5∗10
−2
¿
0.6 −2 −6 0.33
hi= −3
∗2.5∗10 ∗390.3∗( 0.88∗10 )
16∗10
=35.07*10−3 W/m2 F
=115mm
(25−20)
Cross flow area As= ∗574∗115∗10−6
25
=0.013202m2
=2.098kg/sm2
1.1 2 2
Equivalent diameter de= ( ( 25 ) −0.917∗20 )
20
=14.2mm
=107.6F
Specifications of methanol:
density= 782kg/m3
Cp=1.61kj/kgF
Thermal conductivity=0.203W/mF
−3
2.098∗14.2∗10
Re=Gsde/µ= −3 =57.23
0.521∗10
1.61∗0.521
Pr= =6.7
0.203
j h =1.5∗10
−2
0.203
hs= −3
∗1.5∗10−2∗54.23∗4.132
14.2∗10
hs =47.94
1
=
1 1
+ +
20∗10−3 ln ( 2016 ) + 2016∗1 + 20
16
∗1
U o 47.94 50 100 90 35.07∗10
−4
=350.50W/m2 F
Pressure drop:
Tube side
Re=390.3
−2
j s=2.5∗10
=29248.296N/m2
Shell side
Linear velocity
=2.098m/s
Re =57.23
j f =1.5*10−2
( )( )
3
−2 574 4.83∗10 2
∆ Ps=8∗1.5∗10 (782∗0.9 )/2
14.2 115
=64KPa
Results of this example could be other than this. It’s just an example.
BOILER
Boiler safety: Boiler should be used according to the SOP’s of international standards. Keep
proper maintenance.
Ans.: Solvent recovery is used to recover solvents from the residue of production plant, which
are mostly used in the plants during different processes.
Ans.: At solvent recovery spent solvent is charged into still where it is heated to the boiling point
of the solvent (desired product) it passes through the distillation column, then these vapors are
cooled down through condensers and in the end they are collected into receivers.
Ans.: At solvent recovery plant the main equipment used includes 1.reactor (still) 2.distillation
column 3.condenser 4.decanter 5.reflux drum 6.pumps.
Ans.: Steam, cooling water, chilled water, compressed air, electricity, caustic, HCL and
H 2 SO 4 are used inthis plant .
Ans.: In solvent recovery reactor mostly used for boiling the feed.
Ans.: The contents of the reactor are heated through steam, which circulates inside a steam
jacket coiled around the still.
Ans.: Steam is supplied through insulated pipelines coming from the boilers to the plant and then
the heat is transferred to the system through steam jackets.
Ans.: Although packed bed columns are used most often for absorption, they are also used for
the distillation of vapor-liquid mixtures. The packing provides a large surface area for vapor-
liquid contact, which increases the column's effectiveness. Distillation columns are also used to
provide residence time to the constituents of the solvent to purify and it provides temperature
gradients.
Q.10: How many unit operations take place inside the distillation column?
Ans.: Heat transfer, mass transfer, vaporization, condensation, rectification and stripping take
place inside the distillation column.
Ans.: Flash distillation takes place inside the column of solvent recovery.
Ans.: Vapors move in the upward direction due to heat and due to low pressure inside the
distillation column than reactor.
Q.14: How do vapors move from the top of the distillation column to the condenser?
Ans.: When vapors, inside the condenser, condenses, they create vacuum due to condensation so
more vapors enter into the condenser
Ans.: Main condenser uses cooling water as a cooling agent but the backing condenser uses
chilled water as a cooling agent.
Ans.: Decanter is used to settle the components of the fluid coming from the condenser. It is
used to control the supply.
Ans.: Mostly ball valves are used throughout the pipe lines. Safety valves are used at still
(pressure relief valves).
Ans.: Centrifugal pumps are used for transferring solvents. Vacuum pump is used along the PA
recovery. Pneumatic pumps are used for charging still and drums.
Q.23: Why does steam enter from the top of the still?
Ans.: Steam enters from the top of the still because when it condenses, the condensate moves in
the downward direction. If steam enters from the bottom the condensate moves downward and it
accumulate steam there so heat transfers to the condensate instead of solvent in the still.
Q.24: Why do vapors enter from the top of the main condenser?
Ans.: Vapors enter from the top because in the condenser when vapors condense, they move in
the downward direction due to gravity. If vapors enter from the bottom the condensate does not
allow the vapors to enter inside the condenser.
Q.25: Which type of flow meter is used to measure the flow rate?
Ans.: we come to know by collecting sample from the receivers and reflux drum, by checking
the moisture from QC lab. When the amount of moisture is according to the requirement the
product is collected in the recovered tank.
Q.28: How much amount of packing is used inside the distillation column?
Q.29: Why are some of the distillation column taller and some shorter?
Ans.: Effluent and crude are treated in the recovery have shorter column.
Ans.: It’s main purpose to avoid backward flow or to trap gases and fluid.
Ans.: Air pollution control device can be used to remove some particulates or gases from
industrial exhaust streams. Scrubbers are used to suck fumes from contaminated area and release
them in the atmosphere in safe condition.
Ans.: To wash the gases and fumes which are going to be exhausted and the exhaust gases of
combustion may contain substances considered harmful to the environment, the scrubber may
remove or neutralize them. A wet scrubber is used for cleaning air, fuel gas or other gases of
various pollutants and dust particles.
Ans.: Where there are chances of fire or corrosive material needs to be transferred then
preferable choice is the pneumatic pump.
Pneumatic systems are reliable generally have long operating lives and require little
maintenance. Because gas is compressible, equipment is less subject to shock damage. Gas
absorbs excessive force, whereas fluid in hydraulics directly transfers force. Compressed gas can
be stored, so machines still run for a while if electrical power is lost.
Safe to use, they can operate at inflammable places, because of pneumatic pump very low
chance of fire.
Q.35: What is the power of pump used at solvent recovery?
Q.37: What is the capacity of the vessels and equipment used at solvent recovery?
Ans.: In general
Q.38: What are the specifications of the solvents recovered at solvent recovery?
1. MC 1.33 39
2 MIBK 0.8 117-118
3. PA 0.905 165
4. IPA 0.786 82.5
5. Methanol 0.785 65
6. Acetone 0.79 56
7. n-Butanol 0.81 121-122
8. EA 0.897 77.1
9. TEA 0.725 89.5
DCM is the least toxic of the simple chlorohydrocarbons, but it is not without health risks, as its
high volatility makes it an acute inhalation hazard.2
1
Rossberg, M. et al. (2006) "Chlorinated Hydrocarbons" in Ullmann's Encyclopedia of Industrial Chemistry,
Wiley-VCH, Weinheim.
2
Rioux JP, Myers RA (1988). "Methylene chloride poisoning: a paradigmatic review". J Emerg Med. 6 (3): 227–238.
Ans. Ethyl Alcohol also called ethanol molecular formula is C2H5OH. Ethyl alcohol is an
important industrial chemical; it is used as a solvent.
irritant.4
liquid.
3
"Isopropanol". Sigma-Aldrich. 19 January 2012. Retrieved 6 July 2012.
4
Kolar, Wes (July 11, 2000). "Lab Safety Review: Danger! – Peroxides Present"
5
Kruse, JA (October 2012). "Methanol and ethylene glycol intoxication.". Critical care clinics. 28 (4)
Pharmagen is one of the reputable companies in the field of bulk production of pharmaceuticals.
I worked at solvent recovery as an internee, I observed that they reduced the waste as much as
they can, which save loss of useful products and also save the environment. By periodic
maintenance of equipment company can save the loss of steam and other utilities at solvent
recovery.
Install PLC systems to control the process efficiently and effectively at solvent recovery.
CW Cooling Water
MC Methylene Chloride
PA Pivalic Acid
EA Ethyl Alcohol
CR Ceph. Reactor
QC Quality Control