Appendix-A

CHAPTER-1

INTRODUCTION
1.1 HISTORY
Acetaldehyde, CH3CHO, was first prepared by Scheele in 1774, by
the action of manganese dioxide and sulfuric acid on ethanol. The structure
of acetaldehyde was established by Liebig in 1835 when he prepared a pure
sample by oxidizing the ethanol with chromic acid. Liebig named the
compound aldehyde from the Latin words translated as al (cohal) dehyde
(rogenated). The formation of acetal dehyde by the addition of water to
acetylene was observed by Kutscherow in l881.

Acetaldehyde was first prepared from ethyl alcohol by Davy (l8l7)

who employed a platinum black catalyst and passed a mixture of alcohol and
air over it at a lower temperature. More thorough studies of the air oxidation
of ethanol, employing various catalyses, were made by Kuhlman in 1839,
Strecker (1855) and Grimax (1886). Not until the work of Trillatt (l902) and
Orloff (1901), however, were any quantitative data reported. More recently
faith and keyes (1931) carried out extensive investigation of this reaction
and found that the silver gauze was the best catalyst. Employing a flow rate
of 0.57 liter of » alcohol vapors per minute over a heated silver gauze, 12
mm. in dia and 15 mm. long, maintaining a temp. fiarly constant at 515°C,

1
 Appendix-A

they observed 80.6% conversion of ethanol to acetaldehyda with losses of

13.3% to CO2 and 3.2 to acetic acid.

Shreve (1945) and Faith, Keyes, Clark (1950) report slightly higher
yields of 85 to 95% by the air oxidation of ethanol to acetaldehyde by use of
silver catalyst at a temp. of 550 – 570oC and a conversion per pass of 50 to
55%.

However, Groggins (1947) reporting results from a similar process

claims only 70-80% of the theoretical yield of acetaldehyde under identical
conditions.

The production pattern for acetaldehyde has undergone two

significant changes since 1940. At that time, principal industrial routs to
acetaldehyde were hydration of acetylene and oxidation of ethyl alcohol.
However, increasing acetylene costs made this feed stock economically
unattractive and the industry turned to the oxidation of ethanol. The
production of acetaldehyde based on ethanol increased from 63.5 kilotons
per years in 1940 to 403 kilo tons per years in 1960.

In 1960, the two aldehyde Wacker-Hoechst G.m.b.H. processes for the

liquid phase oxidation of ethylene to acetaldehyde began commercial
operation. By 1963, more acetaldehyde was produced by the direct oxidation
of ethylene using the Wacker process than from ethanol, and since then,
production via the Wacker process has increased while production from
ethanol has declined.

2
 Appendix-A

1.2 PHYSICAL PROPERTIES

Acetaldehyde is a colorless, mobile liquid having a pungent

suffocating odor that is somewhat fruity and pleasant in dilute
concentrations. Some physical properties of acetaldehyde are given in
Table(1.1), the vapour pressure of acetaldehyde and its aqueous solutions in
Table(1.2 & 1.3) and the solubility of acetylene, CO 2 and N2 in liquid
acetaldehyde in Table(1.4). The freezing points of aqueous solutions of
acetaldehyde are as follows:

4.8 wt.% - 2.5 oC; 13.5 wt.% - 7.8 oC; & 31.0 wt.% - 23.0 oC

Acetaldehyde is miscible in all proportions with water and most common

organic solvents; acetone, benzene, ethyl alcohol, ethyl ether, gasoline,
paraldehyde, toluene, xylene, tarpeiitine and acetic acid.

Table-1.1: Physical Properties of Acetaldehyde

Formula weight 44.052

Melting point, °C -123.5
Boiling point at 760 mm, °C 20.16
Density, d2o4 0.7730
Vapor density (air = 1) 1.52
Surface tension at 20oC, dyne/cm 21.2
Absolute viscosity at 15oC ( cgs units) 0.02456
Specific heat, cal/(oC)(g) at 0oC 0.522
at 25°C 0.336

3
 Appendix-A

Latent heat of fusion, cal/g 17.6

Latent heat of vaporization, cal/g 139.5
Heat of combustion of liquid at constt.pr. Kcal/mol 279.2
Heat of formation at 273 oK 39.55
Free energy of formation at 273 oK, Kcal/mole -32.60
Critical temp, C 181 .5
Critical pressure, atm. 63.2
Dissociation constant, Ka, at 0 oC 0.7  10-14
Flash point, closed cup, °C -38
Ignition temp. in air, oC 165
Explosive limits of mixtures with air, % acetaldehyde by vol. 4-57

Table-1.2: Vapor Pressure of Acetaldehyde

Vapor Pressure Vapor pressure

Temperature oC Temperature oC
mm Hg mm Hg
-50 19 20 755
-20 123 20.16 760
0 330 30 1069
5 411 50 3096
10 508 70 3696
15 622 100 3607

Table-1.3: Vapor Pressure of Aqueous solutions of Acetaldehyde

Vapor Pressure Vapor pressure

Temperature oC Temperature oC
mm Hg mm Hg
10 4.9 4.9 74.5
10 10.5 10.5 139.8

4
 Appendix-A

20 5.4 5.4 125.2

20 12.9 12.9 295.2
Table-1.4: Solubility of Gases in Liquid Acetaldehyde at 760 mm
(volume of gas [NTP] dissolved in one volume of acetaldehyde)

Temperature oC Acetylene Carbon Dioxide Nitrogen

-6 27 11
0 17 6.6
12 7.3 2.45
0.15
16 5 1.5

1.3 USES

About 95% of the acetaldehyde produced is used internally by the

manufacturers as an intermediate for the production of other organic
chemicals. Figure (1.1) illustrates the significant variety of organic products
(and their end uses) derived from acetaldehyde. Table(1.5), gives an idea of
the use pattern. Imports and exports of acetaldehyde are negligible.

Acetic acid and anhydride are the major derivatives of acetaldehyde

(45% in 1970) followed by n-butanol (19%) and 2-ethylhexanol (17%).
Twenty percent of the acetaldehyde is consumed in a variety of other
products, the most important being pentaerythritol, trimethylolpropane,
pyridines, peracetic acid, crotonaldehyde, chloral, 1,3-butylene glycol, and
lactic acid. The proportion of acetaldehyde used in the manufacture of acetic
acid and acetic anhydride will tend to increase in the near future, and the
proportion used in the synthesis of n-butanol and 2-ethylhexanol will

5
 Appendix-A

decrease. Acetaldehyde is competing with propylene and -olefins as the

raw material for the production of n-butanol and higher alcohols (oxo route).

6
 Appendix-A

Fig-1.1: Acetaldehyde derivatives and uses

Table-1.5 Acetaldehyde, United States Uses in 1970

Acetic acid and anhydride 45 %

n-Butanol 19%
2-Ethylhexanol 17%
AH others 19%

The future growth of acetaldehyde will be mainly dictated by the

acetic acid and anhydride picture and the growth of the other minor
derivatives mentioned above.

1.4 FUTURE TRENDS

In the next decade the major change that will occur in the
acetaldehyde picture is a decrease in the use of acetaldehyde for the
preparation of derivatives that can be manufactured from alternative raw
materials. This has already happened in the production of butanol and 2-
ethylhexanol in which acetaldehyde raw material has been replaced by
propylene and synthesis gas in oxo-type processes. Acetic acid and
anhydride are the major outlets for acetaldehyde. Production of these
chemicals from alternative processes (like methanol carbonylation or
saturated hydrocarbon oxidation would also have an adverse effect on
acetaldehyde consumption in the future. Here again, the energy crisis could
accelerate the expansion of some of these processes that are competing with
acetaldehyde by-making synthesis gas and carbon monoxide available

7
 Appendix-A

through coal gasification. Long range, carbon monoxide and hydrogen could
become the new building blocks of the organic chemical industry.
1.5 HANDLING

In handling acetaldehyde, one has to remember that it is an extremely

reactive compound that can be easily oxidized, reduced, or polymerized, and
is highly reactive with oxygen. It has to be treated as a volatile, flammable,
and toxic material. The following is a list of precautions recommended when
handling acetaldehyde: (1) nitrogen or other inert gases should be used as a
blanketing material whenever exposure to air is a possibility; (2) safety
goggles should be used; (3) transfers should be made in open-air structures
or using suitable gas mask or self-contained breathing equipment .if
necessary; (4) drums should be stored out-of-doors, avoiding direct exposure
to sunlight; and (5) acetaldehyde should be-chilled before transferring and a
nitrogen blanket should be used.

1.6 SHIPPING AND STORAGE

Acetaldehyde is shipped in 5-, 10-, or 55-gal drums, insulated tank

trucks, and insulated tank cars. Acetaldehyde in, the liquid state is non-
corrosive to most metals, but it can be easily oxidized to acetic acid.
especially in the vapor stage. Suitable materials of construction .are stainless
steel and aluminum. Drums coated with phenolic resins have also been used.
If a darker color and some iron contamination are not objectionable, carbon
steel may be used. Because acetaldehyde is classed as a flammable liquid, it
requires a red DOT (Department of Transportation) shipping table.

8
 Appendix-A

Bulk storage held at low temperature and pressure is recommended

over storage in a pressure vessel.

CHAPTER-2

MANUFACTURING
PROCESSES
The economics of the various processes for the manufacture of acetaldehyde
are strongly dependent on the price of the feed stock used. Since 1960 the
liquid phase oxidation of ethylene has been the process of choice. However,
there is still commercial production by the partial oxidation of ethyl alcohol
and the hydration of acetylene.

Acetaldehyde is also formed as a co-product in the high temperature

oxidation of butane. A recently developed rhodium catalyzed process
produces acetaldehyde from synthesis gas as a co-product with ethyl alcohol
and acetic acid.

2.1 HYDRATION OF ACETYLENE

In this process high pricing acetylene is fed with steam to a rubber

lined vertical reactor which contains a catalyst solution of mercury salt (0.5
to 1 wt.%) sulfuric acid (15 to 20 wt.%) ferrous and ferric iron (2 to 4 wt/%)
and water. Minute particles of free mercury are suspended in the catalyst

9
 Appendix-A

solution. The temperature and pressure are controlled at 90 to 95 oC and 1 to

2 atm, respectively. The acetylene conversion per pass is about 55%.

2.2 ETHYLENE OXIDATION PROCESS

The process is essentially based on three chemical reactions.

C2H4 + 2CuCl2 + H2O CH3CHO + Pdo + 2HCl

Pdo + 2CuCl2 PdCl2 + 2CuCl (Pd oxidation)
2CuCl + 2HCl + 1/2O2 2CuCl2 + H2O (CuCl oxidation)
C2H4 + ½O2 CH3CHO (Overall reaction)

In this process, the palladium chloride is required only in very small

concentration, and the copper salts are continuously regenerated with
oxygen. In this way direct oxidation of ethylene take place.

In this process fresh oxygen and ethylene are fed independently to a

vertical ceramic lined reactor containing a water solution of catalyst (PdCl 2
and CuCl2). The reactor is operated to 120 to 130 oC and about 3 atm. The
heat of vaporization is removed by evaporating acetaldehyde and water from
the catalyst solution. The ethylene conversion per pass is 75%.

2.3 OXIDATION OF SATURATED HYDROCARBONS

Acetaldehyde is formed as a co-product in the vapor-phase oxidation

of saturated hydrocarbon such as butane oxidation of butane yields
acetaldehyde, formaldehyde, methanol acetone and mixed solvents as major
products, other aldehydes, alcohols, ketones, glycols acetals, epoxides and

10
 Appendix-A

organic acids are formed in smaller concentrations. This is of historic

interest unlike the acetylene rout, it has almost no chance to be used as a
major process.

2.4 SYNTHESIS GAS PROCESS

A rhodium catalyzed process capable by converting synthesis gas

directly into acetaldehyde in a single step was reported in 1974.

CO + H2 CH3CHO + other products

The process comprises synthesis gas over 5% rhodium on SiO 2 at 300

o
C and 2.0 Mpa (20 atm). The principle co products are acetaldehyde 24%
are acetaldehyde 24% acetic acid 20%, and ethanol 16%. If there is a
substantial degree of coal gasification, the interest in the use of synthesis gas
as a raw material for acetaldehyde production will increase.

2.5 ETHYL ALCOHOL PROCESSES

There are two commercial processes for the production of

acetaldehyde from ethyl alcohol. These are vapor phase oxidation of ethanol.

Ag
CH3CHCH2OH + ½ O2 CH3CHO + H2O
o
550 C

In this process a mixture of ethyl alcohol vapors and oxygen are passed over
silver catalyst filled in tubes of multi-tubular fixed bed reactor. The reaction
is carried out at 550 oC and conversion of ethyl alcohol to acetaldehyde is
50-55% per pass.

11
 Appendix-A

The second process is vapor phase dehydrogenation of ethanol.

Cr and Cu
C2H5OH CH3CHO + H2
o
260 to 290 C

In this process vapors of ethanol are reacted over a chromium copper

catalyst at atmospheric pressure and 260 to 290 oC temperature. The alcohol
conversion is 30 to 50% depending upon reaction temperature and alcohol
flow rate.

Out of these processes we have selected “Ethyl Alcohol Oxidation

Process”. Process description is given below.

2.6 PROCESS DESCRIPTION

Fresh ethyl alcohol (95 %) is mixed with recycled stream from

distillation column D-2 and then this stream is mixed with recycled stream
from separator S-1. The combined stream is pumped to vaporizer v-1 where
80% ethyl alcohol is vaporized and then this vapor liquid mixture is
separated in separator S-1. Liquid is recycled back to the pump suction and
vapors are fed to heat exchanger E-2 where alcohol vapors are superheated
by product gases coming from reactor R-1. Now alcohol vapors are further
heated up to 550 oC in heat exchanger E-4 by steam.

Air is taken from atmosphere and is compressed by compressor C-1

and is fed to heat exchanger E-1, where air is preheated by product gases
coming from reactor R-1. Air is further heated to 550 oC in heat exchanger
E-3, by steam. Alcohol vapors coming from heat exchanger E-4 and

12
 Appendix-A

preheated air coming from heat exchanger E-3, are mixed together and are
fed to reactor R-1. The reactor R-1 is a catalytic reactor. It is multi tube,
fixed bed reactor. Silver catalyst is filled in tubes and cooling water is
flowing on the shell side in order to remove heat of reaction because
oxidation of ethyl alcohol is an exothermic reaction. Reaction temperature is
550 oC.

Reaction product comprised of acetaldehyde, water, ethyl alcohol,

oxygen and nitrogen. These are at 550 oC, so in order to recover heat from
theses product gases, these are fed to heat exchanger E-1 where air is heated
by these gases. Further heat is recovered from these gases in heat exchanger
E-2, where ethyl alcohol vapors are heated by these product gases. The gases
are still at high temperature, when they exit from heat exchanger E-2. So
these are cooled to 30 oC in heat exchanger E-5 by water. This cooled
mixture of ethyl alcohol, acetaldehyde, water, oxygen and nitrogen are fed to
absorption column A-1 where most of the ethyl alcohol and acetaldehyde is
absorbed. Exit gases from absorber A-1 are further scrubbed by cold water in
second absorber A-2 where remaining ethyl alcohol and acetaldehyde are
absorbed and oxygen nitrogen and traces of acetaldehyde and ethyl alcohol
are vent to atmosphere. Liquid from absorber A-2 acts as solvent for
absorber A-1. Liquid from absorber A-1 is pumped by pump P-2 to
pre-heater E-6, where the feed to distillation column D-1 is preheated up to
its bubble point. The feed consists of acetaldehyde, ethyl alcohol and water.
From the top of the distillation column D-1, acetaldehyde (99%) is obtained.
The bottom product from distillation column D-1 consists of ethyl alcohol
and water which are fed to second distillation column D-2 which alcohol
recovery column. The top product (95% ethanol) is recycled back to the

13
 Appendix-A

suction of pump P-1 and product from second distillation as column D-2
containing 1% ethyl alcohol and 99% water are send to biological waste
treatment.

CHAPTER-3

MATERIAL & ENERGY

BALANCE

3.1 MATERIAL BALANCE

BASIS: 416 Kg/hr production of acetaldehyde

VAPORIZER AND SEPARATOR

Separator

Vaporizer

14
 Appendix-A

3 4 5

Amount of alcohol (95%) vapors required = 908.7 Kg/hr

Efficiency of vaporizer = 80%
(i.e. 80% liquid is being vaporized)
so feed to vaporizer (stream – 4) = 908.7/0.8
= 1135.8 Kg/hr
Material with streams-5 = 1133.8 Kg/hr
Material with stream-6 = 908.7 Kg/hr vapors of C2H5OH (95%)
Material with stream-7 = 1135.8 – 908.7 = 227.1 Kg/hr liquid
If we made overall material balance around the system shown, then
Material with stream-6 = Material with stream-3
So material with stream-3 = 908.7 Kg/hr

REACTOR-R1

Material entering with stream-8

C2H5OH = 863.26 Kg/hr = 18.766 Kgmol/hr
H2O = 45.43 Kg/hr = 2.524 Kgmol/hr
O2 = 635.28 Kg/hr = 19.852 Kgmol/hr
N2 = 2090.82 = Kg/hr = 74.62 Kgmol/hr
Chemical reaction involved is
C2H5OH + ½ O2 CH3CHO + H2O
As conversion of C2H5OH is 50% so
C2H5OH converted = 9.383 Kgmol/hr
C2H5OH unvonverted = 9.383 Kgmol/hr

15
 Appendix-A

O2 = converted = 9.383/2 = 4.692 Kgmol/hr

O2 = unconverted = 15.16 Kgmol/hr
CH3CHO formed = 9.383 Kgmol/hr
H2O = formed = 9.383 Kgmol/hr
Total water leaving = 2.524 + 9.383 = 11.907 Kgmol/hr
So material leaving with strea-9
C2H5OH = 9.383 Kgmol = 431.6 Kg
CH3CHO = 9.383 Kgmol = 412.85 Kg
H2O = 11.907 Kgmol = 214.33 Kg
O2 = 15.16 Kgmol = 485.12 Kg
N2 = 74.67 Kgmol = 2090.82 Kg
Total material leaving = 3634 Kg/hr
Total material entering = 3634 Kg/hr

ABSORBER-A1

In first absorber 95% entering acetaldehyde will be absorbed

1 1
0 1

9 1
4

16
 Appendix-A

Material entering with stream-9

CH3CHO = 422.85 Kg/hr
C2H5OH = 431.6 Kg/hr
H2O = 85.33 + 129 = 214.35 Kg/hr
O2 = 485.12 Kg/hr
N2 = 2090.82 Kg/hr
Material with stream-10
CH3CHO = 20.64 Kg/hr
C2H5OH = 17.1 Kg/hr
O2 = 485.12 Kg/hr
N2 = 2090.82 Kg/hr
Material entering with stream-11
H2O = 4064 Kg/hr
CH3OHO = 20.43 Kg/hr
C2H5OH = 17 Kg/hr
Material leaving with stream-14
CH3CHO = 412.6 Kg/hr
C2H5OH = 431.5 Kg/hr
H2O = 4278.6 Kg/hr
Total material entering = 7736 Kg/hr
Total material leaving = 7736 Kg/hr

17
 Appendix-A

ABSORBER-A2

99% of entering CH3CHO is absorbed in second absorber

1 1
0 1

9 1
4

Material entering with stream-10

CH3CHO = 20.64 Kg/hr
C2H5OH = 17.1 Kg/hr
O2 = 485.12 Kg/hr
N2 = 2090.82 Kg/hr
Material leaving with stream-12
CH3CHO = 0.21 Kg/hr

18
 Appendix-A

C2H5OH = 0.1 Kg/hr

O2 = 485.12 Kg/hr
N2 = 2090.82 Kg/hr
Material entering with stream-13 = H2O = 4064 Kg/hr
Material leaving with stream-11
CH3CHO = 20.43 Kg/hr
C2H5OH = 17 Kg/hr
H2O = 4064 Kg/hr
Total material entering = 6677.52 Kg/hr
Total material leaving = 6677.52 Kg/hr

DISTILLATION COLUMN-D1

1
5

1
4
1
6
Product Specifications

Top product
CH3CHO = 99%
C2H5OH = 0.8%
H2O = 0.2%
There should be no CH3CHO in bottoms

19
 Appendix-A

Material entering with stream-14

CH3CHO = 412.6 Kg/hr = 8.05%
C2H5OH = 431.58 Kg/hr = 8.4%
H2O = 4278.6 Kg/hr = 83.52%
Total = 5122.78 Kg/hr
So CH3CHO balance
0.0805 (5122.78) = 0.99 (D)
D = 416.55 Kg/hr
So top product is = 416.55 Kg/hr
Bottom product = 4706.2 Kg/hr
C2H5OH in top product = 0.008  416.55
= 3.33 Kg/hr
H2O in top product = 0.002  416.55
= 0.833
CH3CHO in top product = 412.00 Kg/hr
Material leaving in bottom product
C2H5OH = 431.58 – 3.33 = 428.25 Kg/hr
H2O = 4278.6 – 0.833 = 4277.76 Kg
Total material leaving = 5122 Kg/hr
Total material entering = 5122 Kg/hr

DISTILLATION COLUMN-D2

Product specifications
Top product
C2H5OH = 95%
H2O = 5%

20
 Appendix-A

Bottom product
C2H5OH = 1%
H2O = 99%

1
5

1
4
1
6

Feed
C2H5OH = 428.25 Kg/hr = 9.1%
H2O = 4277.70 Kg/hr = 90.9%
Total = 4706 Kg/hr
C2H5OH balance
0.091 (4706) = 0.95 D + 0.01 (W)
and D + W = 4706
by solving above equations
D = 405.5 Kg/hr
W = 4300 Kg/hr
So material with stream-17
C2H5OH = 0.95  405.5 = 385.22 Kg/hr
H2O = 0.05  405.5 = 20.275 Kg/hr

21
 Appendix-A

Material with stream-18

C2H5OH = 43 Kg/hr
H2O = 4257 Kg/hr
Total material entering = 4706 Kg/hr
Total material leaving = 4706 Kg/hr

3.2 ENERGY BALANCE

VAPORIZER

F
G

Separator
B

Vaporizer
A C D

Temperature of stream-A = 25 oC
Mass flow rate = 503 Kg/hr
Cp of 95% ethyl alcohol = 0.64 Kcal/KgoC
So heat with stream-A = 503  0.64  25
= 8048 Kcal/hr.
Similarly, heat ith stream-B = 27263 Kcal/hr
So, heat with stream-C = 27263 + 8048

22
 Appendix-A

= 35311 Kcal/hr
Flow rate of stream-C = 908.7
Cp = 0.73 Kcal/Kg oC
Temperature of stream-C = Q/mCp
35311
= 908.7  0.73

= 53 oC
Stream-G is saturated liquid at 2.3 atm
Heat with stream-G = Q = mCpT
= 227.1  0.92  112
= 23400 Kcal/hr
Heat with stream-D = 23400 + 35311
= 58711 Kcal/hr
Flow rate of stream-D = 1135.8 Kg/hr
58711
Temperature of stream-D = 1135 .8  0.78

= 66 oC
at 2.3 atm ethyl alcohol (95%) will be vaporized at 112 oC, so, we have to
supply heat to ethyl alcohol in vaporizer.

In vaporizer
Sensible heat
Q1 = mCpT
= 1135.8  0.87 (112 – 66)
= 45454.7 Kcal/hr
Latent heat

23
 Appendix-A

As only 80% ethyl alcohol (95%) is being vaporized so 908.7 Kg/hr of ethyl
alcohol will be vaporized.
Water vaporized = 0.05  908.7
= 45.43 Kg/hr
Latent heat of vaporization of water = 500 Kcal/hr
QH 2O = 22717.5 Kcal/hr
Ethyl alcohol evaporated = 863.2 Kg/hr
Latent heat of vaporization = 175 Kcal/kg
QC 2 H 5OH = 175  863.2 = 151071
Total heat to be supplied = 45454.7 + 22717.5 + 151071
= 219243.5
If steam is used at 130 oC latent heat of steam at 130 oC = 519.8 Kcal/kg
So, flow rate of steam = 219243.5/519.8
= 421 Kg/hr

Reactor
Standard heat of reaction = - 43 Kcal/hr
Heat of reaction at given conditions = 401860 Kcal/hr
So,
401860 Kcal/hr heat should be removed from reactor by cooling water.
Inlet temperature of cooling water = 25 oC
Outlet temperature of cooling water = 45 oC
Mass flow rate of water = m = ?
Q
m = C p T

401860
= 1  20
= 20093 Kg/hr

24
 Appendix-A

DISTILLATION COLUMN

Input = Output
WFHF + QR = QC + WBHB(l) + + WDHD(l)
WF = 256.4595 Kg-mol/hr
WB(l) = 246.9015 Kg-mol/hr
WD(l) = 9.5412 Kg-mol/hr
HF = 3145495 J/Kg-mol. hr
HB(l) = 3169709 Kg-mol/hr
HD(l) = 1473400 Kg-mol/hr
QC = 111507000 J/hr
QR = 1105043000 J/hr
Putting in eq.
917196375 J/hr = 917196375 J/hr

25
 Appendix-A

CHAPTER-4

REACTOR DESIGN

FIXED BED CATALYTIC REACTORS

4.1 INTRODUCTION

Fixed-bed catalytic reactors have been aptly characterized as the

workhorses of me process industries. For economical production of large
amounts of product, they are usually the first choice, particularly for gas-
phase reactions. Many catalyzed gaseous reactions are amenable to long
catalyst life (1-10 years); and as the time between catalyst change outs
increases, annualized replacement costs decline dramatically, largely due to
savings in shutdown costs. It is not surprising, therefore, that fixed-bed
reactors now dominate the scene in large-scale chemical-product
manufacture.

26
 Appendix-A

4.2 TYPES OF FIXED BED REACTOR

Fixed-bed reactors fall into one of two major categories:

 Adiabatic or
 Non-adiabatic.

A number of reactor configurations have evolved to fit the unique

requirements of specific types of reactions and conditions. Some of the more
common ones used for gas-phase reactions are summarized in Table(4.1) and
the accompanying illustrations. The table can be used for initial selection of
a given reaction system, particularly by comparing it with the known
systems indicated.

Table 4.1: Fixed-Bed Reactor Configurations for Gas-Phase Reactions

Classification Use Typical Applications

Single adiabatic bed Moderately exothermic Mild hydrogenation
or
endothermic non-
equilibrium
limited
Radial flow Where low AP is Styrene from
essential ethylbenzene
and useful where
change
in moles is large
Adiabatic beds in series High conversion, SO2 oxidation
with intermediate equilibrium Catalytic reforming
cooling or heating limited reactions Ammonia synthesis
Hydrocracking Styrene
from ethylbenzene
Multi-tabular Highly endothermic or Many hydrogenations
non-adiabatic exothermic reactions Ethylene oxidation to
requiring ethylene oxide,

27
 Feed Stream

Appendix-A

close temperature formaldehyde

control to by methanol oxidation,
ensure high selectivity phthalic anhydride
production
Direct-fired Highly endothermic, Steam reforming
non-adiabatic high temperature
reactions

4.4 SELECTION OF REACTOR TYPE

After analyzing different configuration of fixed bed reactors we have

concluded that for our system the most suitable reactors is multi tube fixed
bed reactor. Because oxidation of ethyl alcohol is highly exothermic
reaction, so cooling will be required otherwise the temperature of reactor
will rise and due to rise in temperature the catalyst activity and selectivity
will be affected and in turn, the formation of by-products will increase which
is direct loss of productions.

As reaction temperature is already high 550 oC if we keep the process

adiabatic temperature of reactor will rise and the structure of the catalyst will
be changed and catalyst will be damaged. For such a situation the best
reactor is multi-tube fixed bed reactor

4.5 CONSTRUCTION AND OPERATION OF

MULTI-TUBE FIXED BED REACTOR

Because of the necessity of removing or adding heat, it may not be

possible to use a single large-diameter tube packed with catalyst. In this

28
 Appendix-A

event the reactor may be built up of a number of tubes encased in a single

body, as illustrated in Fig. The energy exchange with the surroundings is
obtained by circulating, or perhaps boiling, a fluid in the space between the
tubes. If the heat effect is large, each catalyst tube must be small (tubes as
small as 1.0-in. diameter have been used) in order to prevent excessive
temperatures within the reaction mixture. The problem of deciding how
large the tube diameter should be, and thus how many tubes are necessary, to
achieve a given production forms an important problem in the design of such
reactors.

A disadvantage of this method of cooling is that the rate of heat

transfer to the fluid surrounding the tubes is about the same all along the
tube length, but the major share of the reaction usually takes place near the
entrance. For example, in an exothermic reaction the rate will be relatively
large at the entrance to the reactor tube owing to the high concentrations of
reactants existing there. It will become even higher as the reaction mixture
moves a short distance into the tube, because the heat liberated by the high
rate of reaction is greater than that which can be transferred to the cooling
fluid. Hence the temperature of the reaction mixture will rise, causing an
increase in the rate of reaction. This continues as the mixture moves up the
tube, until the disappearance of reactants has a larger effect on the rate than
the increase in temperature. Farther along the tube the rate will decrease.
The smaller amount of heat can now be removed through the wall with the
result that the temperature decreases. This situation leads to a maximum in
the curve of temperature versus reactor-tube length.

29
 Appendix-A

Feed Stream

Cooling
(or Heating)
fluid out

Cooling
(or Heating)
fluid in

Product
30 Stream
 Appendix-A

Figure-4.1: Multi-tubular fixed bed reactor

4.6 EFFECT OF VARIABLES ON MULTI-TUBE FIXED

BED REACTOR

4.6.1 Particle Diameter

The overall heat transfer coefficient declines with decrease in particle

size in the usual practical range. Redial gradients increase markedly with
decrease in particle size. Small size, however, may improve rate or
selectivity in some case by making catalyst inner surface more accessible.

4.6.2 Tube Diameter

Reducing tube diameter reduces the radial profile. Heat transfer area
per unit volume is inversely proportion al to the tube diameter and reaction
temperature is affected by a change in this area.

4.6.3 Outside Wall Coefficient

Improvement up to the point where this resistance becomes

negligible is worthwhile. Boiling liquids are advantageous because of the
high heat transfer coefficient.

31
 Appendix-A

4.6.4 Heat of Reaction and Activation Energy

Accurate values should be used since calculated temp. is sensitive

to both of these, particularly to the value of energy of activation. This
roust be determined carefully over the range of interests, but calculated
results should be obtained based on different activation energies over the
probable range of accuracy for the data so that final equipment sizing can
be done with a feel for uncertainties.

4.6.5 Particle Thermal Conductivity

One of the mechanisms of radial heat transfer in a bed, conduction

through the solid packing which must quite logically depend on the thermal
conductivity of the bed, can be reasoned to have some dependence on the
thermal conductivity of the solid. But since it only affects one of the several
mechanisms, the proportionally cannot be direct. Differences in effective
conductivity and the wall heat transfer coefficient h between beds of packing
having high and low solid conductivity may be in the range of a factor of
2-3. The largest difference will occur at lower Reynolds numbers. Most
catalyst carriers have low conductivities, but some such as carbides have
high conductivities.

32
 Appendix-A

4.7 DESIGN PROCEDURE FOR MULTI TUBE

FIXED
BED REACTOR

 To calculate weight of catalyst required

X A2
W dX A
FAo
   rA
X A1

Volume of reactor
If space time is know then space time = Volumetric flow rate

 By the knowledge of bulk density of catalyst and weight of catalyst

Calculate volume of reactor
weight of catalyst
Volume of reactor = bulk density of catalyst

 Decide the dimensions of tube; keeping in mind that

Dia of tube
Dia of catalyst particle
> 30

 Calculate volume of one tube and then number of tubes required

Volume of Reactor
No. of tubes = Volume of one tube

 Calculate the shell dia

33
 Appendix-A

 2π 
 Ds  k1  4  k 2   Pt  Ds  k1  nk3  k 4 
NT =
1.223 Pt  2

 Calculate pressure drop

ΔP  1  ε  G   α 1  ε  μ 
    βG 
L  ε  D pρ f C1   D p 

 Calculate heat transfer co-efficient

i) Shell side
1501  0.011t b  V 0.8
ho =
 D 0.2
ii) Tube side
0.7 dp
h pd  d pG   4.6
 3.50  e d
k  μ 

iii) Calculate overall heat transfer coefficient

 Calculate area required for heat transfer.

 Calculate area available for heat transfer.

Available area should be greater than required area

34
 Appendix-A

SPECIFICATION SHEET
Identification

Item Reactor
Item No. R-1
No. required 1

Function: Production of acetaldehyde by air oxidation of ethyl alcohol.

Operation: Continuous
Type: Catalytic
Multi tube, fixed bed

Chemical Reaction:
C2H5OH + ½ O2 CH3CHO + H2O
 H298 = - 43 Kcal

Catalyst: Silver, coated on alumina

Shape: Spherical
Size: 1.25 mm

Tube side: Tubes:

Material handled Feed Product No. 709
(kg/hr) (kg/hr) Length 2.438 m
C2H5OH 86326 432.58 O. D 63.5 mm
H2O 45.44 214.35 Pitch 79.37 mm  pattern
CH3CHO ----- 412.8 Material of construction = copper
O2 635.28 484.96
N2 2090.82 2090.82
o
Temp ( C) 550 550
Shell side Shell
Fluid handled = cooling water Dia = 2.66 m

35
 Appendix-A

Temperature 25oC to 45oC Material of construction = Carbon

steel
Heat transfer area required = 77.67 m2
Overall heat transfer coefficient = 10.77 W/m2 oC

CHAPTER-5

DESIGN OF ABSORBER
5.1 ABSORPTIONS

The removal of one or more component from the mixture of gases by

using a suitable solvent is second major operation of Chemical Engineering
that based on mass transfer.

In gas absorption a soluble vapours are more or less absorbed in the

solvent from its mixture with inert gas. The 'purpose of such gas scrubbing
operations may be any of the following;

a) For Separation of component having the economic value.

b) As a stage in the preparation of some compound.
c) For removing of undesired component (pollution).

5.2 TYPES OF ABSORPTION

1) Physical absorption,
2) Chemical Absorption.

36
 Appendix-A

5.2.1 Physical Absorption

In physical absorption mass transfer take place purely by diffusion

and physical absorption is governed by the physical equilibria.

5.2.2 Chemical Absorption

In this type of absorption as soon as a particular component comes in

contact with the absorbing liquid a chemical reaction take place. Then by
reducing the concentration of component in the liquid phase, which
enhances the rate of diffusion.

5.3 TYPES OF ABSOR5SRS

There are two major types of absorbers which are used for
absorption purposes:

 Packed column
 Plate column

5.4 COMPARISON BETWEEN PACKED AND PLATE

COLUMN

1) The packed column provides continuous contact between vapour and

liquid phases while the plate column brings the two phases into
contact on stage wise basis.
2) SCALE: For column diameter of less than approximately 3 ft. It is
more usual to employ packed towers because of high fabrication cost

37
 Appendix-A

of small trays. But if the column is very large then the liquid
distribution is problem and large volume of packing and its weight is
problem.
3) PRESSURE DROP: Pressure drop in packed column is less than the
plate column. In plate column there is additional friction generated as
the vapour passes through the liquid on each tray. If there are large
No. of Plates in the tower, this pressure drop may be quite high and
the use of packed column could effect considerable saving.
4) LIQUID HOLD UP: Because of the liquid on each plate there may be
a Urge quantity of the liquid in plate column, whereas in a packed
tower the liquid flows as a thin film over the packing.
5) SIZE AND COST: For diameters of less than 3 ft. packed tower
require lower fabrication and material costs than plate tower with
regard to height, a packed column is usually shorter than the
equivalent plate column.

From the above consideration packed column is selected as the

absorber, because in our case the diameter of the column is approximately
0.8 meter which is less than 3 ft. As the solubility is infinity so the liquid
will absorb as much gases as it remain in contact with gases so packed tower
provide more contact. It is easy to operate.

5.5 PACKING

The packing is the most important component of the system. The

packing provides sufficient area for intimate contact between phases. The
efficiency of the packing with respect to both HTU and flow capacity

38
 Appendix-A

determines to a significance extent the overall size of the tower. The

economics of the installation is therefore tied up with packing choice.

The packings are divided into those types which are dumped at
random into the tower and these which must be stacked by hand. Dumped
packing consists of unit 1/4 lo 2 inches in major dimension and are used
roost in the smaller columns. The units in stacked packing are 2 to about 8
inches in size, they are used only in the larger towers.

The Principal Requirement of a Tower packing are:

1) It must be chemically inert to the fluids in the tower.

2) It must be strong without excessive weight.
3) It must contain adequate passages for both streams without
excessive liquid hold up or pressure drop.
4) It must provide good contact between liquid and gas.
5) It must be reasonable in cost.

Thus most packing are made of cheap, inert, fairly light materials such
as clay, porcelain, or graphite. Thin-walled metal rings of steel or aluminum
are some limes used.
Common Packings are:

a) Berl Saddle.
b) Intalox Saddle.
c) Rasching rings.
d) Lessing rings.
e) Cross-partition rings.
f) Single spiral ring.

39
 Appendix-A

g) Double - Spiral ring.

h) Triple - Spiral ring.

5.6 DESIGNING STEPS FOR ABSORPTION COLUMN

 Determining the approximate dia of the column

 Selection of column.
 Selection of packing and material
 Calculating the size of packing
 Calculating the actual dia of column
 Calculating the flooding velocity
a) Finding loading velocity with the knowledge the flooding
velocity
b) Calculating actual dia of column

 Finding the no. of transfer units (NoG)

 Determining the height of packing
 Determining the height of the column
 Determining the pressure drop.
a  10 bg 2F
 by equation P = [in. water /ft of packing]
ρG

40
 Appendix-A

SPECIFICATION SHEET

Identification
Item: Packed Absorption Column
Item No. A1
No. required 01

Function: To absorb acetaldehyde and ethyl alcohol in water.

Operation: Continuous
Material Entering gas Exit gas Liquid Liquid
Handled Kg/hr Kg/hr entering leaving
Kg/hr Kg/hr
CH3CHO 412.8 20.64 20.43 412.6
C2H5OH 431.58 17.1 17 414.48
H2O 85.35 ------- 4064 4278.6
O2 484.96 484.96 ------- ------
N2 2090.82 2090.82 ------- ------

Design Data
No. of transfer units = 7
Height of transfer units = 0.2 ft (0.06 m)
Height of packing section = 6.44 ft (1.96 m)
Total height of column = 15 ft (4.5 m)
Inside diameter = 2.62 ft (0.8 m)
Flooding velocity = 2.36 m/sec
Maximum allowable gas velocity = 1.416 m/sec
Pressure drop = 20 mmH2O/m of packing

Internals
Size and type = 66 mm,
Material of packing:
Method of packing:
Packing arrangement:
Type of packing support:
Type of liquid distributor:
intalox saddle
Ceramic
(wet) float into tower filled with water.
dumped
gas injection support
Weir flow distributor

41
 Appendix-A

CHAPTER-6

DESIGN OF DISTILLATION
COLUMN

In industry it is common practice to separate a liquid mixture by distillating

the components, which have lower boiling points when they are in pure
condition from those having higher boiling points. This process is
accomplished by partial vaporization and subsequent condensation.

6.1 CHOICE BETWEEN PLATE AND PACKED COLUMN

Vapour liquid mass transfer operation may be carried either in plate

column or packed column. These two types of operations are quite different.
A selection scheme considering the factors under four headings.

i) Factors that depend on the system i.e. scale, foaming, fouling

factors, corrosive systems, heat evolution, pressure drop, liquid
holdup.
ii) Factors that depend on the fluid flow moment.
iii) Factors that depends upon the physical characteristics of the
column and its internals i.e. maintenance, weight, side stream, size
and cost.

42
 Appendix-A

iv) Factors that depend upon mode of operation i.e. batch distillation,
continuous distillation, turndown, intermittent distillation.

The relative merits of plate over packed column are as follows:

i) Plate column are designed to handle wide range of liquid flow

rates without flooding.
ii) If a system contains solid contents, it will be handled in plate
column, because solid will accumulate in the voids, coating the
packing materials and making it ineffective.
iii) Dispersion difficulties are handled in plate column when flow rate
of liquid are low as compared to gases.
iv) For large column heights, weight of the packed column is more
than plate column.
v) If periodic cleaning is required, man holes will be provided for
cleaning. In packed columns packing must be removed before
cleaning.
vi) For non-foaming systems the plate column is preferred.
vii) Design information for plate column are more readily available
and more reliable than that for packed column.
viii) Inter stage cooling can be provide to remove heat of reaction or
solution in plate column.
ix) When temperature change is involved, packing may be damaged.

For this particular process, “Acetaldehyde, ethyl alcohol and water system”,
I have selected plate column because:
i) System is non-foaming.
ii) Temperature is high (91o C).

43
 Appendix-A

6.2 CHOICE OF PLATE TYPE

There are four main tray types, the bubble cap, sieve tray, ballast or
valve trays and the counter flow trays. I have selected sieve tray because:

i) They are lighter in weight and less expensive. It is easier and

cheaper to install.

ii) Pressure drop is low as compared to bubble cap trays.

iii) Peak efficiency is generally high.

iv) Maintenance cost is reduced due to the ease of cleaning.

6.3 DESIGNING STEPS OF DISTILLATION COLUMN

 Calculation of Minimum Reflux Ratio Rm.

 Calculation of optimum reflux ratio.
 Calculation of theoretical number of stages.
 Calculation of actual number of stages.
 Calculation of diameter of the column.
 Calculation of weeping point.
 Calculation of pressure drop.
 Calculation of thickness of the shell.
 Calculation of the height of the column.

44
 Appendix-A

SPECIFICATION SHEET

Identification:
Item Distillation column
Item No. DC1
No. required 1
Tray type Sieve tray
Function : Recovery of Acetaldehyde
Operation: Continuous
Material handled
Feed Top Bottom
Quantity 256.4595 Kgmol/hr 9.5412 Kgmol/hr 246.9015
Kgmol/hr
Composition of 3.66% 98.2% 0
acetaldehyde
Temperature 91oC 20o C 96 oC

Design Data
No. of trays = 12 hole area/active area = 0.10
Pressure = 1 atm weir length = 0.5867 m
Height of column = 4.3 m weir length = 25.4 mm
Diameter of column = 0.762 m reflux ratio = 3.5:1
Hole size = 3.175mm tray spacing = 0.3048 m
Tray thickness = 3mm Down comer area = 4.56912 . 10-2 m2
Flooding = 53 % Hole area = 0.045576 m2
Active area = 0.34638 m2
CHAPTER-7

45
 Appendix-A

DESIGN OF HEAT
EXCHANGERS

7.1 INTRODUCTION

A heat exchanger is a heat-transfer devise that is used for transfer of

internal thermal energy between two or more fluids available at different
temperatures. In most heat exchangers, the fluids are separated by a heat-
transfer surface, and ideally they do not mix. Heat exchangers are used in the
process, power, petroleum, transportation, air conditioning, refrigeration,
cryogenic, heat recovery, alternate fuels, and other industries. Common
examples of heat exchangers familiar to us in day-to-day use are automobile
radiators, condensers, evaporators, air pre-heaters, and oil coolers.

In our project a number of heat exchangers are used . Here we will

discuss heat exchanger used as

 Condenser
 Vaporizer
 Preheater

All of these are shell and tube heat exchangers.

46
 Appendix-A

Selection Guide To Heat Exchanger Types

Approximate
relative cost
Applications best
Type Significant feature Limitations in carbon
suited
steel
construction
Condensers; liquid-
Temperature difference
liquid; gas-gas; gas-
Fixed tube Both tube sheets fixed to at extremes of about 200
liquid; cooling and o 1.0
sheet shell. F Due to differential
heating, horizontal or
expansion.
vertical, reboiling.
One tubesheet “floats” in High temperature
Floating head Internal gaskets offer
shell or with shell, tube differentials, above
or tubesheet danger of leaking.
bundle may or may not about 200 oF extremes;
(removable Corrosiveness of fluids
be removable from shell, dirty fluids requiring 1.28
and on shell-side floating
but back cover can be cleaning of inside as
nonremovable parts. Usually confined
removed to expose tube well as outside of shell,
bundles) to horizontal units.
ends. horizontal or vertical.
Bends must be carefully
High temperature made, or mechanical
differentials, which damage and danger of
Only one tube sheet
might require provision rupture can result. Tube
U-tube; required. Tubes bent in
for expansion in fixed side velocities can cause 0.9-1.1
U-Bundle U-shape. Bundle is
tube units. Easily erosion of inside of
removable.
cleaned conditions on bends. Fluid should be
both tube and shell side. free of suspended
particles.
Relatively small transfer
Each tube has own shell
area service, or in banks Services suitable for
forming annular space
for larger applications. finned tube. Piping-up a
Double pipe for shell side fluid. 0.8-1.4
Especially suited for large number often
Usually use externally
high pressures in tube requires cost and space.
finned tube.
(greater than 400 psig).
Pipe coil for submersion
Transfer coefficient is
in coil-box of water or Condensing, or
low, requires relatively
Pipe coil sprayed with water is relatively low heat loads 0.5-0.7
large space if heat load is
simplest type of on sensible transfer.
high.
exchanger.
Not well suited for
Composed of metal-
Viscous fluids, corrosive boiling or condensing;
Plate and formed thin plates
fluids, slurries, high heat limit 350-500 oF by 0.8-1.5
frame separated by gaskets.
transfer. gaskets. Used for liquid-
Compact, easy to clean.
liquid only; not gas-gas.
Compact, concentric
plates; no bypassing, Cross-flow, condensing, Process corrosion,
Spiral 0.8-1.5
high turbulence. heating. suspended materials.

47
 Appendix-A

7.2 SHELL AND TUBE HEAT EXCHANGER

In process industries, shell and tube exchangers are used in great
numbers, far more than any other type of exchanger. More than 90% of heat
exchangers used in industry are of the shell and tube type. The shell and tube
heat exchangers are the “work horses” of industrial process heat transfer.
They are the first choice because of well-established procedures for design
and manufacture from a wide variety of materials, many years of
satisfactory service, and availability of codes and standards for design and
fabrication. They are produced in the widest variety of sizes and styles.
There is virtually no limit on the operating temperature and pressure.
7.2.1 Classification of Shell and Tube Heat Exchangers
There are four basic considerations in choosing a mechanical
arrangement that provides for efficient heat transfer between the two fluids
while taking care of such practical matters as preventing leakage from one
into the other.
1) Consideration for differential thermal expansion of
tubes and shell.
2) Means of directing fluid through the tubes.
3) Means of controlling fluid flow through the shell.
4) Consideration for ease of maintenance and servicing.

Heat exchangers have been developed with different approaches to

these four fundamental design factors. Three principal types of heat
exchangers

2) Fixed tube-sheet exchangers

3) U-tube exchangers and

48
 Appendix-A

4) Floating head exchangers—satisfy these design requirements.

Design procedure for shell-and-tube heat exchangers

49
 Appendix-A

7.3 VAPORIZERS

Vaporizers are heat exchangers which are specially designed to supply

latent heat of vaporization to the fluid. In some cases it can also preheat the
fluid then this section of vaporizers will be called upon preheating zone and
the other section in which latent heat is supplied; is known as vaporization
zone but he whole assembly will be called a vaporizer.

Vaporizers are called upon to fulfill the multitude of latent-heat

services which are not a part of evaporative or distillation process.

There are two principal types of tubular vaporizing equipment used in

industry: Boilers and Vaporizing Exchangers. Boilers are directly fired
tubular apparatus, which primarily convert fuel energy into latent heat of
vaporization. Vaporizing Exchangers are unfired and convert latent or
sensible heat of one fluid into the latent heat of vaporization of another. If a
vaporizing exchanger is used for the evaporation of water or an aqueous
solution, it is now fairly conventional to call it an Evaporator, if used to
supply the heat requirements at the bottom of a distilling column, whether
the vapor formed be steam or not, it is a Re-boiler; when not used for the
formation of steam and not a part of a distillation process, a vaporizing
exchanger is simply called a vaporizer. So any unfired exchanger in which
one fluid undergoes vaporization and which is not a part of an evaporation or
distillation process is a vaporizer.

7.4 TYPES OF VAPORIZERS

Some common types of vaporizers are
 Vertical vaporizer

50
 Appendix-A

 Indirect fluid heater

 Tubular low temperature vaporizer
 Electrical resistance vaporizer
 Cryogenic vaporizer

The commonest type of vaporizer is the ordinary horizontal 1-2

exchanger or one of its modifications, and vaporization may occur in the
shell or in the tubes. If steam is the heating medium, the corrosive action of
air in the hot condensate usually makes it advantageous to carry out the
vaporization in the shell.

In the case of vaporizer, however, operation is often at high pressure,

and it is usually too expensive to provide disengagement space in the shell,
since the inclusion of disengagement space at high pressures
correspondingly increases the shell thickness. For this reason vaporizers are
not usually designed for internal disengagement. Instead some external
means. Such as an inexpensive welded drum, is connected to the vaporizer
where in the entrained liquid is separated from the vapor.

When a 1-2 exchanger is used as a vaporizer, it is filled with tubes and

cannot be adapted for blow down, since all the feed to a vaporizer is usually
of value and a rejection as blow down is prohibitive. If the feed were
completely vaporized in the vaporizer, it would emerge as a vapor and any
dirt which a was originally present would be left behind on the tube surface
over which total vaporization of occurred, fouling it rapidly, If the 1-2
exchanger (vaporization) were over-designed, that is, if it contained too
much surface, disengagement would have to occur on the tubes and due to

51
 Appendix-A

the excess surface the vapor would superheat above its saturation
temperature.

The feed to a vaporizer should not be vaporized completely. The value

of this rule is apparent. If less that 100 percent to the feed is vaporized in 1-2
exchangers, the residual liquid can be counted on to prevent the
accumulation of dirt directly on the surface of the heating element. A
maximum of about 80 percent vaporization appears to provide favorable
operation in 1-2 exchanges, although higher percentages may be obtained in
vessels having interval disengagement space.

Forced and Natural – circulation Vaporizer. When liquid is fed to is

fed by forced circulation. The circuit consists of a 1-2 exchanger serving as
the vaporizer and a disengaging drum from which the un-vaporized liquid is
withdrawn and recombined with fresh feed. The generated vapor is removed
form the top of the drum.

The vaporized may also be connected with a disengaging drum

without the use of a reticulating pump. This scheme is natural circulation. It
requires that the disengaging drum be elevated above the vaporizer. The
advantages of forced circulation or natural circulation are in part economics
and a part dictated by space. The forced-circulation arrangement requires the
use of a pump with its continuous operating cost and fixed charges. As with
forced-circulation evaporators, the rate of feed recirculation can be
controlled very closely. If the installation is small, then use of a pump
preferable. If a natural-circulation arrangement is used pump and stuffing
box problems are eliminated but considerably more headroom must be
provided and recirculation rates cannot be controlled so readily.

52
 Appendix-A

The vaporization of a cold liquid coming from storage, the liquid may
not be at its boiling point and may require preheating to the boiling point.
Since the shell of a forced-circulation vaporizer is essentially the same as
any other 1-2 exchangers, the preheating can be done in the same shell as the
vaporization. If the period of performance of a vaporizer is to be measured
by a single overall dirt factor, it is necessary to divide the shell surface into
two successive zones, one for preheating and one for vaporization.

The true temperature difference is the weighted temperature difference

for the two zones, and the clean coefficient is the weighted clean coefficient.

Vaporizers tend to accumulate dirt, and for his reason higher

circulation rates and large dirt factors will often be desirable. Preference
should be given to the use of square pitch and a removable tube bundle.
Although it may reduce the possibility of using a 1-2 vaporizing exchanger
for other services, the baffle spacing can be increased or staggered form inlet
to outlet to reduce the pressure drop of the fluid vaporizing in the shell.

53
 Appendix-A

SPECIFICATION SHEET FOR VAPORIZER

Identification

Unit Vaporizer
Item No. V-1
Type Forced Circulation
No. of Item 1

Function To vaporize the alcohol

Operation Continuous

Heat duty 905318.7 Btu/hr

Heat transfer area 260.7 ft2
Overall heat transfer coefficient 88 Btu/hr-ft2 oF
Dirt factor 0.003hr-ft2 oF/Btu

Shell side Tube side

Fluid circulated Ethyl alcohol Steam
Flow rates 2501.76 lb/hr 966.7 lb/hr
Temperature Inlet = 150.8 oF 266o F
Outlet = 233.6 oF
Pressure 44.1 psi 39 psi
Pressure drop 1.3 psi 0.035 psi
Material of construction Carbon steel Carbon steel
Specifications I.D = 17.25 in OD = ¾ in 16 BWG
C = 0.25 in Pitch = 1 in
B = 4 in Square arrangement,
Length = 8 ft
Nt = 166

54
 Appendix-A

7.5 CONDENSERS

Introduction

A condenser is a two-phase flow heat exchanger in which heat is generated

from the conversion of vapor into liquid (condensation) and the heat
generated is removed from the system by a coolant. Condensers may be
classified into two main types: those in which the coolant and condensate
stream are separated by a solid surface, usually a tube wall, and those in
which the coolant and condensing vapor are brought into direct contact.

The direct contact type of condenser may consist of a vapor which is

bubbled into a pool of liquid, a liquid which is sprayed into a vapor, or a
packed-column in which the liquid flows downwards as a film over a
packing material against the upward flow of vapor. Condensers in which the
streams are separated may be subdivided into three main types: air-cooled,
shell-and-tube, and plate. In the air-cooled type, condensation occurs inside
tubes with cooling provided by air blown or sucked across the tubes. Fins
with large surface areas are usually provided on the air side to compensate
for the low air-side heat transfer coefficients. In shell-and-tube condensers,
the condensation may occur inside or outside the tubes. The orientation of
the unit may be vertical or horizontal. In the refrigeration and air-
conditioning industry, various types of two-phase flow heat exchangers are
used. They are classified according to whether they are coils or shell-and-
tube heat exchangers. Evaporator and condenser coils are used when the
second fluid is air because of the low heat transfer coefficient on the air side.
In the following sections, the basic types of condensers are shown:

55
 Appendix-A

Four Condenser Configuration are Possible

1) Horizontal with condensation is shell side and cooling medium in

the tubes.
2) Horizontal with condensation in tube side cooling medium in shell
side.
3) Vertical with condensation in the shell.
4) Vertical with condensation in the tubes.

Horizontal shell side and vertical tube side are the most commonly
used types of condensers.

In this process we have used the normal mechanism for heat transfer
in commercial condenser which film wise condensation.

Since vapor-liquid heat transfer changes usually occur at constant or

really constant pressure in industry, the vaporization or condensation of a
single compared normally occurs isothermally.

If a mixture of vapors instead of a pure vapor is condensed at constant

pressure, the change does not take place isothermally in most instances.

Types of Condensers

Steam Turbine Exhaust Condensers

Plate Condensers
Air-Cooled Condensers
Direct Contact Condensers

56
 Appendix-A

SPECIFICATION SHEET

CONDENSER

Identification: Item condenser

No. Required = 1
Function: Condense vapors by removing the latent heat of vaporization
(95% ethanol)
Operation: Continuous
Type: 2-4 Horizontal Condenser
Shell side condensation
Heat Duty = 8951684.54 Btu/hr
Tube Side: Tubes: ¾ in. diam. 16 BWG
Fluid handled cold water 468 tubes each 10 ft long
Flow rate = 248657 lb/hr 4 passes
Pressure = 14.7 psia 15/16 triangular pitch
Temperature = 77 oF to 113 oF pressure drop = 472 psi
Shell Side: Shell: 25 in. diam. 2 passes
Fluid handled C2H5OH + H2O Baffles spacing 20 in.
vapor (95% ethanol vapor) Pressure drop = 3.12 psi
Flow rate 22267.8 lb/hr
Pressure 14.7 psia
Temperature 180oF to 178oF
Utilities: Cold water
Ud assumed = 100 Btu/hr-ft2-oF Ud calculated 109 Btu/hr-ft2-oF
Uc calculated = 163 Btu/hr-ft2-oF Allowed dirt factor = Rd = 0.003

CHAPTER-8

57
 Appendix-A

PUMP AND COMPRESSOR

SELECTION
8.1 FACTORS AFFECTING CHOICE OF A PUMP

Many different factors can influence the final choice of a pump for a
particular operation. The following list indicates the major factors that
govern pump selection.
.
1) The amount of fluid that must be pumped. This factor determines the
size of pump (or pumps) necessary.

2) The properties of the fluid. The density and the viscosity; of the fluid
influence the power requirement for a given set of operating
conditions, corrosive properties of the fluid determine the acceptable
materials of construction. If solid particles are suspended in the fluid,
this factor dictates the amount of clearance necessary and may
eliminate the possibility of using certain types of pumps.

3) The increase in pressure of the fluid due to the work input of the
pumps. The head change across the pump is influenced by the inlet
and downstream reservoir pressures, the change in vertical height of
the delivery line, and frictional effects. This factor is a major item in
determining the power requirements.

4) Type of flow distribution. If nonpulsating flow is required, certain

types of pumps, such as simplex reciprocating pumps, may be

58
 Appendix-A

unsatisfactory. Similarly, if operation is intermittent, a self-priming

pump may be desirable, and corrosion difficulties may be increased.

5) Type of power supply. Rotary positive-displacement pumps and

centrifugal pumps are readily adaptable for use with electric-motor or
internal-combustion-engine drives; reciprocating pumps can be used
with steam or gas drives.

6) Cost and mechanical efficiency of the pump.

PUMP P-1

The duty of P-I is to pump ethyl alcohol from 1 atm to 2.3 atm with a flow
rare of 1135.8 Kg/hr. for this purpose the best choice is centrifugal pump
because the required pressure is not so high.

PUMP P-2

The duty of pump-2 is to pump a mixture of water, ethyl alcohol and

acetaldehyde with slight pressure development and the flow late required is
5122.78 Kg/hr. Centrifugal pump is most suitable pump for such a service
i.e. high flow rate and low pressure development.

8.2 COMPRESSOR SELECTION

Compressor C-1

The duty of compressor is to compress the air from 1 atm to 2.3 atm and to
made the air flow with flow rate 2726 Kg/hr/

59
 Appendix-A

As compression ratio is less than 5 so, single stage compressor will be

sufficient and type of compressor suitable for this situation is “centrifugal
compressor”, because our objective is to develop just 2.3 atm pressure with
relatively high flow rate.

CHAPTER-9

60
 Appendix-A

INSTRUMENTATION AND
PROCESS CONTROL
Measurement is a fundamental requisite to process control. Either the control
can be affected automatically, semi-automatically or manually. The quality
of control obtainable also bears a relationship to the accuracy,
re-productability and reliability of the measurement methods, which are
employed. Therefore, selection of the most effective means of measurements
is an important first step in the design and formulation of any process
control system.

9.1 TEMPERATURE MEASUREMENT AND CONTROL

Temperature measurement is used to control the temperature of outlet

and inlet streams in heat exchangers, reactors, etc.

Most temperature measurements in the industry are made by means of

thermo-couples to facilitate bringing the measurements to centralized
location. For local measurements at the equipment bi-metallic or filled
system thermometers are used to a lesser extent. Usually, for high
measurement accuracy, resistance thermometers are used.

All these meters are installed with thermo-wells when used locally.
This provides protection against atmosphere and other physical elements.

61
 Appendix-A

9.2 PRESSURE MEASUREMENT AND CONTROL

Like temperature pressure is a valuable indication of material state

and composition. In fact, these two measurement considered together are
the primary evaluating devices of industrial materials.

Pumps, compressor and other process equipment associated with

pressure changes in the process material are furnished with pressure
measuring devices. Thus pressure measurement becomes an indication of
energy increase or decrease.

Most pressure measurement in industry are elastic element devices,

either directly connected for local use or transmission type to centralized
location. Most extensively used industrial pressure element is the Bourderi
Tube or a Diaphragm or Bellows gauges.

9.3 FLOW MEASUREMENT AND CONTROL

Flow-indicator-controllers are used to control the amount of liquid.

Also all manually set streams require some flow indication or some easy
means for occasional sample measurement. For accounting purposes, feed
and product stream are metered. In addition utilities to individual and
grouped equipment are also metered.

Most flow measures in the industry are/ by Variable Head devices. To

a lesser extent Variable Area is used, as are the many available types as
special metering situations arise. .

9.4 CONTROL SCHEMES OF DISTILLATION COLUMN

62
 Appendix-A

GENERAL CONSIDERATION

9.4.1 Objectives

In distillation column control any of following may be the goals to

achieve
1. Over head composition.
2. Bottom composition
3. Constant over head product rate. .
4. Constant bottom product rate.

9.4.2 Manipulated Variables

Any one or any combination of following may be the manipulated

variables

1. Steam flow rate to reboiler.

2. Reflux rate.
3. Overhead product withdrawn rate.
4. Bottom product withdrawn rate
5. Water flow rate to condenser.

9.5 LOADS OR DISTURBANCES

Following are typical disturbances

1. Flow rate of feed

63
 Appendix-A

2. Composition of feed.
3. Temperature of feed.
4. Pressure drop of steam across reboiler
5. Inlet temperature of water for condenser.

9.6 CONTROL SCHEME

Overhead product rate is fixed and any change in feed rate must be
absorbed by changing bottom product rate. The change in product rate is
accomplished by direct level control of the reboiler if the stream rate is fixed
feed rate increases then vapor rate is approximately constant & the internal
reflux flows must increase.

ADVANTAGE

Since an increase in feed rate increase reflux rate with vapor rate being
approximately constant, then purity of top product increases.

DISADVANTAGE

The overhead reflux change depends on the dynamics of level control

system that adjusts it.

64
 Appendix-A

Figure: Control scheme

CHAPTER-10

65
 Appendix-A

HAZOP STUDY
INTRODUCTION

A HAZOP survey is one of the most common and widely accepted methods
of systematic qualitative hazard analysis. It is used for both new or existing
facilities and can be applied to a whole plant, a production unit, or a piece of
equipment It uses as its database the usual sort of plant and process
information and relies on the judgment of engineering and safety experts in
the areas with which they are most familiar. The end result is, therefore
reliable in terms of engineering and operational expectations, but it is not
quantitative and may not consider the consequences of complex sequences
of human errors.

The objectives of a HAZOP study can be summarized as follows:

1) To identify (areas of the design that may possess a significant

hazard potential.

2) To identify and study features of the design that influence the

probability of a hazardous incident occurring.

3) To familiarize the study team with the design information

available.

66
 Appendix-A

4) To ensure that a systematic study is made of the areas of significant

hazard potential.

5) To identify pertinent design information not currently available to

the team.

6) To provide a mechanism for feedback to the client of the study

team's detailed comments.

A HAZOP study is conducted in the following steps:

1) Specify the purpose, objective, and scope of the study. The purpose
may he the analysis of a yet to be built plant or a review of the risk
of un existing unit. Given the purpose and the circumstances of the
study, the objectives listed above can he made more specific. The
scope of the study is the boundaries of the physical unit, and also
the range of events and variables considered. For example, at one
time HAZOP's were mainly focused on fire and explosion
endpoints, while now the scope usually includes toxic release,
offensive odor, and environmental end-points. The initial
establishment of purpose, objectives, and scope is very important
and should be precisely set down so that it will be clear, now and
in the future, what was and was not included in the study. These
decisions need to be made by an appropriate level of responsible
management.

2) Select the HAZOP study team. The team leader should be skilled
in HAZOP and in interpersonal techniques to facilitate successful
group interaction. As many other experts should be included in the

67
 Appendix-A

team to cover all aspects of design, operation, process chemistry,

and safety. The team leader should instruct the team in the HAZOP
procedure and should emphasize that the end objective of a
HAZOP survey is hazard identification; solutions to problems are a
separate effort.

3) Collect data. Theodore16 has listed the following materials that are
usually needed:

 Process description
 Process flow sheets
 Data on the chemical, physical and toxicological properties of
all raw materials,, intermediates, and products.
 Piping and instrument diagrams (P&IDs)
 Equipment, piping, and instrument specifications
 Process control logic diagrams
 Layout drawings
 Operating procedures
 Maintenance procedures
 Emergency response procedures

 Safety and training manuals

68
 Appendix-A

69
 Appendix-A

Table-10.2: HAZOP Guide Words and Meanings

Guide Words Meaning

No Negation of design intent
Less Quantitative decrease
More Quantitative increase
Part of Qualitative decrease
As well as Qualitative Increase
Reverse Logical opposite of the intent
Other than Complete substitution

4) Conduct the study. Using the information collected, the unit is

divided into study "nodes" and the sequence diagrammed in Figure
, is followed for each node. Nodes are points in the process where
process parameters (pressure, temperature, composition, etc.) have
known and intended values. These values change between nodes as
a result of the operation of various pieces of equipment' such as
distillation columns, heat exchanges, or pumps. Various forms and
work sheets have been developed to help organize the node process
parameters and control logic information.

When the nodes are identified and the parameters are identified, each
node is studied by applying the specialized guide words to each parameter.
These guide words and their meanings are key elements of the HAZOP
procedure. They are listed in Table(10.1).

70
 Appendix-A

Repeated cycling through this process, which considers how and why
each parameter might vary from the intended and the consequence, is the
substance of the HAZOP study.

5) Write the report. As much detail about events and their

consequence as is uncovered by the study should be recorded.
Obviously, if the HAZOP identifies a not improbable sequence of
events that would result in a disaster, appropriate follow-up action
is needed. Thus, although risk reduction action is not a part of the
HAZOP, the HAZOP may trigger the need for such action.

The HAZOP studies are time consuming and expensive. Just getting
the P & ID's up to date on an older plant may be a major engineering effort.
Still, for processes with significant risk, they are cost effective when
balanced against the potential loss of life, property, business, and even the
future of the enterprise that may result from a major release.

HAZOP Study of Storage Tank for Ethyl Alcohol

A HAZOP study is to be conducted on ethyl alcohol storage tank, as

presented by the piping and instrumentation diagram show in fig(10.2).
In this scheme, ethyl alcohol is unloaded from tank trucks into a
storage tank maintained under a slight positive pressure until it is transferred
to the process. Application of the guide words to the storage tank is shown in
Table(10.2) along with a listing of consequences that results from process
deviation. Some of the consequences identified with these process deviations
have raised additional questions that need resolution to determine whether or
not a hazard exist.

71
 Appendix-A

Ethyl Alcohol
Storage Tank

Figure-10.2: Piping and instrumentation diagram

72
 Appendix-A

Deviations Consequences of this

from What event could cause deviation on item of Process
operating this deviation equipment under indications
conditions consideration
Level:
Less Tank runs dry Pump cavitates LIA-1
FICA-1
Rupture of discharge line Reagent released LIA-1,
V-3 open or broken FICA-1
V-1 open or broken Reagent released LIA-1
Tank rupture (busting of Reagent released LIA-1
vessel) Reagent released LIA-1

More Unload too much from Tank overfills LIA-1

column
Reverse flow from Tank overfills LIA-1
process
Temperature:
Less Temperature of inlet is Possible vacuum
colder than normal
More Temperature of inlet is Region released
hotter than normal
External fire Tank fails

73
 Appendix-A

CHAPTER-11

ENVIRONMENTAL IMPACT
ASSESSMENT

HEALTH HAZARD INFORMATION

Acute Effects:

The primary acute (short-term) effect of inhalation exposure to acetaldehyde

is irritation of the eyes, skin, and respiratory tract in humans. Erythema,
coughing, pulmonary edema, and necrosis may also occur and, at extremely
high concentrations, respiratory paralysis and death.

Acute inhalation of acetaldehyde resulted in a depressed respiratory

rate and elevated blood pressure in experimental animals.

Tests involving acute exposure of animals, such as the LC 50 and LD50

tests in rats, rabbits, and hamsters, have demonstrated acetaldehyde to have
low acute toxicity from inhalation and moderate acute toxicity from oral or
dermal exposure.

74
 Appendix-A

Chronic Effects (Noncancer)

In hamsters, chronic (long-term) inhalation exposure to acetaldehyde has

produced changes in the nasal mucosa and trachea, growth retardation, slight
anemia, and increased kidney weight.

Symptoms of chronic intoxication of acetaldehyde in humans

resemble those of alcoholism.

The RfC for acetaldehyde is 0.009 mg/m3 based on degeneration of

olfactory epithelium in rats.

EPA has medium confidence in the principal studies because

appropriate histopathology was performed on an adequate number of
animals and a no-observed-adverse-effect level (NOAEL) and a lowest-
observed-adverse-effect level (LOAEL) were identified, but the duration
was short and only one species was tested; low confidence in the database
due to the lack of chronic data establishing NOAELs and due to the lack of
reproductive and developmental toxicity data; and, consequently, low
confidence in the RfC.

EPA has not established an RfD for acetaldehyde

Reproductive/Developmental Effects

No information is available on the reproductive or developmental effects of

acetaldehyde in humans. Acetaldehyde has been shown, in animals, to cross
the placenta to the fetus.

75
 Appendix-A

Data from animal studies suggest that acetaldehyde may be a potential

developmental toxin. In one study, a high incidence of embryonic
resorptions was observed in mice injected with acetaldehyde. In rats exposed
to acetaldehyde by injection, skeletal malformations, reduced birth weight,
and increased postnatal mortality have been reported.

Cancer Risk

Human data regarding the carcinogenic effects of acetaldehyde are

inadequate. Only one epidemiology study is available that several limitations
including short duration, small number of subjects, and concurrent exposure
to other chemicals and cigarettes.

An increased incidence of nasal tumors in rats and laryngeal tumors in

hamsters has been observed following inhalation exposure to acetaldehyde.

EPA has classified acetaldehyde as a Group B2, probable human

carcinogen.

EPA uses mathematical models, based on human and animal studies,

to estimate the probability of a person developing cancer from breathing air
containing a specified concentration of a chemical. EPA calculated an
inhalation unit risk estimate of 2.2 H 10-6 (m g/m3)-1. EPA estimates that, if
an individual were to breathe air containing acetaldehyde at 0.5 m g/m3*
over his or her entire lifetime, that person would theoretically have no more
than a one-in-a-million increased chance of developing cancer as a direct
result of breathing air containing this chemical. Similarly, EPA estimates that
breathing air containing 5.0 m g/m3 would result in not greater than a one-

76
 Appendix-A

in-a-hundred thousand increased chance of developing cancer, and air

containing 50.0 m g/m3 would result in not greater than a one-in-ten
thousand increased chance of developing cancer.

EPA's Office of Air Quality Planning and Standards, for a hazard

ranking under Section 112(g) of the Clean Air Act Amendments, has ranked
acetaldehyde in the nonthreshold category. The 1/ED10 value is 0.033 per
(mg/kg)/d and this would place it in the low category under Superfund's
ranking for carcinogenic hazard.

ATMOSPHERIC PERSISTENCE

Acetaldehyde exists in the atmosphere in the gas phase. It also can be

formed in the atmosphere as a result of photochemical oxidation of organic
pollutants in urban atmospheres. The dominant atmospheric loss process for
acetaldehyde is by reaction with the hydroxyl radical. Based on this reaction,
the atmospheric half-life and lifetime is estimated to be 15 hours and 22
hours, respectively. The products of this reaction include formaldehyde and
peroxyacetyl nitrate (PAN).

77
 Appendix-A

CHAPTER-12

COST ESTIMATION

An acceptable plant design must present a process that is capable of

operating under conditions which will yield a profit.0^ Since, Net profit total
income-all expenses

It is essential that chemical engineer be aware of the many different

types of cost involved in manufacturing processes. Capital must be allocated
for direct plant expenses; such as those for raw materials, labor, and
equipment. Besides direct expenses, many other indirect expenses are
incurred, and these must be included if a complete analysis of the total cost
is to be obtained. Some examples of these indirect expenses are
administrative salaries, product distribution costs and cost for interplant
communication.

78
 Appendix-A

12.1 ESTIMATION OF EQUIPMENT COST

Equipment Cost (Rs.)

Vaporizer V-I 290436
Exchanger E-I 154427
Exchanger E-2 183702
Heater E-3 175501
Heater E-4 279200
Cooler E-5 193459
Pre-heater E-6 61770
Condenser E-7 70890
Condenser E-8 1283730
Re-boiler E-9 938765
Re-boiler E-10 1415840
Distillation Column D-1 7748874
Distillation Column D-2 11069820
Absorber A-1 7431117
Absorber A-2 9085370

12.2 ESTIMATION OF TOTAL CAPITAL INVESTMENT

Direct Cost (Rs)

Purchased equipment cost = Rs. 40382901

79
 Appendix-A

Purchased equipment installation = 0.47  40382901 = Rs. 18979963

Instrumentation & Process Control = 0.12  40382901 = Rs. 2277595
Piping (installed) = 0.66  40382901 = Rs. 26652714
Building (Including Services) = 0.18  40382901 = Rs. 7268922
Yard improvements = 0.1  40382901 = Rs. 4038290
Service facilities (installed) = 0.7  40382901 = Rs. 5088245
Land = 0.06  40382901 = Rs. 305294
Total direct plant cost = Rs. 104993924

Indirect Cost

Engg & Supervision = 0.33  40382901 = Rs. 13326357

Construction expenses = 0.41  40382901 = Rs. 16556989
Total Indirect Cost = Rs. 29883346
Total Direct & Indirect Cost = Rs. 134877270
Contractor’s fee = 0.05  134877270 = Rs. 6743863
Contingency = 0.1  134877270 = Rs. 13487727

Fixed Capital Investment = Total direct + indirect cost + contigency +

Contractor’s fee
= Rs. 155108860

Total Capital Investment = F.C.I + W.C.

Now
W.C = 0.15 (T.C.I)
= 0.15 (155108860 + W.C)
W.C = Rs. 27372151

80
 Appendix-A

T.C.I = 155108860 + 27372151

= Rs. 182481011

APPENDIX-A

81
 Appendix-A

A-1) DESIGN CALCULATIONS OF MULTI-TUBULAR

FIXED BED REACTOR

PRODUCT
CH3CHO = 412.8 Kg/hr
C2H5OH = 431.58 Kg/hr
H2O = 214.35 Kg/hr
O2 = 484.96 Kg/hr
N2 = 2090.8 Kg/hr

Cooling Water Out

Cooling Water in

FEED
C2H5OH = 863.26 Kg/hr
H2O = 45.44 Kg/hr
Volume of Reactor O2 = 635.28 Kg/hr
N2 = 2090.8 Kg/hr
Volumetric flow rate of feed to reactor = Vo = 63.84 m3/min

82
 Appendix-A

Space velocity = S = 15 min-1

as we know that
S = Vo/V where, V = Volume of reactor.
V = Vo/ S
= 63.84/15 = 4.256 m3

Weight of Catalyst

(Silver Catalyst on Alumina Support of size 1.25 mm is used)

volume of reactor = 4.256 m3
porosity = 0.4
so volume of catalyst = 0.6  4.256 = 2.5536 m3
particle Density of catalyst = 2250 Kg/m3
mass of catalyst = 2250  2.553 b
= 5746 Kg

Number of Tubes

Length of tube = 8 ft = 2.439 m

To calculate tube dia
As we know that to prevent deviation from plug flow assumption
Dt/Dp > 30
Where Dt = dia of tube
Dp = dia of particle
Let inside dia of tube = 2.204 in = 55.98 mm
Dt/Dp = 55.98/1.25 = 44.78 which is satisfactory
Volume of one tube = /4  Dt2  Lt

83
 Appendix-A

= 3.14/4  (55.98/1000)2  2.439

= 0.785  0.00313  2.439
= 0.006 m3
As total volume = 4.256 m3
So number of tubes required = 709 tubes

Diameter of Shell

To calculate shell dia eq. (from Ludwig)

 2π 
 D s - K1  4  K 2  - Pt  D s - K1  nK 3  K 4 
NT 
1.223 Pt  2

where NT = number of tubes = 709

Ds = shell dia = ?
PT = pitch = 1.25  0.1 of tube
= 1.25  2.5
= 3.125 in. (76.2 mm)
for this pitch
K1 = 1.08 K2 = - 0.9
K3 = 0.69 K4 = - 0.8
n = 1 ( 1 tube pass)
By solving above eq.
Ds = 104.72 in.
= 8.72 ft = 2.66 meter

Shell Height

Length of tube = 2.439 m

84
 Appendix-A

Leaving 20 % spacing above and below

So height of shell = 2 (0.2  2.439) + 2.439
= 3.415 m

Pressure Drop

ΔP  1    G   α1    μ 
     βG 
L   3  D P  f G   D P 

 = porosity = 0.4
DP = particle dia = 1.25 mm = 0.125 cm
Lf = feed density = 0.000948 g/cm3
G = mass velocity = 0.0579 g/cm2 Sec
 = viscosity of feed = 0.000343 g/cm. Sec
C1 = 981.46 cm/sec2
For smoth particles
α = 180 β = 1.8
L = length = 2.439 m = 243.9 cm
Putting values in above eq. gives
ΔP = 210.83 gm/cm2
And 1033.074 g/cm2 = 1 atm
So ΔP = 0.204 atm

Calculations of Heat Transfer Co-efficients

Shell Side
For water a simplified equation for heat transfer co-efficient

85
 Appendix-A

1501  0.011t b  V 0.8

ho 
 D 0.2
tb = average water temperature; oF
25  45
= = 35o C = 95o F
2

D = Diameter, in
4  flow area
Equivalent diameter = heated perimeter

Flow area =
4

π 2 2
Ds  N t Dot 
Ds = 104.72 in
Nt = 709
Dot = 2.5 in
Flow area = 5130 in2
Heated perimeter = Nt  Dot  
= 709  2.5  3.14
= 5565 in.
4  5130
De = 5565
= 3.68 in

Now to calculate V = velocity of water in fps

Mass velocity = G = W/as
W = flow rate of water = 2009.9 Kg/hr
= 44237 lb/hrs
flow area = as = 5130 in2 = 35.625 ft2
G = 44257/35.625 = 1242 lb/hr. ft2
Also G = V
 = density of water = 62.5 lb/ft3

so velocity V = G/ = 1242/62.5

86
 Appendix-A

= 19.87 ft/hr
= 0.00552 fps
1501  0.011  85 0.00552 0.8
so ho 
 3.68 0.2
= 3.691 Btu/ hr. ft2 oF

Tube Side
An equation proposed by LEVA to find heat transfer co-efficient
inside the tubes filled with catalyst particles.
0.7
h pd  dpG  dp
 3.5  e  4.6
k  μ  d

G = 420 lb/hr. ft2

 = 0.0829 lb/hr. ft
k = 0.0315 Btu/hr. ft oF
Dp = dia of particle = 0.0041 ft
D = dia of tube = 0.1836 ft
Putting values in above eq.
h p  0.1836 0.7
 0.0041  420 
 3.5 
0.0315  0.0829 

5.828 hp = 3.5 (8.36) (0.9023)

hp = 4.53 Btu/hr. ft2 oF
ID 4.53  2.204
hio = 4.53 4.53  = = Btu/hr. ft2
OD 2.5

Dirt Factor
Assume dirt factor = 0.003
Over all H.T. Coefficient
1 1 1
   RD
U D h io h o

87
 Appendix-A

1 1 1
   0.003
U D 4 3.691

= 0.5273
UD = 1.896 Btu hr. ft2
Area required for Heat Transfer
Q = 1519488 Btu/hr
LMTD = 515o C = 959CH
o 3CHO = 20.64 Kg/hr
F
C2H5OH = 17.1 Kg/hr
UD = 1.896 Btu/hr. ft2 O2 = 484.96 Kg/hr
θ N2 = 2090.82 Kg/hr
1519488
A=  = 835 ft2 = 77.67 m2
U D LMTD 1.896  959

Area Available for Heat Transfer

Length of tube = Lt = 2.439 m
H2O = 4064 Kg/hr
Outer Dia of tube = Dot = 0.0635 m CH3CHO = 20.43 Kg/hr
C2H5OH = 17 Kg/hr
Surface area of one tube = πDot L t
= 3.14  0.0635  2.439
= 0.486 m2

Total surface area available = 709  0.486

= 344.9 in2
so sufficient area is available for heat transfer.
A-2) DESIGN CALCULATIONS OF ABSORBER-A1
CH3CHO = 412.8 Kg/hr
C2H5OH = 431.58Kg/hr
O2 = 484.96 Kg/hr
N2 = 2090.82 Kg/hr
H2O = 214.35 Kg/hr

CH3CHO = 412.6 Kg/hr

C2H5OH = 414.48
88 Kg/hr
H2O = 4278.6 Kg/hr
 Appendix-A

89
 Appendix-A

We want to scrub 412.59Kg acetaldehyde and 431.48kg/hr ethyl

alcohol. This duty is done by two absorbers .In fist absorber 95% of
acetaldehyde is absorbed and about 99.96% of alcohol is absorbed.
The solvent used for this purpose is water.

Compositions of Components in Gas Mixture at Enterance

Components Kg Kg mol Mol %

CH3CHO 412.8 9.38 8.27
C2H5OH 431.58 9.38 8.27
H2O 85.35 4.78 4.18
O2 484.96 15.15 13.37
N2 2090.82 74.67 65.89
Total G = 3505 Gm = 113.32

Composition of Components in Liquid

Components Kg Kg mol Mol %

H2O 4064 225.7 0.996
CH3CHO 20.43 0.464 0.002
C2H5OH 17 0.37 0.0016
Total L = 4101.43 Lm = 226.534

Temperature of entering gas = 30 oC

Pressure = 1.1 atm
Average molecular weight of Gas = 3505/113.32
= 30.93 Kg/Kg-mol
G = PM/RT (where, R = 0.08205)
1.1  30.93
G = 0.08205  303
= 1.36 g/L = 1.36 Kg/m3

water = L = 997 Kg/m3 (at 25 oC)

90
 Appendix-A

Approximation of column dia

Approximate column dia from figure

Dia  1 meter = 3.28 ft
When the dia of column less than 3ft or near about 3ft use packed columns.
Because it is always economical to use packed column when the dia is about
1 m or less 1 m.

Selection of Packing

We have selected ceramic Intalox saddle.

Intalox saddle and pall rings are most popular choices. We have selected
ceramic intalox saddle because they are most efficient. We have selected the
ceramic material of packing because in our system oxygen and water are
present and they can cause corrosion and ceramic material will prevent
corrosion.

Size of the Packing

Now we will find the maximum size of intalox saddle which would be used
for this particular dia of the column.
1 D 1 1
Packing size =  = 0.0666 m = 66 mm
15 15

Although the efficiency of higher for small packings, it is generally

accept that it is economical to use these small sizes in an attempt to improve
the performance of a column. It is preferable to use the largest recommended
size of a particular type of packing and to increase the packed height to
compensate for small loss of efficiency.

91
 Appendix-A

Flooding Velocity

L ρG
G ρliquid

where,
L = 4101.43 Kg/hr
G = 3505 Kg/hr
L = 997 Kg/m3
. G = 1.36 Kg/m3
Let superficial velocity should be 60% of flooding velocity.
Superficial velocity = 0.6  2.36 = 1.416 m/sec
Note: This velocity is near the loading velocity.
Mass velocity of gas = density  velocity
= 6932.73 Kg/hr-m2
As flow rate of gas = 3505 Kg/hr
Mass velocity  flow rate of gas/cross sectional area
π 2
A= D = 3505/6932.74 = 0.5055-m2
4

D2 = 0.64
D = 0.80 m
This the actual diameter of column.
Number of Transfer Units (NOG)

y1 = mole fraction of acetaldehyde in entering gas = 0.0828

y2 = mole fraction of acetaldehyde in exit gas = 0.0052
As gas is dilute mixture of acetaldehyde.
So by Fig-25 of Appendix-B.

92
 Appendix-A

y1/y2 = 15.945
Gm
m =?
Lm

where m = slop of equilibrium curve and it is straight line because system is

dilute one.
Let m = 1.6
Gm 1.6  113 .3
m = = 0.8
Lm 226.24

where
Lm = optimum liquid flow rate. It has been optimized before the liquid
enters the 2nd column.
Gm
Optimum value for term m will lie between 0.7 to 0.8
Lm

So by using Fig.25
NOG = 7

Height of Packing(Z)

For ceramic intalox saddle:

 Gm  0.316
HOG = 1.14
 Lm  0.315
Where
Gm = gas flow rate, lb moles/hr. ft2
Lm = liquid flow rate, lbmol/hr.ft2
We have,
Gm = 113.3 Kgmol/hr
Since cross-section area = A = 0.502 m2
Gm = 113.3/0.502 Kg mol/m2hr = 225.69 Kgmol/m2hr
Similarly,

93
 Appendix-A

Lm = 226.24/0.502 Kgmol/m2hr = 450.67 Kgmol/hr. m2

Gm = 225.69 Kgmol/hr.m2
= 46.15 lbmol/hrft2
Similarly,
Lm = 92.15 lbmol/hr.ft2
 46.15 0.316
HOG = 1.14 
 92.15 0.315
HOG = 0.92 ft
Where
HOG = height of a transfer unit
Z = HOG  NOG
Z = 0.92  7 = 6.44 ft
Z = 1.96 m
Where Z is the height of packing.
Allow 2.0 ft for good liquid distribution through the packing from top.
Allowance for supports
= (2 ft)  (2 sections) = 4 ft
Total packing height required = Z = 6.44 + 2 + 4 = 12.44 ft
use 15 ft of packing.

Degree of wetting
Liquid rate
LP = Specific are of packing

Liquid rate = 2.27 m3/m2sec

And
Specific area of packing = 118 m2/m3
LP = 2.27  10-3/118 = 1.92  10-5 m3/m.sec

94
 Appendix-A

Pressure Drop

p = a.10b  g2F/  G
A, b = constants obtained from table 5-1.
p = pressure drop
 = liquid flow rate lb/ft2sec

gF = gas flow rate lb/ft2.sec

G = gas density lb/ft3
Note: Above equation is applicable for condition near the flooding.

The pressure drop is higher than the value predicted by equation given above
and account should be taken of this fart where appropriate.
From table for 2-in (50mm) ceramic intalox saddles.
A = 0.12
B = 0.1
L = 0.464 lb/sec ft2
Similarly,
gF = 0.39 lb/sec.ft2
 G = 0.084 lb/ft3

P = 0.12  100.10.464  (0.39)2 / 0.084

P = 0.24 in. of water/ft of packing.

To convert above P to S.I units by multiplying the value of P by the factor

83.3 to obtain the units of (mm/m)
P = 0.24  83.3
= 19.99  20

95
 Appendix-A

= 20 mm H2O/m. of packing.

TOP PRODUCT
CH3CHOH = 98.2 %
C2H5OH = 0.75 %
A-3)
FEEDDESIGN CALCULATIONS OF DISTILLATION
CH CHOH = 3.66 % H2O = 0.97 %
3
COLUMN (DC-1)
C2H5OH = 3.66 %
H2O = 92.69 %

BOTTOMS
96 C2H5OH = 3.77 %
H2O = 96.2 %
 Appendix-A

Process Design

Temperature of feed = 91o C

Temperature of top product = 20o C
Temperature of bottom product = 99o C
P = 1 atm

Minimum Reflux Ratio

Feed Top Bottom Relative

Component
F Xf D Xd W Xw Volatility 

97
 Appendix-A

CH3CHO 0.0366 0.982 0 10.87

C2H5OH 0.0366 0.0075 0.0377 2.27
H2O 0.9269 0.0097 0.962 1.00

Light key component = CH3CH2OH = B

Heavy key component = H2O = C
Lighter than light key component = CH3CHO = A
Using underwood equation
α A xfA α B xfB α C xfC
   1 q
αA  θ αB  θ αC  θ

As feed is at its bubble point so q = 1

Bt trial  = 3.5
Using eq. of min. reflux ratio,
α A xfA α B xfB α C xfC
   R m 1
αA  θ αB  θ αC  θ

putting all values Rm = 2.62

No. of plates at total reflux
Using Fenske’s equation


X
  
log  X d X 
X B

s 
C

Nm  1 
C B

log α BC  ave

Nm 
log  0.0097
0.0075  0.962  
0.0377
log2.27

Relative Volatility Method for Plate to Plate Calculations

Above feed plate:

Ln = RD = 3.5  9.5412 = 33.3942 Kg mol/hr

98
 Appendix-A

Vn = (R+1) D = 4.5  9.5412 = 429354 Kgmol/hr

Below feed plate:

Lm = Ln + F = 33.3942 + 256.4595 = 289.8537 Kgmol/hr
Vm = Lm – W = 289.8537 – 246.9015 = 42.9522 Kgmol/hr

Operating lines above feed point:

Ln D
ym  X n 1  xd
Vn Vn

yn CH3CHO = 0.7778 Xn+1 + 0.2806

yn C2H5OH = 0.7778 Xn+1 + 0.0021
yn H2O = 0.7778 Xn+1 + 0.0028
Operating lines below feed plate:

Lm W
ym  X m 1  Xw
Vm Vm

ym CH3CHO = 6.748 Xm+1

ym C2H5OH = 6.748 Xm+1 – 0.2167
ym H2O = 6.748 Xm+1 – 5.5269

Starting from top plate:

Xt = X1 =
Componen Xd = yt y1
t

yt
Yt/ Xt   Y1 Y1/ X1  α
y y
 t  1α
CH3CHO 10.8 0.782 0.90 0.8739 0.96 0.20 0.0794
C2H5OH 7 0.007 3 0.032 0 0.02 0.0680
H2O 2.27 5 0.01 0.0939 0.02 7 0.4282

99
 Appendix-A

1.00 0.009 7 7 0.17

7 0.00 0.07 0
9 5

Below feed
Y2 X2 X3 Y8
plate
0.342 ------ 0.0363 0 0
0.055 ------ 0.0361 ------ 0.0370
0.336 ------ 0.9258 ------ 0.963

No. of plates = 8
Rebioler acts as one plate, so actual
No. of trays = 7
Feed plate = 2 from bottom

Tray Efficiency:

20  96
Average temperature of column = = 58oC
2

Feed viscosity at average temperature = ave = 0.224 Cp

(relative volalitoly of key component)  ave = 2.27  0.224 = 0.509
from graph (17) of Appendix-B, overall efficiency of column = 60%
7
So, No. of actual trays = 0.6
= 12

2
location of feed point = 0.6
=3

Determination of the Column Diameter

Top Conditions Bottom Conditions

Ln = 33.394 Kgmol/hr Lm = 289.8537 Kgmol/hr

100
 Appendix-A

Vn = 42.9354 Kgmol/hr Vm = 42.9522 Kgmol/hr

Average mol. Wt. = 43.73 Kg/Kgmol Average mol. wt. = 19.05 Kg/Kgmol
T = 96o C
T = 20o C Liquid density = L = 0.99178 g/cm3
Liquid density = L = 0.78158
gm/cm3 Vapor density = V = 1.433  10-3
Vapour density = V = 3.56  10-3 gm/cm3
gm/cm3

Because liquid and vapour flow rates are greater at bottom so based upon
bottom flow rates.

Vapour load at bottom

Vm
QV  = 0.15861 m3/Sec
ρ V  3600

Liquid load at bottom

Lm
QL  = 1.542  10-3 m3/Sec
ρ L  3600

Tray Dynamic

i) Flow Parameter:
0.5 0.5
 L  ρ   289.8537  1.433  10-3 
FLV   m  v  =  


 = 0.2565
 Vm  ρ L   42.9522  0.99178 

ii) Capacity Parameter:

Assumed tray spacing = 12 in. = 30.48 Cm

From Fig (24) of Appendix-B, sieve tray flooding capacity,

101
 Appendix-A

Csb(20) = 0.028 m/Sec

Surface tension of system =  = 74.62 dynes/Cm
0.2
 
Corrected Csb = Csb(20)   = 0.0364 m/Sec
 20 
0.5
 ρ  ρV 
Now Unf = C bs  L  = 0.7361 m/Sec
 ρV 

iii) Tray Selection

We have selected single crossflow sieve tray with segmental down

comer. For this type of tray,
Down comer area = Ad = 0.12 AT
Weir length = Lw = 0.77 DT
Selected weir height = hw = 1 in. = 25.4 cm
Hole size (range 1/8“ to ½”) = 1/8” = 3.175 mm
Assumed tray spacing = 12 in.

iv) Tower Diameter

Let flooding = 53% (Correct trial)

F* = 0.53
Un* = Unf  F* = 0.390133 m/Sec
Un* = flooding velocity based upon net area.
Net area An = AT – Ad = 0.88 AT
An QV
AT = = 0.88U * = 0.461992 m2
0.88 n

π
AT = D2 = 0.461992 m2
4

D = 0.76715 m = 2.517 ft.

102
 Appendix-A

Selected D = 2.5 ft. = 0.761963 m

π
AT = D2 = 0.45576 m2
4

v) Flooding Check

QV QV
Un = A = 0.88A = 0.395467 m/Sec
n T

 Un 
Now F = F*  
U *
 n 

= 0.537
Now following information are available,
Tower area = AT = 0.45576 m2
Net area = An = 0.88 AT = 0.40107 m2
Active area = Aa = 0.76 AT = 0.34638 m2
Down comer area = Ad = 0.12 AT = 5.46912  10-2 m2
Hole area = Ah = 0.1 AT = 4.5576  10-2 m2

vi) Calculation of Entrainment

At FLV = 0.2565 and F = 53%

From Figure (23) of Appendix-B, fractional entrainment,
 = 0.0015
since  < 0.2, so now process is satisfactory
ψ
e = 1 - Lψ = 8.295 Kg/hr here, L = Lm  mol. wt.

vii) Tray Pressure Drop

a) Hole Velocity

103
 Appendix-A

QV 0.15861
Uh = A = 0.1 0.45576
h

Tray thickness = 3mm = 0.118 in. [for steel tray]

Hole dia = 1/8” = 3.175 mm
Tray thickness/Hole dia =0.9449
4.5576  10 2
Hole area / active area = = 0.1315
0.34638

 hole area 
Now gross % free area =    100% = 10 %
 tower area 

From Fig (20) of Appendix-B,

2
 1 
   1.8
 C vo 

Cvo = dry orifice co-efficient

2
 ρV  2  1 
Dry tray pressure drop = Pdry = 5.08   U h  
 ρ L   C vo 

= 0.288 cm
since  < 0.1, no need of correction factor.

b) Areated Liquid Drop, ha:

Q 
Fva =  V  h  = 0.01733
0.5
 Aa 

From figure (19) of Appendix-B, aeration factor of liquid on tray,

Qp = 0.8
Lw = 0.77 DT = 0.5867 m
So height of liquid on the weir,
0.67
 QL 
How = 6.66   = Hw = 1 in. = 2.54 cm
 LW 

ha = Qp (hw + how)

104
 Appendix-A

= 0.8 (2.54 + 12435)

= 2.13148 cm
ha = height of areated liquid drop

c) Total Pressure Drop:

PT = Pdry + ha = 0.288 + 2.13148 = 2.41948 cm

Estimation of Weep Point

L = 0.99178 gm/cm3 = 991.78 Kg/m3

 = 74.62 dynes/cm3 = 0.07462 J/N2
dh = 3.175 mm
ha = 4.16348
4.14  10 4 α
h = ρ Ld h
= 0.98106 cm

Now Pdry + h = 1.26906 cm

hw + how = 2.04896 inch
Hole area / active area = 0.1315
From figure (22) of Appendix-B, the point of intersection is above the
relevant line, so no weeping problem.

Down Commer Residence Time

Down comer velocity based upon clear liquid,

L
Vd = A dρ L

Here, L = Lm  mol. wt.

= 5.5917 Kg/hr

105
 Appendix-A

So, Vd = 0.02828 m/Sec, L = 991.78 Kg/m3

Tray spacing
Residence time = Vd
= 10.78 Sec

Which is greater than 3. so, satisfactory.

Calculation of Liquid Gradient

a) Height of Froth
hσ 0.98106
hf = 2Q p - 1 = 2(0.8) - 1
= 1.6351

b) Hydraulic Radius:
Rh = cross section / wetted perimeter
L w  DT
Df = = 0.676925 m
2
h f Df
So, Rh = 2h  100D = 0.02 m
f f

c) Velocity of aerated mass Uf:

for Fva = 0.01733,  = 0.59 [figure(19) of Appendix-B]
100Q L
Uf = h φD = 0.244394 m/sec
f f

d) Reynold’s modulus:
R h Uf ρL
Reh = μL

mix = 0.6442 Cp = 6.442  10-4 N.S/m2

L = 491.78 Kg/m3
Rh = 0.02 m
Uf = 0.244394 m/Sec

106
 Appendix-A

Reh = 7525

e) Friction factor:
f = 0.10 Fig (18) of Appendix-B

f) Calculation of gradient ():

100fU f2 L w
= g  9.81m/Sec 2
R hg

= 0.14137 cm
Now Pdry = 0.288 cm
1/2 Pdry = 0.144 cm
Because  < ½ Pdry
Its is satisfactory

g) Height of aerated mass in down comer:

Assuming a try clearance 38 mm. between down comer apron. And
the try.
hda = 13.1 (QL/Ada)2
= 13.1 (1.542  10-3/0.022294)2
hda = 0.06267 [Ada = Lw  clearance in m]
So height of liquid in down comer,
hdc = PT + hw + how +  + hda
= 2.41 + 2.54 + 0.12435 + 0.14137 + 0.06267
= 5.28779 cm
height of aerated liquid = hdc/Qp = 6.609738 cm
Tray spacing = 12” = 30.48 cm
½ Tray spacing = 15.24 cm

107
 Appendix-A

half of tray spacing > hdc/Qp

so process is satisfactory.

Mechanical Design
1) Shell Thickness
Material of construction = Stainless steel 316
Operating Pressure = 14.7 Psi
Design Pressure = 25 Psi
Shell thickness is given by
PD
tm  C
2fJ  P

Where f = max – allowable working stress = 18700 Psi

J = weld efficiency factor (max) = 0.8
C = corrosion factor = 0.002 in./year
For 25 year life C = 0.002  25 = 0.05 in
Period = 25 year, D = 2.5 ft = 30 in
25  30
tm   0.05 = 0.0525 in
2 0.8 1.8700   25

for each 20 ft height 1/16” is added

tm = 0.0525 + 1/16 = 0.11 in = 3 mm

Tray Specifications

Total area for holes

Total no. of holes = Area of one hole

0.045576  100  2
=
0.01265625   2.54  2

= 5582

108
 Appendix-A

5582/  2.54  2
No. of holes/in2 of tray = = 10
0.34638

Now from graph Fig (21) of Appendix-B,

Pitch = 2.0  3.175 = 8.89 mm

Height of Distillation Column

No. of plates = 12
Tray spacing 1 ft
Distance between 12 plates = 12 ft
Top clearance = 1 ft
Bottom clearance = 1 ft
Tray thickness = 3 mm/plate = 0.00983 ft/plate
0.118  12
Total thickness of trays = = 0.118 ft
12

Total height of column = 11 + 1 + 1 + 0.118

= 13.118 ft
= 3.998 ft
= 4 ft

NOMENCLATURE OF DISTILLATION COLUMN

Aa = Active area (m2)

Ad = down comer area (m2)
Ah = hole area (m2)
An = Net area (m2)
AT = total area (m2)
Ada = area under down comer apron (m2)

109
 Appendix-A

C = corrosion allowance (in/year)

Csb(20) = capacity parameter for liquids ( = 20 dynes/cm)
Csb = Capacity parameter of liquid
D = Diameter of tower (m)
Df = flow width normal to liquid flow (m)
Dh = hole diameter (m)
e = total entrainment (Kg/sec)
F = feed (Kgmol/hr)
F* = Design % loading
HF = Enthalpy of feed (J/Kgmol K)
HB(l) = Enthalpy of bottom (J/Kgmol K)
HD(L) = Enthlpy of the distillate (J/Kgmol K)
ha = head loss due to created liquid (cm)
hf = froth height on tray (cm)
had = had loss due to down comer apron (cm)
hdc = height of clear liquid in down comer (cm)
hw = weir height (cm)
how = height of liquid crest over weir (cm)
ho = head loss due to bubble formation (cm)
J = weld efficiency factor
L = liquid flow rate (Kg/hr)
Lw = weir length (m)
Nm = min. no. of plates
P = period (years)
Pdry = dry pressure drop (cm)
PT = total pressure drop (cm)

110
 Appendix-A

QL = Liquid flow rate (Kg/m3)

Qv = Vapour flow rate (Kg/ m3)
Qc = condenser duty (J/ m3)
QR = Rebotr duty (J/hr)
QP = Areatio factor
Rh = Hydraluic radius of aerated mass (m)
Reh = Modified Reynold No.
Rm = Min. reflux ration
R = operational reflux ratio
Tm = thickness of shell (mm)
Uh = vapour velocity through holes (m/sec)
Vm = vapour flow rate at bottom (Kgmol/hr)
WF = mass flow rate of feed (Kgmol/hr)
WB() = bottoms (Kg/hr)
W D() = mass flow rate distillate (Kg/hr)
Unf = flooding velocity based upon net area (m/sec)
Vd = down comer liquid velocity (m/sec)
 = relative volatility
L = density of liquid (Kg/m3)
v = density of vapor (Kg/m3)
average = average viscosity of feed (Cp)
 = fractional entrainment factor
 = relative froth density
 = surface tension (J/N2)
 = liquid gradient

111
 Appendix-A

A-4) DESIGN CALCULATIONS OF VAPORIZER

966.7 lb/hr
Steam 266o F
266o F

233.6o F 150.8o F
2501 lb/hr
Alcohol

Heat Duty
Qt = Q1 + Q2
1)=> Preheating 2)=> Vaporization
Q1 = mCpT
= 1135.8  0.87 (112-66)
= 45454.7 Kmol/hr = 180.375.8 Btu/hr
Q2 = Qalcohol + QH2O
Latent heat of vaporization of H2O = 185.32 Kcal/Kg
Latent heat of vaporization of alcohol = 500 Kcal/Kg
Q2 = 863.2 + 45.43 + 500
Q2 = 182685 Kcal/hr = 724942.5 Btu/hr
Qt = Q1 + Q2

112
 Appendix-A

= 228140.2 Kcal/hr
= 905318.7 Btu/hr

FOR PREHEATING ZONE

For steam T1 = 130o C = 266 oF

T2 = 130o C = 266 oF
For process fluid,
T1 = 66o C = 150.8 oF
T2 = 112o C = 233.6 oF
t1 = LMTD
 266  233.6    266  50.8
=  266  233.6 
ln 
 266  150.8 

= 65.27 oF

For Vaporization Zone

t2 = 266 – 233.6 = 32.4 oF

Qt
t, weighted = Q Q2
1

Δt 1
 Δt
2

905318.3
t, w = 180375.8
 724942.5
65.28 32.4

t, w = 36 oF

113
 Appendix-A

assume UD = 95 Btu/hr. oF. ft2

as Qt = UD A t, w
905318.3
A = 95  36

= 264.71 ft2

Exchange Layout

1-2, shell & tube heat exchanger

¾OD, 1 sq. pitch,
A = at  Nt  Lt
A = 0.1963 ft
Lt = 8 ft.
at = 0.1963
A = 0.1963  8  Nt
264.7
Nt = 0.1963  8
= 168

Nt = 166 (Nearest count)

So
A = 260.68 ft2
UD = 96 Btu/hr. ft2. oF

SPECIFICATIONS

Shell Side Tube Side

17 ¼, C = 0.25” ¾ OD, 1 sqr. Pitch
B = 4 in 16. BWG

114
 Appendix-A

Calculations (Tube Side)

0.302  166
at = = 0.174 ft2
144  2

Ft = m/at = 966.7/0.174 = 5555.74 lbm/hr. ft2

D = (I.D)Tube/2 = 0.62/12 = 0.052 ft
R,t = DGt/
t T = 130o C = 266 oF
 = 0.014 Cp = 0.03388 lb/ft hr
0.052  5555.74
Re,t = 0.03388
= 852.7

For condensing steam,

hio = 1500 Btu/hr. ft2 oF

Shell Side Calculations

I.D  CB
as = 144Pt

17.25  0.25  4
= = 0.119 ft2
144  1

Gs = m/as = 2501.76/0.119 = 21023 lb/hr ft2

Res = De Gs/
De = 0.95/12 = 0.079167 ft
 (for liquid) = 0.25 Cp
 = 0.25  2.42 = 0.604 lb/hr. ft
0.079167  21023
Re,s = 0.604
= 2745

JH = 29
ho = JH (K/De)(C/K)1/3
= 78 Btu/hr.ft2 oF

115
 Appendix-A

U1 = hioho/ho + hio
U1 = 74 Btu/hr.ft2 oF
Q1
A1 = U t
1 1

= 37 ft2
For vaporization zone
(at 112o C for vaps) = 0.012 Cp
= 0.012  2.42 = 0.029 lb/hr. ft
0.079  21023
Re,s = DeGs/ = 0.029

Re,s = 57269
JH = 140
ho = JH(K/De)(c/K)1/3
= 141.8 Btu/hr.ft2 oF
h io  ho
U2 =
h io  ho

=129.5 Btu hr. ft2 oF

Clean surface required for vaporization
A2 = Q2/U2(t)2
A2 = 172.78 ft2
Total clean surface required
Ac = A1 + A2
= 37 + 172.78
Ac = 209.78 ft2

Weighted clean overall co-efficient

U1A1  U 2A 2
Uc,w = A1  A 2

116
 Appendix-A

= 119 Btu/hr. ft2 oF

Rd = 0.003
1/UD = 1/UC + Rd
UD = 88 Btu/hr ft2 oF (Correct)
PRESSURE DROP CALCULATIONS

Tube side Pressure Drop

At Re,t = 8527
f = 0.00028
Specific volume of steam at 39 Psi
 = 10.854 ft3/lb
1
s=
10.854 ftlb  62.5 ftlb
3

s = 0.00147
Gt = 5555.7 lb/hr. ft2
fG 2tL n
Pt = 1/2
5.22  1010  0.052  0.00147  1

100028   5555374  2  8  2
= 1/2 
5.22  1010  0.052  0.00147  1

Pt = 0.035 Psi

Shell Side Pressure Drop

For preheating zone

At Re,s = 2745 f = 0.0027
1 A
Length of preheating zone = LP = L t  A
c

= 1.41 ft

117
 Appendix-A

12  1.4
No. of crosses, (N + 1) = 8

= 4.2
s = 0.81
Ds = 17.25/12 = 1.44 ft
f G s2 D3  N  1
Ps1 =
5.22  1010  s  s

Ps1 = 0.22 Psi

For vaporization zone
At Re’,s = 57269 f = 0.0018
2 A
Length of vaporization zone) = Lv = L t  A
c

= 6.6 ft
Lv
No. of crosses, (N+1)’ = 12 
B
= 19.74
outlet liquid = 0.81  62.5 = 50.625
44.1  42.3
outlet varps = PM/RT = 10.73  693.6

= 0.25
1135.8
soutlet mix = 62.5
908.7  227.1
0.25 50.625
= 0.005
0.81  0.005
smean =  N  1 2 = 0.4

fG s2 Ds N  1 2
Ps2 =
5.22  1010  De  s  1

= 1.08 Psi

118
 Appendix-A

Ps = Ps1 + Ps2

Ps = 1.3 psi
A-5) DESIGNING CALCULATIONS OF PRE-HEATER-E6

Design Calculations

T2=240 oF T1=240 oF

t1=122 oF t2=195.8 oF

Inlet temperature of the process stream = t1 = 122 oF

Outlet temperature of the process stream = t2 = 195.8 oF
Inlet temperature of steam = T1 = 240 oF
Outlet temperature of steam = T2 = 240 oF
Mass flow rate of process stream = m = 11281.45 lb/hr
Specific heat capacity of the process stream = Cp = 0.943 Btu/lb oF

Heat load
Q  mC p T

Q  11281 .45 x 0.943 x 78.3

Q  785114 .46 Btu

hr

Mass flow rate of steam

119
 Appendix-A

Q
m


785114 .46
m
952.1

m  860.33 lb
hr

LMTD

(T1  t 2 )  (T2  t1 )
Tm 
(T  t )
ln 1 2
(T2  t1 )

(240  195.8)  (240  122)

Tm 
(240  195.8)
ln
(240  122)

Tm  75.72 o F

Since steam is condensing medium therefore R = 0 and FT = 1 so

Tm  t

Assumed calculations

Value of UD assumed

U D  195 Btu
hrft 2 o F

Heat transfer area

Q
A
U D t

120
 Appendix-A

785114 .46
A
195 x75.72

A  53.17 ft 2
Now, let’s take
Tube length = 6ft
Tube O.D. = ¾ in
Area of one tube = πDL = 1.178 ft2
No. of tubes = 46 tubes
From tube count table
For 50 tubes shell I.D. = 10 in for one pass
Pitch = PT = 1.25 x ¾ = 0.937 in
Baffle spacing = B = 5 in Clearance = 0.187 in

Shell Side Calculations

Flow area

IDxC ' B
as 
144 PT

10 x0.187 x5
as 
144 x0.937

a s  0.052 ft 2

Mass velocity

W
Gs 
as

11281 .45
Gs 
0.052

121
 Appendix-A

G s  216951.52 lb
hrft 2

Reynolds No.

DeGs
Re 


0.046 x 216951.92
Re 
1.2

Re  8316.49

Value of JH from shell side heat transfer curve

JH = 55

Thermal conductivity

k = k1x1 + k2x2 + ………….. + knxn

k = 0.36 Btu/hrft2 (oF/ft)

Shell side coefficient

1
ho k  Cp  3
 JH  
o De  k 
1
ho 0.36  0.943 x1.2  3
 55  
o 0.046  0.36 

ho
 632.74 Btu
o hrft 2 o F

for coefficient correction

wall temperature

122
 Appendix-A

hio
tw  ta  (t a  Ta )
hio  hi

t w  215.94 o F
at wall temperature

 w  0.6354 lb fthr

0.14
  
s     1.089
 w 

corrected coefficient

ho
ho  s
o

ho  688.92 Btu
hrft 2 o F

TUBE SIDE CALCULATIONS

Flow area

at '  0.302in

N t at '
as 
144n

50 x0.302
as 
144 x 2

a s  0.046 ft 2

Mass velocity

W
Gt 
at

123
 Appendix-A

860.33
Gt 
0.046

Gt  18702.82 lb
hrft 2

Reynolds No.
D Gt
Re 


0.0517 x18702.82
Re 
0.029

Re  33342.61

for steam

hio  1500 Btu

hrft 2o F

Clean overall coefficient

hio ho
UC 
hio  ho

1500 x688.92
UC 
1500  688.92

U C  472.09 Btu
hrft 2 o F

Design overall coefficient

1 1
  Rd
UD UC

1 1
  0.003
UD 462.09

124
 Appendix-A

U D  202 Btu
hrft 2 o F

Pressure drop (Shell side)

for Re = 8316.49
friction factor for shell side = f = 0.0025
No. of crosses , N+1 = 12L/B = 14.4 = 15

2
fG s D s ( N  1)
Ps 
5.22 x1010 De s s

0.0025 x 216951.92 2 x0.833x15

Ps 
5.22 x1010 x0.046 x0.89 x1.085

Ps  0.6 psi

Pressure drop (Tube side)

for Re = 33342.61
friction factor for tube side = f = 0.00018
2
1 fG t Ln
Ps 
2 5.22 x1010 Ds t

1 0.00018 x18702.82 2 x6 x 2
Ps 
2 5.22 x1010 x0.0517 x 0.00098 x1.0

Ps  0.2 psi

125
 Appendix-A

A-6) DESIGN CALCULATIONS OF CONDENSER

T2 = 178 oF T1 = 180 oF

t1 = 77 oF t2 = 113 oF

Inlet temperature of the process stream = T1 = 180 oF

Outlet temperature of the process stream = T2 = 178 oF
Inlet temperature of the water = t1 = 77 oF
Outlet temperature of the water = t2 = 113 oF
Mass flow rate of the process stream = m = 22267.8 lb/hr
Enthalapy of saturated vapor (95% Ethanol) = Hv = 500 Btu/lb
Enthalapy of saturated liquid (95% Ethanol) = Hl = 98 Btu/lb

Heat Load
Q = m(Hv – Hl)
Q = 22267.8  (500 – 98)
Q = 8951684.54 Btu/hr

126
 Appendix-A

Mass flow rate of cooling water

Q
m
C pΔt

127
 Appendix-A

8951684.54
= 1  36

= 248657.5 lb/hr

LMTD

Tm 
 T1 - t 2  -  T2 - t1 
T - t 
ln 1 2
 T2 - t1 
Tm 
180 - 113t 2  - 178 - 77 
ln
180 - 113 
178 - 77 
= 81 oF
Since process is condensing therefore R=0 and FT = 1 so, Tm  t

Assumed Calculations

Value of UD Assumed
UD = 100 Btu/hr.ft2 oF

Heat Transfer Area

Q
A
U DΔt

8951684.54
A
100  81

= 1105 ft2
Assume 4 passes
Now, lets take
Tube length = 10 ft
Configuration is 2 shell side passes and 4 tube side passes

128
 Appendix-A

Tube O.D. = ¾ in.

Area of one tube = DL = 2.35 ft2
No. of tubes = 1105/2.35 = 470
From tube count table
For 468 tube shell I.D. = 25 in for one pass
Pitch = PT = 1.25  ¼ = 0.937 in.
Baffle spacing = B = 20 in
Clearance = 0.187 in
Then
Corrected A = 1099 ft2
Corrected UD = 100.5 Btu/hr.ft2 oF

Shell Side Calculations

Flow Area
ID  CB
as 
144Pr

25  187  20
= as 
144  937

= 0.692 ft2

Mass Velocity
W
Gs 
as

129
 Appendix-A

22267.8
= Gs 
0.692

= 32177.74 lb/hr ft2

Loading
W
G 
LN1/3
t

22267.8
G 
10   466  2 / 3

= 37.09
Assumption
h = ho = 200
hio = 909.33 Btu/hr.ft2 oF
h
= h  t a  h  h  Tv  t a 
io
tw
io i

= 110 oF

Film Temperature
Ta  t w
Tf =
2

Physical Properties at tf

Thermal conductivity kf = 0.116 Btu/hr-ft-oF

Specific gravity sf = 081 lb/hr-ft
Viscosity f = 1.45 lb/hr-ft
From Figure(6) of Appendix,
h = ho calculated = 200 Btu/hr-ft2-oF

130
 Appendix-A

Tube Side Calculations

Flow Area
at = 302 in.
at = Ntat/144a
468  0.302
a t =
144  4

= 0.245 ft2

Mass Velocity
Gt = W/at
Gt = 248657/0.245
= 1014926 lb/hr-ft2

Water Velocity
V = Gt / 3600
= 1014926 / 7600  62.5 = 4.512 ft/sec
At ta = 95 oF
 = 1.7 lb/ft-hr
I.D of tube = 0.62/12 = 0.0517 ft

Reynold No.
Ret = DGt/
= 0.0517  1014926.5 / 1.7 = Ret = 30865

from figure of (Kerm) hi = 1100 Btu/hr-ft2-oF

I.D
hio = hi  O.D
= 909.33 hr-ft2-oF

131
 Appendix-A

Clean Overall Coefficient

h io h o
UC 
h io  h o
909.33  200
UC 
909.33  200

= 163.94 Btu/hr-ft2 oF

Design Overall Coefficient Calculated

Allowable dirt factor Rd = 0.003

1
UD   Rd
UC

= 1/150 + 0.003
= 109.89 Btu/hr-ft2-oF

Pressure Drop (Shell Side)

Reynolds No.

At T = 180 oF
ap = 0.01  2.42 = 0.0242
De = 0.55/12 = 0.0458 ft2
Res = DeGs/
= 0.0458  32177.74/0.0242
= 60898
For Res = 60898
Friction factor for shell side f = 0.0015
No. of crosses, N + 1 = 1210/20 = 6

132
 Appendix-A

Density = f = 0.085 (by using ideal ged equation)

S = specific gravity = 0.085/82.5 = 0.0012
fG s2Ds  N  1
Ps 
5.22  1010 Dess

0.0015 32177.74 2  2.08  6

=
5.22  1010  0.0458  0.0013

= 3.12 psi

Pressure Drop (Tube Side)

Reynolds No.
Ret = DG/
= 144930/1.7
= 20865
for Ret = 30865
Friction factor for tube side f = 0.00021 ft2/in.
fG 2t Ln
Pt 
5.22  1010 Ds t

0.00021 11014930  2  10  4
=
5.22  1010  1  1

= 2.0 psi
Pr = 440.12 / 1 = 0.12 psi
PT  Pt  Pr = 2.8 + 1.98 = 4.72 psi

REFERENCES

133
 Appendix-A

1) Ludwig, E.E, “Applied Process Design”, 3rd ed, vol.

2, Gulf Professional Publishers, 2002.

2) Ludwig, E.E, “Applied Process Design”, 3rd ed, vol.

3, Gulf Professional Publishers, 2002.

3) McKetta, J. J., “Encyclopedia of Chemical

Processing and Design”, Executive ed, vol. 1, Marcel Dekker Inc,
New York, 1976.

4) Kuppan, T., “Heat Exchanger Design Hand Book,

Marcel Dekker Inc., New York, 2000.

5) Levenspiel, O., “Chemical Reaction Engineering:,

2nd ed, John Wiley and Sons Inc., 1972.

6) Peters, M.S. and Timmerhaus, K.D., “Plant Design

and Economics for Chemical Engineering”, Fourth ed, McGraw Hill,
1991.

7) Rase, H.F., “Fixed Bed Reactor Design and

Diagnostics, Butterworth Publishers, 1990.

8) Thomas, J. M., and Thomas, W.T., “Introduction to

the Principles of Heterogeneous Catalysis, Acedenic Press, 1967.

9) Bockhurst, J.F. and Harker, J.H, “Process Plant

Design”, Heinemann Educational Books Ltd, 1973.

10) Coulson, J.m., and Richardson, J.F., “Chemical

Engineering”, 4th ed, Vol.2, Butterworth Heminann, 1991.

134
 Appendix-A

11) Peacock, D.G., “Coulson & Richardson’s Chemical

Engineering”, 3rd ed, vol, Butterworth Heinenann, 1994.

12) Sinnot, R.K., “Coulson and Richardson’s Chemical

Engineering”, 2nd ed, vol 6, Butterword Heinemann, 1993.

13) Kern, D.Q., “Process Heat Transfer”, McGraw Hill

Inc., 2000.

14) McCabe, W.L, “Unit Operations of Chemical

Engineering”, 5th Ed, McGraw Hill, Inc, 1993.

15) Perry, R.H and D.W. Green (eds): Perry’s Chemical

Engineering Handbook, 7th edition, McGraw Hill New York, 1997.

16) www.nist.com

17) www.uspto.gov

18) www.haverstandard.com

135