1

Acknowledgement
This training report is prepared after undergoing 6 week industrial training
from 1stJune to 1stAugust, 2016, in the process department at Ind-Swift
Laboratories Ltd (ISLL) Derabassi, Punjab. The report gives a brief
description of various processes and the equipments used in the plant. The
report is based on study of the Solvent Recovery Plant (SRP).

I am highly thankful to Mr. Subodh Gupta, for taking me as trainee to get

hands-on training at the plant. I also express my sincere thanksto the HR
department, Mrs. Sarika, Surinder Sir and Mr. Daljit Singh (Sr. Executive of
SRP plant), all the operators and workers at the plant forhelping and guiding
me throughout my training and making it fruitful first hand experience for
me.

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COMPANY PROFILE
Ind-Swift is one of the leading pharmaceutical grounds in India engaged in
manufacturing of drugs, formulations, and health care products. The
various establishments of the group are located in Punjab (Derabassi),
Haryana (Panchkula), Himachal Pradesh (Parwanoo) and Jammu.

The group has total strength of trained and motivated manpower of over
1500 persons, Including 300 strong field strength and 30 doctorates and
postgraduates in various fields of science and technology.

The visionary promoters with their techno managerial skills have nurtured
the growth and diversification of the group in and around the nucleus of
pharmaceutical business. Since it’s established in 1984, Ind swift has
developed considerable technical expertise and significant experience.

The strength of the group is in its strategic and timely diversification,

massive infrastructure, physical resources and a team of dedicated
professionals pursuing higher level of quality, productivity and excellence.

ABOUT THE COMPANY

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Laboratories Ltd is a part of the Ind-swift Group and

is based at Chandigarh, India. The company manufactures and sells active
pharmaceutical ingredients (API).

 Ind-Swift product pipeline consists of 25 products, which includes

drugs, which include Clarithromycin, Atorvastatin,
Fexofenadine,Clopidogrel, Nitazoxanide, Pioglitazone, Letrozole and
Anastrozole, Venlafaxine and Quetipine and Aripirazole.

 The company has one subsidiary namely, Ind-Swift Laboratories Inc in

USA. Ind-Swift Laboratories Ltd was incorporated in the year 1995 as
a joint venture between Ind-Swift Ltd and Punjab State Industrial
Development Corporation.

 Later, Ind-Swift purchased Punjab State Industrial Development

Corporation equity to emerge as a single largest shareholder in the
company. The company commenced their production in the year
1997. Over a short period, the company has emerged as a
respectable and dependable supplier of Bulk-Actives in more than 40
countries.

 In the year 1997, the company went public and concentrated on the
manufacture of Active Pharmaceutical Ingredients (API). In the year
1998-99, it launched two molecules, Clarithromycin and
Roxithromycin. The in-house R&D developed Clarithromycin Granules
for the first time in India.

 In the year 2000, the company developed a new drug namely,

Astrovastatin. In addition, it entered into an agreement with eight
international pharmaceutical companies to source their requirements
for Clarithromycin Fexofenadine Roxithromycin and Candesartan
from the company.
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 During the year 2003-04, the company increased the production

capacity of bulk drugs/ intermediates from 81.18 TPA to 120 TPA. In
addition, it commissioned the granulation facility as per CGMP
standards.

 It launched four new products namely, Acamprosate, Ezetimib,

Anastrazole and Nitazoxanide. In January 2, 2004, the company
incorporated a wholly owned subsidiary, namely Ind-Swift
Laboratories Inc in USA to strengthen the company's presence in
contract research and manufacturing services. In June 2004, the
subsidiary company commenced their operations.

 During the year 2004-05, the company expanded the production

capacity of bulk drugs/ intermediates from 120 TPA to 150 TPA. It
commissioned waste heat recovery unit to reduce energy costs. It
opened an office in China to facilitate the import of raw materials.
The company introduced five new products in the market.

 During the year 2005-06, the company completed and commissioned

a new plant at Samba in Jammu & Kashmir to manufacture products
for the domestic markets. Also, a new state of the art Research &
Development center was set up at Mohali, Punjab with an investment
of USD 5 million.

 It increased the production capacity of bulk drugs/ intermediates by

87.03 TPA to 237.03 TPA. The company launched new products
namely, Letrozole, Anastrozole,
Venlafaxine,Lavofloxacin,Quetipine&Aripirazole in the market.

 It entered into a joint venture with FarayandChemi Hakim Co, a

private joint stock company registered under the law of Iran to focus
on the marketing of the products in Middle East & Iran.

 During the year 2006-07, the company expanded the production

capacity of bulk drugs/ intermediates by 18.85 TPA to 255.88 TPA. In
April 2006, the company inaugurated their new manufacturing
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facilities at Baddi in Himachal Pradesh to manufacture tablets,

injectibles and liquids.

 During the year 2007-08, the company entered into the field of
Phytochemicals, where, the company has put to operation a new
manufacturing facility to manufacture mint-based products. It
increased the production capacity of bulk drugs/ intermediates by
162.30 TPA to 418.18 TPA.

Derabassi Plant

Products

Product Name Therapeutic Category

 Acamprosate Calcium Alcohol Abstinence

 Anastrozole Aromatase Inhibitor

 Aripiprazole Anti Psychotic

 AtomoxetineHCl Hyperactivity disorder (ADHD)

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 Bexarotene Retinoids

 CinacalcetHCl Hyperparathyroidism

 Clarithromycin Macrolide Antibiotic

 Colesevelam Antilipemic

 Donepezil HCl Alzheimer Disease

 Dutasteride Prostatic Hyperplasia

 EletriptanHBr Anti Migraine

 Exemestane Breast Cancer

 Ezetimibe Cardiovascular

 Fexofenadine HCl Anti Allergic

 ImatinibMesylate Anti Neoplastic

 Ivabradine Cardiovascular

 Letrozole Aromatase Inhibitor

 NaratriptanHCl Anti Migraine

 Nateglinide Anti Diabetic

 Nitazoxanide Anti Diarrheal

 Olmesartan Antihypertensive

 Pioglitazone HCl Anti Diabetic

 Pregabalin Anticonvulsant

 QuetiapineFumarate Anti Psychotic

 RaloxifeneHCl Osteoporosis

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 Ranolazine Cardiovascular

 Risedronate Na Osteoporosis

 RopiniroleHCl Parkinson Disease

 Telmisartan Antihypertensive

 Temozolomide Brain Cancer

 Venlafaxine HCl Anti Depressant

ABOUT THE MANUFACTURING FACILITIES

• 1,50,000 sq. ft. covered area

• 5 Dedicated Blocks operating as per US FDA guidelines.
• 132 Stainless Steel and Glass Lined Reaction Vessels with
capacities ranging from 50 to 6000 liters. (Total Volume 245 kilo
liters)
• 3 Automated Fluidized Bed Coaters with capacity of
manufacturing 3 MT of Granules per month.
• Pilot Plant having 7 reaction vessels with capacities ranging from
250 to 1000 liters. (Total Volume 3.63 kilo liters)

PLANT LOCATION

An apt location is the foremost factor that affects the working of any
industry. The plant is located in the Derabassi-Barwala industrial belt. The
various factors that have been considered are:-

1. Man power- Since the location is in an industrial belt so there is cheap

and most importantly experienced labour available.

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2. Raw Material- raw material is made easily available by the state highway
by which the plant is located.

3. Power- Since the plant is located in the industrial belt so power is easily
available from the grid.

4. Water- Almost all the water need is met by the presence of huge
underground water reserve.

5. Transportation- it is again eased by the state highway which passes by

the plant.

Report:
Introduction- the following study was undertaken the SRP, Derabassi Plant
of ISLL. I had a great exposure in presence of personnel in-charge. During
the training I studied the concept of Batch Distillation With Reflux and could
closely see and evaluate the working heat exchangers, and tried to design a
condenser by carrying out basic design calculations on an industrial scale.

Solvent Recovery Plant (SRP)

Solvents Recovered At SRP

1. Dimethylsulfoxide (DMSO)

2. Absolute Alcohol

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3. Methyldichloride (MDC)

4. Toluene

Utilities Used

1. Chilled Water((4-7 ̊C)

2. Water(20-30 C
̊ )

3. Brine(-10 ̊C)

Pre-Requisite Knowledge
1. Definition of a “Solvent”

2. Methods of Solvent Recovery

3. Properties of the Above Solvents

 DMSO  Absolute Alcohol

Appearance- Colorless Appearance- Colorless
Solubility in Water- Miscible Formula C2H5OH
Formula C2H6OS Mol Mass 46.07g mol-1
Mol Mass 78.13 g mol-1 Density 0.789 g cm-3
Density 1.1004 g cm-3 Melting point -114 ̊C
Melting point 19 ̊C Boiling point 78.37 ̊C
Boiling point 189 ̊C

 MDC  Toluene
Appearance- Colorless Appearance- Colorless
Solubility in Water- 13 g/l (20-25 Solubility in Water- 0.47 g/l (20-
C) 25 ̊C)
Formula CH2Cl2 Formula C6H5CH3
Mol Mass 84.93 g mol-1 Mol Mass 92.14 g mol-1
Density 1.33 g cm-3 Density 0.87 g cm-3
Melting point -96.7 ̊C Melting point -95 ̊C
Boiling point 39.6 ̊C Boiling point 110.6 ̊C

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PLANT PRIMA FACIE

The plant has ten rectors (distillation vessels) to its account, with piping
running all over the facility, surrounded by many solvent tanks. Each reactor
has a temperature probe, temperature display both mass and vapour,
pressure indicators, vents, agitation motors, jackets, a Distillation column
rising two floors above the first floor. The piping is accompanied by a
number of valves (mainly gate valves), jacketing for the steam pipes,
rotameters for volumetric reading, and Centrifugal pumps for pumping the
fluids. The reactors stand checked and monitored by the personnel in-
charge at all times. The floor above is occupied by a number of heat
exchangers, all shell and tube type, aimed at condensing the vapour rising
in the distillation column. The heat exchangers are also supplied by utilities
which act as the heat sink for the vapours.

OPERATION EVALUATION

The operation is similar for all the solvents except with little variation, the
main operation carried out at the plant is Distillation, a batch is charged
into a Reactor, and rector is heated by the Steam Jacket. Vapours rise
through Distillation column (Packed Column) above and are cooled in the
Condenser (Heat Exchanger) above, condensate then runs down into
receiver tanks. The operation is guided by the dimension of temperature
and time for the person in-charge. Collection and reflux is set as per the
requirement of stabilization of temperature. The collection being taken is
run down to larger tanks, and is divided into two that is pure form and the
fraction which is defined by the mass or the vapour temperature. In this
way one after the other batches are processed. A strict attention is paid to
the quality, by analysis of samples by the Quality Check Department.

PROCESS BRIEFING

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1. DMSO- DMSO recovery is aimed at minimizing its water content to as

low as 0.4%. DMSO has a high boiling point of 189̊C hence requires a
heavy heat load for distillation, the ‘huge ask’ of heat is reduced by
the application of Vacuum. Recovery of DMSO is a two stage process,
first the feed (mixture of DMSO and Water with little Toluene) is
dehydrated to 1.5%, then finally to 0.4%.

Operation:-

 The feed is charged into 2 rectors, which form the first stage of water
removal.

 Vacuum of nearly 650-700mm, created by Vacuum Ejector System is

applied by opening the vacuum valve.

 Feed is then heated to distillation, and the pure or the first fraction is
collected while maintaining a temperature of about 65̊C (vapour
temperature) by collection and reflux rates.

 A ‘Second fraction’ is then collected upto 95 ̊C vapour temperature

again by maintaining the reflux ratio. The second fraction is charged
with the next batch and serves to ease the Solvent Recovery.

 Sample is then collected for the water content limit of 1.5% and sent
to QC.

 The vacuum is released by introducing nitrogen in the reactor, and

vacuum is applied in the final stage reactor as a result of which the
batch flows into it.

 Steam is then applied to the final stage and DMSO of required purity
is collected, vacuum is again released and the residue is charged into
yet another reactor for final recovery from it.

 Final recovery aims at collection till mass temp of 135 ̊C under

vacuum; the column here used is hollow and serves for the Flash
Distillation.

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 A sample is further taken and sent for final analysis.The reactors are
then washed with water and prepared for the next batch.

2. Absolute Alcohol- unlike the DMSO recovery, the recovery of alcohol

is relatively simple, feed of Clarithromycin ML is simply distilled over
to give alcohol at specific temperature, and the process is carried out
under atmospheric pressure.

Operation:-

 The reactor is checked and is made ready to use, and the feed is
charged into it.

 Steam is applied and distillation starts.

 Heat to reflux to about 79 ̊C

 Start collection at about 78-82 ̊C

 Sampling is then done, finally heating is stopped and residue is

unloaded

 Vessel is washed with absolute alcohol and made ready for the next
batch.

3. MDC- its recovery is a two stage process, with the first stage being
the washing of the crude layer with water and HCl, the washed MDC
settles down the tank having greater density, and is drained out. The
drained out MDC is again charge and distilled over to give MDC
finally.

Operation:-

 In the first stage of the operation a reactor is charged with crude

layer of MDC

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 Then water and HCl are added in specific quantities in order to give
the crude layer a washing to remove the impurities

 The mixture is then stirred for about 30min and then settled for the
same time.

 The mixture then separates into two layers one MDC layer and upper
layer being the aqueous one, aq. Layer is then drained off and MDC
layer is collected into a tank.

 The same MDC layer is then charged into the reactor and again
washed with water and a washed MDC layer is yet again collected
into the tank

 Reactor is washed with water, the reactor is then charged with the
washed MDC as feed

 Reactor is heated to reflux

 The collection range of temperature is about 39-41̊C

 Sampling is done, heating is stopped and residue is unloaded.

4. Toluene- recovery of toluene is done from a mixture of toluene and

MDC, MDC is first recovered, the fraction left is given a washing and
then charged to recover toluene. Toluene is first recovered as a low
boiler with relatively less purity and then as pure fraction at higher
specified temperature.

Operation:-

 The reactor is first charged with a mixture of MDC and toluene

 The mixture is then heated and MDC is recovered upto

temperature of 40̊C

 At about 45̊C mix fraction is obtained

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 This fraction is again charged into the rector, after stopping the
steam and cooling

 The charge is then given a HCl washing, followed with two water
washes

 The heating resumes and low boiler is obtained at about 100̊C and
pure toluene is collected at 110̊C.

HIGHLIGHTS OF THE PROCESSES AT SRP

1. INTRODUCTION to “Batch Distillation With Reflux”

2. Application of vacuum to increase the heat economy of the plant

3. Creation of vacuum with the simplest equipment, i.e. the Ejector

Nozzle

4. Use of second fractions to ease recovery from next batch

5. Use of more than one heat exchanger, hence efficient operation

TROUBLESHOOTING AT SRP
1. Problem- vibration in the collection pump, fall in the pumping rate

Possible Cause- condensate getting too hot, Cavitation.

Solution- increase the reflux, so as too cool the condensate.

2. Problem- very little condensate in the first stage of DMSO

Possible Cause- filling of DMSO in vacuum line

Solution- release the line vacuum, so as to flush out any entrained DMSO

3. Problem- incomplete vacuum

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Possible Cause- ejector fluid getting too heated up

Solution- cool the fluid by draining a part of it in the hold up and fill
cooler fluid

4. Problem- Choking of feed line

Possible Cause- filling of DMSO/MDC/Toluene in the line

Solution- the source valve should be shut off first and then the valve at
the receiver end.

HEAT EXCHANGER DESIGN

Information on manufacturing processes, equipment parameters, materials

of construction, costs and the physical properties of process materials are
needed at all stages of design; from the initial screening of possible
processes, to the plant start-up and production. When a project is largely a
repeat of a previous project, the data and information required for the
design will be available in the Company’s process files, if proper detailed
records are kept. For a new project or process, the design data will have to
be obtained from the literature, or by experiment (research laboratory and
pilot plant), or purchased from other companies. The information on
manufacturing processes available in the general literature can be of use in
the initial stages of process design, for screening potential process; but is
usually mainly descriptive, and too superficial to be of much use for
detailed design and evaluation. The literature on the physical properties of
elements and compounds is extensive, and reliable values for common
materials can usually be found. The principal sources of physical property
data are listed in the references at the end of this chapter. Where values
cannot be found, the data required will have to be measured
experimentally or estimated.

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THE DESIGN PROCESS

PROCEDURE
The general equation for heat transfer across a surface is:

Q=U.A.∆Tlm

Q= Heat transferred per unit time, W

A=Heat transfer area, m2

∆Tlm=The mean temperature difference, the driving force̊C.

U=The overall heat transfer coefficient, W/m2.̊C

Where
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The main motive is to find the area required for heat transfer that is known
by the temperature differences. The design then proceeds by calculating no
of tubes other design parameters resulting in the final design.

The steps in a typical design procedure are as:

• Define the duty: heat transfer rate, fluid flow rates, temperature.

• Collect together the fluid physical properties required: density,

viscosity, thermal conductivity.

• Decide on the type of exchanger to be used.

• Select a trial value for the overall coefficient, U.

• Calculate the mean temperature difference, ∆Tlm.

• Calculate the area required and decide the exchanger layout.

• Calculate the individual coefficients.

• Calculate the overall coefficients and compare with the trial value. If
the trial value differs from the estimated value, substitute the calculated for
the estimated value and return to step vi.

• Calculate the exchanger pressure drop.

• Have a look at the mechanical design and optimize the design.

Design Calculations

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1. To design a condenser to condense vapours of isopropyl alcohol (IPA)

from 81 C̊ to 60 C
̊ . Flow rate of IPA is 2000 kg/hr. Water is used as coolant
with the temp rise from 25 to 34̊C. Composition of solvent IPA is 95% IPA
and 5% water.

Solution:

• Fluid flow rate = 2000kg/hr

Water temperature =25 C

̊ -34̊C IPA temperature = 81 C
̊ -60 C
̊

 PHYSICAL PROPERTIES:

IPA- Water-
Viscosity (μ), 0.262 mN.s/m2 Viscosity (μ), 1 mN.s/m2
Density (ρ), 786 kg/m3 Density (ρ), 996 kg/m3
Heat Capacity (Cp), 2.214KJ/kg C
̊ Heat Capacity (Cp), 4.20 KJ/kg C
̊
Thermal conductivity (k), 0.145 Thermal conductivity (k), 0.59
W/m. C̊ W/m. C̊
Heat of Vaporization, 664.30 Heat of Vaporization, 2260.15
KJ/kg KJ/kg
Molecular weight, 60.00 g mol-1 Molecular weight, 18.00 g mol-1

• TYPE OF HEAT EXCHANGER:

The shell and tube type of heat exchanger is used in the company. As the
coolant is corrosive in nature,so is allowed to pass through tubes. Here we
use one shell and two tubepass.

1. MASS FLOW RATES

Mass flow rate of IPA = 2000*0.95 = 1900 kg/hr.

Mass flow rate of water = 2000*.05 = 100 kg/hr.

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2. HEAT LOAD
Heat load Q (in kW) ={mass flow rate of IPA × ((Cp×∆t) +latent heat of IPA) +
mass flow rate of water×((Cp× ∆t) + latent heat of water)}/3600

={1900 × (2.6 (81 – 60) + 667) + 100 × (4.2 (81 – 60) + 2260.15) /3600
= 389.57 kW

3. WATER FLOW RATE

Mw= 389.57/ (4.2 × (34-25))
Mw= 10.30 kg/s = 37102.51kg/hr

4. LMTD

Temperature of incoming vapours(T1) = 810 C

Temperature of outgoing condensate (T2) = 600C

Temperature of incoming water (t1) = 250C

Temperature of outgoing water (t2) = 350C

LMTD = {(T1 – t2) – (T2 – t1)} / ln {(T1 – t2) / (T2 – t1)}

= {(81 – 34) – (60 – 25)} / ln {(81 – 34) – (60 -25)}

= 40.700 C

R = (T1 – T2) / (t2 – t1)

= (81 – 60) / (34 – 25)

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= 2.333

S = (t2 – t1) / (T1 – t1)

= (34 – 25) / (81 – 25)

= 0.1607

Therefore Ft = 0.97 (from RC VOL. 6 .fig 12.19)

Mean temperature difference:

∆Tm = LMTD * Ft = 40.70 * 0.97

= 39.4790 C

5. TRIAL VALUE OF OVERALL HEAT TRANSFER COEFFICIENT, U:

Let U=900W/m2.̊C (from RC VOL. 6 .fig 12.1)

6. AREA

A = Q / U. ∆Tm = 389570 / 900 × 39.47

A= 11 m2

7. TUBE DIMENSIONS :

Assume outside diameter of tube = 20 mm

Assume inside diameter of tube = 18 mm

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Assume tube length = 4 m

Pt= 1.25 × d0

= 1.25 × 20

= 25 mm

Area of tube = π × d0 × L

= 3.14 × 20 × 10-3× 4

= 0.2513 m2

No. of tubes Nt= Heat transfer area / Area of tube

= 11/ .2513

= 44

8. BUNDLE CALCULATIONS

Db = d0( Nt/ K1 )1/n

Db = Bundle diameter

do = outside diameter of tube

Nt = number of tubes

K1 and N1 are constants. For triangular pitch and two passes

K1 = 0.249, N1 = 2.207 (From RC VOL 6. Table 12.4)

Db = 20 (44/ 0.249)1/2.207
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= 208.57 mm

9. FOR SPLIT RING FLOATING HEAD:

c = 51mm (From RC VOL6. fig 12.10)

Shell diameter = d0 + c

= 208.57 + 51

= 259.57mm

10. NO. OF TUBES IN CENTRAL ROW=Nr = do / Pt= 208.57 /25

=9

11. TO CALCULATE SHELL SIDE COEFFICIENT :

Assume condensing coefficient hc = 1900W/m2 0C

Mean Temperature of Shell side = (81 + 60)/ 2= 70.50 C

Mean Temperature of tube side = (34 + 25) / 2= 29.50C

Now (70.5 – Tw) ×1900 = (70.5 – 29.5) × 900

Tw =51.070C

Mean Temperature of the condensate = (Tw + shell side mean

Temperature/2)

= (51.07+ 70.5) /2

Mean Temperature of condensate = 60.780C

= 333.78 K
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Density of solution = 0.05 × 1000 + 0.95× 786

= 796.7 kg /m3

Average molecular weight of solution = Total weight / Mole of IPA+ Mole of

water

= 2000 / (1900/60) + (100 / 18)

= 53.73 g mol-1

Vapour density at mean Temperature (ρv) = 53.73×273 / 22.4 ×333.78

= 1.96 kg /m3

Γh = Wc /L×Nt

Where Γh = Tube loading, condensate flow per unit length of tube kg / m.s

Wc= total condensate flow kg / s

L = Tube length (m)

Nt = No. of tubes

Γh= 2000 / 4×3600×44

= 3.16× 10-3kg / m.s

Nr = 2/3 × No. of tubes in central row

= 2/3 × 9

Nr = 6

Shell side coefficient:

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= 1943.87 W/m2 0C

Closed to the assumed one 1900 W/m2 0C

12. TO CALCULATE TUBE SIDE COEFFICIENT :

Tube cross section area = /4

= 254.34 mm2

Tube per pass = 44/2

= 22

Tube flow area = Tube per pass × cross sectional area

= 22× 254×10-6

= 5.588× 10 -3 m2

Mass velocity = Cooling water flow / tube flow rate

= 10.30 / 5.588×10-3

= 1843.23 kg/m2s

Water linear velocity ut = 1843.23 / 1000

= 1.84 m/s

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Tube side coefficient

Di is in mm

= 7444.76 W/m2.0C

13. OVERALL COEFFICIENT

Let us assume kw = 50 W/m0C

Fouling factor = 5000 W/m0C, both side.

Uo-1 = 1.09

Uo = 915.50 W/m2 0C

This agrees with the value initially assumed.

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14. TUBE SIDE PRESSURE DROP

Re = ρ ut d/ µ

= 1000× 1.84× 18 ×10-3/ 10-3

= 33120

jf= 3.6×10-3 (RC VOL 6 fig 12.3)

= 24 kPa, acceptable

15. AREA OF CROSS FLOW

Using 2 baffles, lB= 259.57/2= 129.78mm

Area Of Cross Flow = (25 – 20) ×259.57×10-3×129.78×10-3 / 25

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= 6.73×10-3m2

Mass flow rate:

Gs = Mass flow rate / cross sectional area

= 2000 / (3600×6.73×10-3)

= 82.54 kg/ m2 s

Equivalent diameter (de) = 1.10 (Pt2 – 0.917 di2) / d0

= 14.4 mm

Re = Gs*de / µ

= 1188.70

Using baffle cut = 25%

Jf = 0.07 (From RC VOL 6. Fig. 12.30)

Us = Gs /ρ

= 4.12/ 1.96

= 42.11m/s

L/lb = Nb+1 = 2+1 = 3

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∆Ps = 8×0.07(259.57 / 14.4) 3 (1.96 × 42.112 / 2)

= 52625.69 Pa

∆Ps = 52.625kPa (Negligible pressure drop, hence accepted)

PROPOSED DESIGN

• Split Ring Float Head 1 shell 2 tube passes

• 44 carbon steel tubes, 20mm O.D, 18mm I.D, triangular pitch

• Pitch 25mm

• Heat transfer area (based on O.D.) 11m2

• Shell I.D 259.57mm, baffle spacing 129.78mm, 25% cut baffles

Solvent recovery
Solvent refers to substance that has the ability to dissolve a given
compound with a fair specificity.Many plants, such as pharmaceutical,
printing, explosives, electronic and chemical, generate waste solvents that
must be either shipped away for disposal or recovered. There are many
parameters to be addressed to determine the feasibility of solvent
recovery.

The most important parameters are:

o Prices of solvents to be recovered

o Costs of disposal of solvents if not recovered

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o Capital and operating costs of a solvent recovery system

o Achievable purity of recovered solvents

 There are also less tangible benefits to recovery. For example, when the
solvents are recovered, there is no potential liability for solvents shipped
out for disposal. Also, the recovery reduces the vulnerability to
shortages and price increases.

 Many separation techniques can be used for the recovery of the spent
solvent, in order to make the process economic and avoid wastage of
solvent. These processes may be classified depending on the phases
involved, that is; gas-liquid, liquid-liquid and solid-fluid operations. The
various operations used are absorption, distillation, and liquid
extraction, adsorption, drying or leaching. While dealing with liquids
with difference in volatilities, the best method is distillation which gives
products with highest purity.

 Distillation may be carried out batch wise, continuous rectification, flash

or as batch with reflux. For solvent recovery, batch distillation is still the
most common technique used for the purification of solvents. Although
in the process industries, most distillation systems are continuous, batch
systems are preferred for the distillation of relatively small quantities of
solvents. Also, to separate a multi-component mixture of n components
by continuous distillation, a minimum of n-1 separate columns are
required, which involves a significantly higher capital cost.

 The advantage of batch distillation is the added dimension of time,

which allows multiple cuts to be taken from the top of the column. Thus,
the components can be taken off as products in order of their volatility.
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In addition, the process can be stopped at any time to allow for the
addition of a further component for use as an extraction agent. The
main disadvantage of batch distillation is that it essentially has only one
theoretical stripping stage. It is a rectification process. Therefore, this is
an inefficient process when it is required to recover the least volatile
component at high purity.

Distillation
HISTORY

 The first clear evidence of distillation comes from

Greek alchemists working in Alexandria in the first century AD.
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 Distilled water has been known since 200 AD, when

Alexander described the process. Arabs learned the process from the
Egyptians and used it extensively in their chemical experiments.

 Clear evidence of the distillation of alcohol comes from the School of

Salerno in the 12th century. Fractional distillation was developed by
TadeoAlderotti in the 13th century.

 In1500, German alchemist HieronrymusBraunschweig published Liber

de arte destillandi(The Book of the Art of Distillation)the first book
solely dedicated to the subject of distillation, followed in 1512 by a
much expanded version.

 As alchemy evolved into the science of chemistry, vessels

called retorts became used for distillations. Later, copper alembics
were invented. These were called pot stills. Today, the retorts and
pot stills have been largely supplanted by more efficient distillation
methods in most industrial processes.

 In the early 19th century the basics of modern techniques including

pre-heating and reflux were developed, particularly by the
French,and then in 1830 a British Patent was issued to Aeneas
Coffey for a whiskey distillation column, which worked continuously
and may be regarded as the archetype of modern petrochemical
units.

 In 1877, Ernest Solvay was granted a U.S. Patent for a tray column
for ammonia distillation and the same and subsequent years saw
developments of this theme for oil and spirits.

With the emergence of chemical engineering as a discipline at the end of

the 19th century, scientific rather than empirical methods could be applied.
The developing petroleum industry in the early 20th century provided the
impetus for the development of accurate design methods such as
the McCabe-Thiele method and the Fenske equation.

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BASIC PRINCIPLES OF DISTILLATION

Separation of components from a liquid mixture via distillation depends on
the differences in boiling points of the individual components. Also,
depending on the concentrations of the components present, the liquid
mixture will have different boiling point characteristics. Therefore,
distillation processes depends on the vapour pressure characteristics of
liquid mixtures.

The vapour pressure of a liquid at a particular temperature is

the equilibrium pressure exerted by molecules leaving and entering the
liquid surface. Here are some important points regarding vapour pressure:

1. energy input raises vapour pressure

2. vapour pressure is related to boiling

3. a liquid is said to ‘boil’ when its vapour pressure equals the

surrounding pressure

4. the ease with which a liquid boils depends on its volatility

5. liquids with high vapour pressures (volatile liquids) will boil at lower
temperatures

6. thevapour pressure and hence the boiling point of a liquid mixture

depends on the relative amounts of the components in the mixture

7. distillation occurs because of the differences in the volatility of the

components in the liquid mixture

The distillation equipment to achieve the desired aims will generally consist
of:
• heating system to evaporate the solvent;
• Condensers and coolers;
• fractionating column
• Storage both as part of the plant as a still kettle and to hold residue,
products and feed.
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APPLICATIONS
 Distillation is among the most important and widely used industrial
operations today. About 95 percent of all separation processes today
are carried out in industry with more than 40,000 distillation systems.
For example, a petroleum refining plant is usually distinguished by a
group of distilling towers that rise more than 100 feet (30 meters)
into the air. The principle on which such towers operate, though, is
no different from the one described above.

 In petroleum refineries, crude oil is heated at the bottom of the

refining tower. The hundreds of compounds that make up crude oil
each boil off at their own characteristic boiling point. They rise in the
refining tower, are cooled, and condense to liquids. Collectors at
various heights in the tower are used to draw off those liquids into
various fractions known by designations such as gasoline, diesel oil,
heating oil, and lubricating oil.

 In countless processes in the food industry, products are isolated and

recovered from solvents by means of precipitation or extraction.
When recovering these solvents, it is important that the product is
treated carefully, that the redistilled materials are sufficiently clean
and that energy is used effectively.

Typical distillation examples are:

o manufacture of pectin by precipitation with alcohol
o production of hop extract
o production of egg lecithin

DISTILLATION FURTHER HAS FOLLOWING TYPES

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 VACUUM DISTILLATION
Vacuum distillation is a method of distillation whereby the pressure above
the liquid mixture to be distilled is reduced to less than its vapour
pressure (usually less than atmospheric) causing evaporation of the
most volatile liquid(s) (those with the lowest boiling points). This distillation
method works on the principle that boiling occurs when the vapour
pressure of a liquid exceeds the ambient pressure. Vacuum distillation is
used with or without heating the mixture.
Vacuum distillation increases the relative volatility of the key components
in many applications. The higher the relative volatility, the more separable
are the two components; this connotes fewer stages in a distillation
column in order to effect the same separation between the overhead and
bottoms products. Lower pressures increase relative volatilities in most
systems.
A second advantage of vacuum distillation is the reduced temperature
requirement at lower pressures. For many systems, the products degrade
or polymerize at elevated temperatures.
Vacuum distillation can improve a separation by:
 Prevention of product degradation or polymer formation because of
reduced pressure leading to lower tower bottoms temperatures,
 Reduction of product degradation or polymer formation because of
reduced mean residence time especially in columns
using packing rather than trays.
 Increasing capacity, yield, and purity.
Another advantage of vacuum distillation is the reduced capital cost, at the
expense of slightly more operating cost. Utilizing vacuum distillation can
reduce the height and diameter, and thus the capital cost of a distillation
column.
 AZEOTROPIC DISTILLATION
Azeotropic distillation is a widely practiced process for the dehydration of a
wide range of materials including acetic acid, chloroform, ethanol, and
many higher alcohols. The technique involves separating close boiling
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components by adding a third component, called an entrainer, to form a

minimum boiling, normally ternary azeotrope which carries the water
overhead and leaves dry product in the bottom. The overhead is
condensed to two liquid phases; the organic, "entrainer rich" phase being
refluxed while the aqueous phase is decanted. Given the non-idealities, the
phase splitting, the distillation boundaries present, and the possible
existence of multiple steady states in such a system, columns like these can
be extremely difficult to simulate and to operate.

 EXTRACTIVE DISTILLATION
Extractive distillation is a vapour-liquid process operation that uses a third
component, or solvent, to effect a chemical separation. The extractive
agent creates or enhances the volatility difference between the
components to be separated. The extractive agent and the less volatile
component flow to the bottom of the distillation column, where the
extracted component is recovered by a subsequent distillation. The non-
extracted species are distilled to the top of the extractive distillation tower.

 CONTINUOUS DISTILLATION
The most common form of distillation used by the chemical, petroleum and
petrochemical industries is the continuous mode system. In continuous
distillation, feed constantly is charged to the column at a point between the
top and bottom sections. The section above the feed point rectifies or
purifies the more volatile component while the column section below the
feed point strips out the more volatile from the less volatile component. In
order to separate N components with continuous distillation, a minimum of
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N-1 distillation columns is required. Sidedraws can be taken to remove

extra streams from the column but only when high purity of individual
components is not required.

Continuous Distillation Tower

 FLASH DISTILLATION
Flash distillation is the simplest method of separation.A feed stream is
“flashed” into a chamber or “flash drum” and the liquid and vapour are
allowed to separate under equilibrium.It is “flashed” by throttling the feed
stream through a nozzle or valve into the chamber – the pressure drops
through the valve. The more volatile component will be concentrated in the
vapour stream – the less volatile in the liquid stream.The system is very
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close to a single “equilibrium stage”.Separation is usually not very high for a

single equilibrium stage.

 BATCH DISTILLATION WITH REFLUX

Batch distillation with only a simple still does not give a good separation
unless the relative volatility is very high. In many cases, a rectifying column
with reflux is used to improve the performance of the batch still. If the
column is not too large, it may be mounted on top of the still or it may be
supported independently, with connecting pipes for vapour and liquid
streams. The system may be operated to keep the top composition
constant by increasing the reflux ratio as the composition of the liquid in
reboiler changes.

Equipments Used

 REACTORS

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The Batch reactor is the generic term for a type of vessel widely used in the
process industries. Its name is something of a misnomer since vessels of this
type are used for a variety of process operations such as solids
dissolution, product mixing, batch distillation, crystallization, liquid/liquid
extraction, chemical reactions and polymerization. In some cases, they are
not referred to as reactors but have a name which reflects the role they
perform (such as crystallizer, or bio reactor).
A typical batch reactor consists of a tank with an agitator and integral
heating/cooling system. These vessels may vary in size from less than 1 l to
more than 15,000 l. They are usually fabricated in steel, stainless steel, glass
lined steel, glass or exotic alloy. Liquids and solids are usually charged via
connections in the top cover of the reactor. Vapours and gases also
discharge through connections in the top. Liquids are usually discharged out
of the bottom.
The advantages of the batch reactor lie with its versatility. A single vessel
can carry out a sequence of different operations without the need to break
containment. This is particularly useful when processing toxic or
highly potent compounds.

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 Agitation
The usual agitator arrangement is a centrally mounted driveshaft with an
overhead drive unit. Impeller blades are mounted on the shaft. A wide
variety of blade designs are used and typically the blades cover about two
thirds of the diameter of the reactor. Where viscous products are
handled, anchor shaped paddles are often used which have a close
clearance between the blade and the vessel walls.
Most batch reactors also use baffles. These are stationary blades which
break up flow caused by the rotating agitator. These may be fixed to the
vessel cover or mounted on the interior of the side walls.
Despite significant improvements in agitator blade and baffle design, mixing
in large batch reactors is ultimately constrained by the amount
of energy that can be applied. On large vessels, mixing energies of more
than 5 Watts per l can put an unacceptable burden on the cooling system.
High agitator loads can also create shaft stability problems. Where mixing is
a critical parameter, the batch reactor is not the ideal solution. Much higher
mixing rates can be achieved by using smaller flowing systems with high
speed agitators,ultrasonic mixing or static mixers.

 Heating/Cooling Systems
Products within batch reactors usually liberate or absorb heat during
processing. Even the action of stirring stored liquids generates heat. In
order to hold the reactor contents at the desired temperature, heat has to
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be added or removed by a cooling jacket or cooling pipe. Heating/cooling

coils or external jackets are used for heating and cooling batch reactors.
Heat transfer fluid passes through the jacket or coils to add or remove heat.
Within the chemical and pharmaceutical industries, external cooling jackets
are generally preferred as they make the vessel easier to clean. The
performance of these jackets can be defined by 3 parameters:

 Response time to modify the jacket temperature

 Uniformity of jacket temperature
 Stability of jacket temperature
It can be argued that heat transfer coefficient is also an important
parameter. It has to be recognized however that large batch reactors with
external cooling jackets have severe heat transfer constraints by virtue of
design. It is difficult to achieve better than 100 W/l even with ideal heat
transfer conditions. By contrast, continuous reactors can deliver cooling
capacities in excess of 10,000 W/l. For processes with very high heat loads,
there are better solutions than batch reactors.
Fast temperature control response and uniform jacket heating and cooling
is particularly important for crystallization processes or operations where
the product or process is very temperature sensitive.

 Single external jacket

The single jacket design consists of an outer jacket which surrounds the
vessel. Heat transfer fluid flows around the jacket and is injected at
high velocity via nozzles. The temperature in the jacket is regulated to
control heating or cooling.
The single jacket is probably the oldest design of external cooling jacket.
Despite being a tried and tested solution, it has some limitations. On large
vessels, it can take many minutes to adjust the temperature of the fluid in
the cooling jacket. This results in sluggish temperature control. The
distribution of heat transfer fluid is also far from ideal and the heating or
cooling tends to vary between the side walls and bottom dish. Another
issue to consider is the inlet temperature of the heat transfer fluid which
can oscillate (in response to the temperature control valve) over a wide
temperature range to cause hot or cold spots at the jacket inlet points
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 EJECTORS FOR VACUUM CREATION

Steam jet Ejectors are based on the ejector-venturi principal and operate by
passing motive steam through an expanding nozzle. The nozzle provides
controlled expansion of the motive steam to convert pressure in to velocity
which creates a vacuum with in the body chamber to draw in and entrain
gases or vapours. The motive steam and suction gas are then completely
mixed and then passed through the diffuser or tail, where the gases velocity
is converted in to sufficient pressure to meet the predetermined discharge
pressure.
Vacuum Ejectors are used in a variety of applications in the process, food,
steel and petrochemical industries. Typical duties involve filtration,
distillation, absorption, mixing, vacuum packaging, freeze drying,
dehydrating and degassing. Ejectors will handle both condensable and none
condensable gas loads as well as small amounts of solids or liquids, however
accidental entrainment of liquids can cause a momentary interruption in
vacuum but this will not cause damage to the ejector.
Primary advantages over other vacuum pumps can be seen below:
 No Moving Parts - Ejectors are exceedingly simple and reliable. There
are no moving parts to wear or break in a basic ejector.
 Low Cost - Units are small in relation to the work they do and cost is
correspondingly low.
 Versatile - Various piping arrangements permit adapting to
environmental conditions.
 Self Priming - Ejectors are self-priming. They operate equally well in
continuous or intermittent service.
 Easy to Install - Relatively light in weight, ejectors are easy to install,
and require no foundations. Even multi stage units are readily
adaptable to existing conditions.
 Corrosion and Erosion Resistant - Because they can be made of
practically any workable material, or coated with corrosion-resistant
materials, ejectors can be made highly resistant erosion and
corrosion.
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 High Vacuum Performance - Ejectors can handle air or other gases at

suction pressures

 DISTILLATION COLUMNS

 Tray Columns
While there are perhaps five basic distillation trays suitable for
industrialuse, there are many design variations of differing degrees of
importanceand a confusing array of trade names applied to their products
by traymanufacturers. The most modern and commonly used devices
include sieve,valve, bubble cap, dual flow, and baffle trays — each with its
advantages andpreferred usage. Of these, the sieve and valve type trays
currently are mostoften specified.For a better understanding of tray design,
following figure defines and locatestypical tray components.

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The material of construction usually is 14 gaugewith modern trays adopting

the integral truss design which simplifiesfabrication. A typical truss tray is
shown in Fig (i). For columns less than3 ft. (0.9m) in diameter, it is not
possible to assemble the truss trays in thecolumn; therefore, trays must be
pre-assembled on rods into a cartridgesection for loading into the column.
Fig (ii) shows this arrangement in scalemodel size.
The hydraulic design of a tray is a very important factor. The upper
operatinglimit generally is governed by the flood point, although in some
cases,entrainment also can restrict performance before the onset of
flooding.Flooding is usually caused by either massive entrainment, termed
jet flooding,or by downcomerback-up. Downcomer back-up occurs when a
tray designprovides insufficient downcomer area to allow for the liquid flow
or when thepressure drop across the tray is high, which forces liquid to
back up in thedowncomer. When the downcomer is unable to handle all the
liquid involved,the trays start to fill and pressure drop across the column
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increases. Thisalso can occur when a highly foaming liquid is involved.

Flooding associatedwith high tray pressure drops and small tray spacing
takes place when therequired liquid seal is higher than the tray spacing.
Downcomer design alsois particularly important at high operating pressure
due to a reduction in thedifference between vapour and liquid densities.
The lower limit of tray operation, meanwhile, is influenced by the amountof
liquid weeping from one tray to the next. Unlike the upward force
ofentrainment, weeping liquid flows in the normal direction and
considerableamounts can be tolerated before column efficiency is
significantly affected.As the vapour rate decreases, however, a point
eventually is reached when allthe liquid is weeping and there is no liquid
seal on the tray. This is known asthe dump point, below which there is a
severe drop in efficiency.
Various Trays Used Are
o Sieve Tray
o Dual Flow Tray
o Valve Tray

o Bubble Cap Tray

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o Baffle Tray

 PACKED COLUMNS

A packed distillation column allows for continuous contact of liquid and

vapour, however it is convenient to analyze the column as if it were
discontinuous (a staged tower). The packing in the column can be divided
up into segments that are of equal height.
 Each of these segments can be looked at as a “stage”. It can be
assumed that each stage allows the vapour and liquid to leave the stage
in equilibrium with each other. This method of assuming that the
packing can be broken down into stages is not physically accurate, but
can be used for calculations.
 Height equivalent to a theoretical plate (HETP), HETP is defined as the
height of packing needed to obtain the change in composition obtained
with one theoretical contact. HETP is measured experimentally and
usually can range from one to four feet. A small HETP indicates a small
column and more efficient packing.
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 To measure the HETP, the compositions of the top and bottoms streams
must be found at total reflux and the number of equilibrium stages
must be calculated.
For many types of duties, particularly those involving small diameter
columns,packing is the most economical tower internal. One advantage is
that mostpacking can be purchased from stock on a volumetric basis. In
addition,the mechanical design and fabrication of a packed column is quite
simple.Disadvantages of packing include its unsuitability for fouling duties,
breakageof ceramic packing, less predictive performance,particularly at
low liquid loads or high column diameters.
The most widely used packing is the random packing, usually RashigRings,
Pall Rings and ceramic saddles. These are available in variousplastics, a
number of different metals and, with the exception of Pall Rings,in ceramic
materials. While packings in plastic have the advantage ofcorrosion
resistance, the self-wetting ability of some plastic packing such
asfluorocarbon polymers sometimes is poor, particularly in aqueous
systems.This considerably increases the HETP when compared with
equivalentceramic rings.

 HEAT EXCHANGER- CONDENSERS

The basic concept of a heat exchanger is based on the premise that the loss
of heat on the high temperature side is exactly the same as the heat gained
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in the low temperature side after the heat and mass flows through the heat
exchanger. Heat exchanger ‘simply’ exchanges the heat between those two
sides; as a result, it is decreasing the temperature of higher temperature
side and increasing the temperature of lower temperature side. But
designing heat exchanger might be a challenge; it needs iteration for
manual calculation. Many factors have to be considered in heat exchanger
selection. Generally, suitability of types of heat exchanger to be used in
processing industrials is selected based on TEMA (Tubular Exchanger
Manufacturers Association) Standards. TEMA divides heat exchanger into
classes based on their application. Selection might be done by referred to
some valid standards or guideline, but understanding the basic concept and
theory behind heat exchanger is also important.
Furthermore, basic theories about heat transfer are also extremely needed
to do heat exchanger sizing. Selection and sizing are related each other;
changing in heat exchanger component, such as tube pattern and baffle,
would affect the calculation. Some required data is commonly pictured in a
graph or listed in a table.
SHELL AND TUBE HEAT EXCHANGER

 It is the most common type of heat exchanger in oil refineries and other
large chemical processes, and is suited for higher-pressure applications.
 It consists of a tube bundle enclosed in a cylindrical casing called a shell.

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 One fluid runs through the tubes, and another fluid flows over the
tubes (through the shell) to transfer heat between the two fluids.
 Two fluids, of different starting temperatures, flow through the heat
exchanger. One flows through the tubes (the tube side) and the other
flows outside the tubes but inside the shell (the shell side).
 Heat is transferred from one fluid to the other through the tube walls,
either from tube side to shell side or vice versa.
 The fluids can be either liquids or gases on either the shell or the tube
side. In order to transfer heat efficiently, a large heat transfer area
should be used, so there are many tubes. In this way, waste heat can be
put to use. This is a great way to conserve energy.
 Typically, the ends of each tube are connected to plenums through
holes in tube sheets. The tubes may be straight or bent in the shape of a
U, called U-tubes.
 Most shell-and-tube heat exchangers are either1, 2, or 4 pass designs
on the tube side. This refers to the number of times the fluid in the
tubes passes through the fluid in the shell. In a single pass heat
exchanger, the fluid goes in one end of each tube and out the other.
 There are often baffles directing flow through the shell side so the fluid
does not take a short cut through the shell side leaving ineffective low
flow volumes.
Since most distillation column condensers are of shell and tube design, the
processor has the option of condensing on either the shell or tube side.
From the process point of view, condensation on the shell side is preferred
since there is less subcooling of condensate and a lower pressure drop is
required. These are important factors in vacuum duties. Furthermore, with
cooling water on the shell side, any fouling can be removed more easily.
Tube side condensation, on the other hand, can be more advantageous
whenever process fluid characteristics dictate the use of more expensive,
exotic materials. Capital cost of the unit can be reduced by using a carbon
steel shell.

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 CENTRIFUGAL PUMP
Centrifugal pumps are used to transport liquids/fluids by the conversion of
the rotational kinetic energy to the hydro dynamics energy of the liquid
flow. The rotational energy typically comes from an electric motor or
turbine. In the typical simple case, the fluid enters the pump impeller along
or near to the rotating axis and is accelerated by the impeller, flowing
radially outward into a diffuser orvolute chamber (casing), from where it
exits.
Common uses include water, sewage, petroleum and petrochemicals. The
centrifugal pump's relative with opposite function is the water turbine that
uses the potential energy of water converts to mechanic energy.

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REFERENCES

1. SINNOT, R.K. Chemical Engineering Design, Richardson and Coulson’s

Chemical Engineeing, Vol.6, 4th Edition.

2. PERRY, ROBERT.H. Perry’s Chemical Engineers’ Handbook, 7th Edition(McGraw-Hill).

3. Wikipedia

4. Plant Manuals

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