Plant Design of MIBK

Table of Contents
1.INTRODUCTION ............................................................................................................................1
1.1PHYSICAL PROPERTIES ........................................................................................................1
1.2USES...........................................................................................................................................2
2. MANUFACTURING PROCESS ....................................................................................................4
2.1 PROCESS SELECTION ...........................................................................................................4
2.2 OVERALL PROCESS DESCRIPTION ...................................................................................6
3. MATERIAL BALANCE .................................................................................................................9
4. ENERGY BALANCE ...................................................................................................................16
5. EQUIPMENT DEIGN ...................................................................................................................31
5.1 LIST OF ITEMS TO BE REPORTED ....................................................................................31
5.2 AVAILABLE INFORMATION .............................................................................................31
5.3 ADDITIONAL INFORMATION ...........................................................................................31
5.4 DESIGN METHODOLOGY...................................................................................................35
5.5 DESIGN COMPUTATION (PROCESS)................................................................................41
5.6 DESIGN METHEDOLOGY (MECHANICAL) .....................................................................46
5.7 DESIGN COMPUTATIONAL (MECHANICAL) .................................................................50
6. DESIGN DATA SHEET ...............................................................................................................55
7. NOMENCLEATURE ....................................................................................................................56
8. REFERENCES ..............................................................................................................................58
0
1.INTRODUCTION
Methyl isobutyl ketone (MIBK) (CAS no. 108-10-1), also known as 4-methyl-2-pentanone,
(chemical formula C6H12O) is a chemically stable compound possessing a bland, ketonic odor and
used generally as a solvent. The structure of MIBK is as follows.
It is by far the most important of all the acetone derivative solvents. In terms of production volume
MIBK lies behind acetone and 2-butanone. The total produced amount of MIBK in world in 1987
is 1,80,000 ton and in 1996 3,80,000 ton [1]. MIBK is a medium evaporating solvent. This higher
ketone homolog of acetone methyl ethyl ketone is miscible with most organic solvents. MIBK also
exhibits strong solvency for many natural and synthetic resins, gums, waxes, oils, cellulose esters
and other coating systems. Water solubility of MIBK is not good compare to other ketone solvents
like acetone and MEK (methyl ethyl ketone). This property makes MIBK an useful liquid-liquid
extraction solvent.
1.1PHYSICAL PROPERTIES
MIBK is a colorless liquid with a less pronounced ketone like odor. Some physical properties are given
below.
Melting point -80 0C
Boiling point 116 0C
Density₄20 0.8004
nD20 1.3959
Enthalpy of evaporation 36.15 kJ/mol
Specific heat (20 0C) 1922 kJ/g
Enthalpy of combustion 3740 kJ/mol
Flash point (DIN 51 755) 14 0C
Ignition temperature 475 0C
Ignition class (VED) G1
Explosion class (VED) 1
Solubility at 25 0C MIBK in water Water in MIBK 1.7 wt.% 1.9 wt.%
MIBK is poorly soluble in water but is miscible with common organic solvents. It forms an
azeotrope with water and a large number of solvents. For example, the azeotrope with water (bp
87.9 0C) contains 75.7 wt.% and that with n-butanol (bp 114.4 0C) 70 wt.% MIBK.
1
MIBK undergoes auto-oxidation to form peroxide. After evaporation of MIBK-water mixture in
presence of air, a dangerous, increasing concentration of peroxide in the aqueous phase has been
reported [1].
In condensation reactions with carbonyl compounds, the α-methyl group usually reacts. Only
formaldehyde is able to undergo condensation reactions with the α-methylene group. The industrial
reactions such as hydrogenation and reductive amination may be carried out with the keto group.
1.2USES
More than 60% of the MIBK produced in the United States is used as a protective coating solvent.
Significant volumes are also used in the manufacture of rubber anti-ozonates, in rare metal
extraction, as a solvent for pesticides, in adhesives and pharmaceuticals and as a denaturant for
ethyl alcohol. A profile of MIBK used in the United States in 1980 is given in Table 1 [4].
Table 1. MIBK uses in United States in 1980
Use Percentage
Surface coatings (industrial, lacquers) 68
Rubber anti-ozonates 8
Rare metal extraction 8
miscellaneous 6
Export 10
Total 100
Surface Coating:
In surface coatings, MIBK is often used as the medium-boiling component of nitrocellulose lacquer
solvent blends. It is frequently blended with cheaper aromatic solvents to achieve blended active
solvent characteristics in high solid lacquers.
Due to its strong solvency and low density, MIBK finds application in the higher-solid coating
systems. MIBK has demonstrated that it can be successfully used in high solids acrylic,
acrylic/urethane polyesters, and oil-modified polyesters formulations. These high-solids coatings
are required in many applications where EPA air quality regulations limit the maximum weight of
organic solvent per unit volume of coating. Because of its strong solvency, MIBK can be used to
increase solids content of the coating solution while maintaining desirable viscosity characteristics.
A further use is as a solvent for dyes in printing industry.
Rare Metal Extraction:
A rapidly growing field of application for MIBK is in the recovery, separation and purification of
rare transition elements, usually as their complexes. Typical applications include zirconium from
hafnium for nuclear reactors, tantalum from niobium for electronics and nuclear applications,
tungsten from molybdenum, and uranium from thorium.
2
Others:
A derivative of MIBK, n-(1,3-dimethylbutyl)-n-phenyl-p-phenylenediamine is used as an
antioxidant for rubber. Miscellaneous end uses for MIBK include pharmaceuticals, where it is used
by major antibiotic producers in the extraction and purification of penicillin from the fermentation
broth, in adhesive formulations based on nitrile rubber and acrylics, and in pesticides, in the
removal of paraffins from mineral oil, for the production of lubricating oils where it is used as a
solvent for active ingredients. The importance of MIBK as an intermediate for synthesis is
relatively low. The most important product is 4-methyl-2-pentanone obtained by hydrogenation of
ketone. It has some importance as a polymerization initiator for ethylene and for handling of
unsaturated polyester resins [1].
3. STORAGE AND TRANSPORTATION
MIBK is available with a purity of >99%. Typical specification is given below
Content >99 wt.%
Water content (ASTM D 1364) 0.1 % max.
Hazen colour no. (APHA, DIN 53 409) 10 max.
Nonvolatile residue (ASTM D 1353) 0.002 wt.% max.
Boiling range (DIN 51 751) 114-117 0C
Acid content (as acetic acid) 0.002 wt.% max.
Conditions that could lead to auto-oxidation (presence of air, light, heat or heavy metals) or
condensation (strongly acidic or basic media) should be avoided during storage. Containers of V2A
steel are recommended for both storage and transportation. Hazard codes for transportation are as
follows:
IMDG code: class 3.2
RID/ADR: class 3, number 3 b
CFR 49: 172.101 flammable liquid
UN number: 1245
3
2. MANUFACTURING PROCESS
There are several commercial processes discussed in the literature for the manufacture of MIBK
from acetone. These include:
i. Low temperature condensation of acetone in the presence of a base catalyst in the liquid phase to
yield di-acetone alcohol (DAA) followed by dehydration of the DAA to mesityle oxide (MO) in the
presence of acid catalyst. MO is then hydrogenated to MIBK in the presence of a nickel catalyst
[2].
ii. Higher temperature condensation of acetone in the liquid phase in the presence of either a basic
or acid catalyst directly to MO followed by hydrogenation to MIBK. Isophorone is a by-product of
this reaction [3,4]. This process is of commercial significance only if Isophorone is recovered as a
co-product since MO yields are lower than low temperature condensation process. Catalyst such as
copper chr..omite[1]or zirconium phosphate [1]is used for condensation, and palladium on
aluminum oxide for the hydrogenation.
iii.Vapour phase condensation of acetone and hydrogen in the presence of a catalyst to directly
form either MO or MIBK [5].
iv. Direct liquid phase condensation-dehydration-hydrogenation of acetone in the presence of
hydrogen using a bi-functional catalyst to form MIBK. For this process a combination of a cation
exchanger with palladium is generally used as a catalyst [1]. The acetone is fed with hydrogen over
the palladium charged catalyst at 1300C and 0.5-5.0 MPa. A selectivity of >95% at a conversion of
< 50% is thereby attained. As a result of the increasing production of acetone by dehydrogenation
of isopropyl alcohol, the production of 4-methyl-2-pentanone as a byproduct in this process is
becoming more important [1].
2.1 PROCESS SELECTION
The low temperature condensation of acetone route and the direct liquid phase condensation-
dehydration-hydrogenation processes are of commercial significance. Several advantages are
clamed for the one step MIBK synthesis including:
1. Proton catalysis and metal catalysis with one specific resin.
2. The thr..ee steps of condensation, dehydration and hydrogenation all takes place at the same
time.
3. High conversion rate of acetone because MO is removed from the equilibrium.
4. No need for additional separate hydrogenation unit.
But this one step synthesis of MIBK is relatively latest technology and most of the advancement of
the process is copyright protected. The process description of this process is not usually available in
literature. On the other hand the low temperature condensation route is the oldest process for
4
manufacturing MIBK. Most of the plants in world producing MIBK follow this route. That’s why
the low temperature condensation of acetone route is selected for the plant design purpose and
reaction chemistry is discussed in further details.
MIBK Via Low Temperature Condensation Of Acetone
As said earlier, thr..ee distinguished steps are involved in this route of MIBK manufacture, viz.
condensation, dehydration and hydrogenation. These steps are discussed below in detail.
Condensation of Acetone to DAA:
The production of diacetone alcohol (DAA) by acetone condensation at low temperature is
expressed by the following chemical equation. This is a base catalyzed aldol condensation reaction.
⇔ ( ) ( )
Acetone DAA
The industrial production of DAA takes place in the liquid phase using an alkaline catalyst. Water
inhibits the condensation reaction, so it is advantageous to use acetone containing not more than 0.5
wt.% water [6]. According to a Shell patent [7], solid catalysts, e.g., Ba(OH)2 or Ca(OH)2 ,
impregnated on a suitable carrier, are used in a fixed bed reactors the condensing agent. Dilute
NaOH can also be used as catalyst in a well-mixed reactor. When dilute catalyst are employed, they
must be removed from the reactor product or neutralized prior to recovery of the DAA.
The reaction of acetone to DAA is equilibrium controlled. Increasing the temperature decreases the
equilibrium concentration of DAA [2]. Temperatures of 10-30 0C are used commercially and at 20
0C the yield of DAA is about 6 mol/1000 mol catalyst/h using the solid catalyst system. When
using a soluble catalyst in the liquid phase, the reactor residence time is reported to be 5-10 min [2].
The reaction is exothermic and the heat of reaction is 4.9 kcal/g-mol[2].
About 8-10 % conversion (80-90 % of equilibrium conversion) is obtained per pass thr..ough the
reactor. Selectivity to DAA is reported to be 90-95 % [2]. By products are mainly MO and higher
molecular weight condensation products according to the following reaction.
( )
acetone MO
Dehydration of DAA to MO:

DAA is converted to MO in the presence of a mineral acid at 100-120 0C. The catalyst normally
employed is 0.05% phosphoric acid even though sulfuric acid and other dehydrating agents can be
used. The reaction is equilibrium limited. However, since it can be carried out in the base of a
distillation tower, the MO and water are continuously removed from the reaction zone and the
reaction can be essentially carried to completion [2]. The reaction is highly selective (90-95%) to
5
MO [2].Mesitylene and phorone(EQ. 4 and 5) are main by-products of the reaction. The reaction
scheme is shown below.
( ) ( ) → ( )
DAA MO
( )
Acetone Mesitylene
( ) ( )
Acetone Phorone
Hydrogenation of MO to MIBK:
MIBK is produced by hydrogenation of MO either in the liquid or vapour phase. Catalyst employed
for either vapour or liquid phase hydrogenation are nickel [2,8], copper-chr..omium [9], or
palladium on carbon or alumina [10]. The vapour phase hydrogenation is usually carried out at 150-
170 0C and atmospheric pressure using a space velocity of 0.5 to 1.5 volumes/h/volume of catalyst,
based on the liquid MO feed. The liquid phase reaction is carried out at 60-130 0C and pressure
ranging from 3 to 30 atm. [2]. Liquid hourly space velocities are about 10h-1 when feeding pure MO
to 1h-1 when feeding lower concentrations of MO. Over-hydrogenation to MIBC can occur if the
MIBK concentration in the reactor outlet increases above 90 %. Selectivity to MIBK is 90-98 % if
the conversion of MO is less than 95%. By-products of this reaction include acetone and
isopropanol.
( ) ( )
MO MIBK
( )
Acetone isipropanol
( ) ( ) ( )
MIBK MIBC
2.2 OVERALL PROCESS DESCRIPTION

An overall flow plan for the manufacture of MIBK from acetone is presented in the following flow
sheet. Acetone is fed directly into reactor packed with Ca(OH)2. The reactor can be staged with
inter-cooling between each stage to take advantage of favorable equilibrium of DAA at low
temperature. The reactor may be jacketed with the arrangement of cooling water supply for the
same purpose. For economic reasons, the reactor outlet temperature is maintained at 0-20 0C to
achieve a conversion per pass of about 9%. After the reaction step is completed, the product can be
6
stabilized with phosphoric acid and stripped free of acetone, producing a 90 % DAA mixture.
Recovery of acetone from DAA should be carried out at low pressure to avoid reversion of the
DAA back to acetone at temperature greater 120 . The crude DAA is mixed with 0.05 wt.%
phosphoric acid and fed to a dehydrating column where acetone and MO-water azeotrope mixture
are distilled overhead. Heavy by-products are purged from the bottom of the column. Acetone is
then recovered for recycle from MO in the MO recovery column. The can further purified from
water prior to hydrogenation if required.
The hydrogenation may be carried out in the liquid phase or the gaseous phase. Hydrogenation in
the liquid phase is a simpler process, since inter alia it is possible to operate at lower temperatures,
the mesityl oxide does not need to be previously evaporated, and there is no need to recondense the
reaction product after completion of the reaction. However, that hydrogenation in the liquid phase
has the drawback that the life of the catalyst is very short. It has now been found that this drawback
can be obviated by treating the crude mesityl oxide with hydrogen peroxide and inorganic base
solution prior to the hydrogenation [11]. Any suitable inorganic base can be used in the treatment,
but relatively strong inorganic bases such as aqueous caustic alkali solutions are particularly
advantageous. Sodium or potassium hydroxides are examples of suitable caustic alkalis which can
be used successfully. The treatment with hydrogen peroxide and inorganic base solution can be
carried out simply by adding an aqueous solution of hydrogen peroxide and base solution to the
mesityl oxide. A good contact between the reagents can be ensured by stirring or other suitable
measures. The contact time does not need to be long; in most cases 10 seconds is quite sufficient. In
practice, however, it is more convenient to work with longer contact times and there is no objection
to this. There is generally no advantage in extending the time of treatment beyond about 30
minutes, however. The hydrogen peroxide and the inorganic base solution can be added to the
mesityl oxide in any given sequence, or simultaneously. In view of the comparatively low degree of
stability of hydrogen peroxide in an alkaline medium, but generally it is advised first to admix the
hydrogen peroxide well with the mesityl oxide and only then to add the inorganic base solution, in
order to prevent unnecessary consumption of hydrogen peroxide. The reaction may be carried out
at room temperature, although there is no abjection to using higher or lower temperatures. The
operating temperature normally lies between about 5° and about 50° C. The quantities of the
reagents required are not large. They can, for example, be used in amounts, per liter of crude
mesityl oxide, ranging from about 0.3 to about 1.0 ml. of hydrogen peroxide solution of 8%
concentration and from about 0.3 to about 1.0 ml. of caustic alkali solution of 10% concentration,
or in equivalent amounts of solutions of other concentrations. The concentrations of the solutions
are not critical, in practice they are so chosen as to make it easy to proportion with the desired
accuracy the small amounts of the reagents required. Hydrogen peroxide solutions of about 5 to
7
about 15% w. concentration in water and aqueous inorganic base solutions of about 5 to about 15
wt.% concentration are conveniently used. After the treatment with hydrogen peroxide and
inorganic base according to the invention, it is sufficient to separate the aqueous phase from the
mesityl oxide in a simple manner, as, for instance, by decantation. Washing with water is possible
but is not generally necessary.
MIBK is produced from MO by hydrogenation in a reactive distillation tower or in a fixed bed
reactor over Ni catalyst in the presence of hydrogen [11]. Raney nickel is preferably employed as
nickel catalyst. Pure MIBK is finally recovered from uncovered MO in a two-step distillation
scheme where lights are removed in the first tower and pure MIBK is recovered as an overhead
product in the second tower.
8
3. MATERIAL BALANCE
Data required for calculation:
Compound Chemical Molecular Sp. Heat Boiling Heat of Standard
Formula weight (kJ/kg 0C) point @ vaporization heat of
(kg/kmol) 1atm. (0C) (kJ/kg) formation
(kJ/mol)
Acetone C3H6O 58 0.084 56.5 523.00
DAA C6H12O2 116 3.49 166 -551.69
MO C6H10O 98 3.84 129 2001.93 -253.54
MIBK C6H120 100 1.25 117 462.94 -288.54
Mesitylene C9H12 120 1.16 164.7
Phorone C9H14O 138 1.50 198.5
Isopropanol C3H8O 60 1.26 108 880.12
Hydrogen H2 2 14.304 0
Water H2O 18 4.188 100 2245.00 -241.83 (as
vapour)
Production rate of MIBK:

Production rate of MIBK: Basis: 20 TPD
Plant operating hour: 24 hr. /day
Production rate: 833.34 kg/hr.
It is assumed that 1% MIBK will be lost in the downstream. So, MIBK to be produced in the
reactor: 833.34 × 1.01 kg/hr. = 841.67 kg/hr. = 8.4167 kmol/hr.
1. HYDROGENATION REACTOR (MIBK REACTOR):

Assumption:

95% conversion of the reaction (6).
100% conversion of the reaction (7) 
Reaction (8) is neglected since there is no possibility of over-hydrogenation.
5% excess MO is taken. 
No excess hydrogen is used. 

9wt% i.e. 84.63 kg/hr. MO is present in the reactor outlet.
1.8 wt. % i.e. 18.00kg/hr.acetone is present in the reactor outlet
Calculation:
MIBK to be produced in the reactor: 8.4167 kmol/hr.
9
MO required: (8.4167/0.95) kmol/hr. = 8.8596 kmol/hr. = 868.24 kg/hr.
Excess MO in output: 868.24 × 0.05 = 43.412kg/hr.
H2 required: (8.4167/0.95)kmol/hr. = 8.8596 kmol/hr. = 17.19kg/hr.
Excess H2 in outlet: 8.8595 ×0.05 kmol/hr. = 0.4429 kmol/hr. = .8859 kg/hr.
MO in inlet: 868.24 + (84.68 – 43.413) kg/hr. = 910 kg/hr.

H2 used for reaction (7): .4429 kmol/hr.
Isopropanol formed: 0.4429 kmol/hr. = 26.57kg/hr.
Acetone required: 0.4429 kmol/hr. = 25.68kg/hr.
Acetone in inlet: (25.68 + 18.00) kg/hr. = 43.68 kg/hr.
Component Inlet (kg/hr.) Outlet (kg/hr.)
MO 910.00 84.63
Acetone 43.68 18.00
Hydrogen 17.19
MIBK 841.67
Isopropanol 25.79
Total 970.87 9970.87
2. DEHYDRATING COLUMN (MO REACTOR):
Assumption:

100% conversion for reaction (3).
80% conversion for reaction (4).
90% conversion for reaction (5).
1 wt. % i.e. 10.65 kg/hr.mesitylene is present in the reactor outlet. 
9 wt. % i.e. 10.66 kg/hr.phorone is present in the reactor outlet. 
4.34wt% i.e. 50.101 kg/hr.acetone is present in the reactor outlet.
Calculation:
MO to be produced: 910 kg/hr. = 9.28 kmol/hr.
DAA required: 9.28 kmol/hr. = 1073 kg/hr.
Water produced: 9.28 kmol/hr. = 170.79 kg/hr.
Mesitylene to be produced: 10.65 kg/hr. = 0.088 kmol/hr.
Acetone required: (3 × 0.088)/0.80 = .33 kmol/hr. = 19.30 kg/hr.
Excess acetone in outlet: 0.33 × 0.2 = 0.66 kmol/hr. = 38.28 kg/hr.
Water produced: (3 × 0.088) kmol/hr. = 0.264kmol/hr. = 4.75 kg/hr.
10
Phorone to be produced: 10.66 kg/hr. = 0.077 kmol/hr.
Acetone required: (3 × 0.077)/0.90 = .2566 kmol/hr. = 14.88 kg/hr.
Excess acetone in outlet: .2566 × 0.2 = 0.0513 kmol/hr. =2.59 kg/hr.
Water produced: (2 × 0.077) kmol/hr. = 0.154 kmol/hr. = 2.772 kg/hr.
Acetone in inlet: (50.101+ 19.30 + 14.88 – 38.28– 2.59) kg/hr. = 79.20 kg/hr.
DAA 1073
Acetone 79.20 50.101
MO 910.00
water 170.79
Mesitylene 10.65
Phorone 10.66
Total 1152.20 1152.20
3. DAA REACTOR:
Assumption:


Conversion and selectivity of reaction (1) is 9% and 59% respectively.
96.6% conversion for reaction (2). 
The acetone used as raw material contains 99.8 wt. % pure acetone and rest 0.2 wt. % water. 
Calculation:
DAA to be produced: 1073 kg/hr. = 9.28 kmol/hr.
Acetone required: (2 × 9.28)/0.09 kmol/hr. = 206.22 kmol/hr. = 11993.37 kg/hr.
Excess acetone in outlet: 206.22× 0.91 = 187.66kmol/hr. = 10884.29 kg/hr.
We know, selectivity = (moles of desired product/moles of undesired product)
Thus moles of undesired product (MO) = (9.28/59) kmol/hr. = 0.1572 kmol/hr. = 15.43 kg/hr.
Water formed: 0.788 kmol/hr. = 18.18 kg/hr.
Acetone required: (2 × 0.788)/0.966 kmol/hr. = 1.632 kmol/hr. = 94.68 kg/hr. This amount of
acetone is used from the unreacted acetone of the reaction (1). Unutilized acetone in the reactor
outlet: (10884– 94.68)kg/hr. = 10895.01 Total acetone in inlet: (100/99.8) × 11993.37× 0.998
kg/hr. = 11993.37kg/hr.
Water in inlet: (100/99.8) × 11993.37 × 0.002 kg/hr. = 24.13 kg/hr.
11
Component Inlet (kg/hr.) [2] Outlet (kg/hr.) [3]
Acetone 11993.37 10895.01
Water 24.13 34.06
DAA 1073
MO 15.43
Total 12017.50 12017.50
4. ACETONE RECOVERY COLUMN:

Assumption:
Distillate composition is similar to raw material composition i.e. 99.8 wt.% acetone and rest 0.2

wt.% water.
Calculation:
Acetone at top: (10895.01 – 79.01) = 10816
Total distillate flow rate: (100/99.8) × 10816 kg/hr. = 10837.67 kg/hr.
Water at top: (10837.67 - 10816) kg/hr. = 21.67 kg/hr.
Component Inlet (kg/hr.) [4] Outlet (kg/hr.)
Top [4A] Bottom [5]
Acetone 10895.01 10816.00 79.01
Water 27.67 21.67 5.998
DAA 1079.40 1079.40
MO 15.43 15.43
10837.67 1179.85
Total 12017.50 12017.50
Since in the DAA reactor, some amount of MO and water is produced as the side product, they will
enter into the dehydrating column (MO reactor). So the material balance of the MO reactor and
thereafter that of the MIBK reactor will be changed accordingly. The revised material balances of
these reactors are shown below sequentially.
The change in material balance is not complex. There is some amount of MO and water in the inlet
stream and they will carry forward. Since the MO reactor is a reactive distillation (RD) tower, the
material balance table is arranged like a distillation tower.
12
Top [7] Bottom [6A]
DAA 1079.40
Acetone 79.01 50.10
MO 15.43 927.34
Water 5.998 181.06
Mesitylene 10.65
Phorone 10.66
1158.51 21.32
Total 1179.84 1179.84
6. MO RECOVERY COLUMN:
Assumption:
Distillate composition is similar to raw material composition i.e. 99.8 wt.% acetone and rest 0.2

wt.% water.
Calculation:
Acetone at top: (250.53 – 225.79) kg/hr. = 24.74 kg/hr.
Total distillate flow rate: (100/99.8) × 24.74 kg/hr. = 24.78 kg/hr.
Water at top: (24.78 – 24.74) kg/hr. = 0.04 kg/hr.
Top [7A] Bottom [8]
Acetone 50.10 4.94 45.15
Water 181.066 0.008 181.05
MO 927.35 927.35
4.95 1153.56
Total 1158.52 1158.52
7. DECANTER:
Assumption:

Volume of mixing is neglected.
1ml 8 wt.% H2O2 solution and 1ml 10 wt.% NaOH solution is required per liter of crude MO
solution [11].
Calculation:
Calculation of the volume of the inlet stream:
13
3
Component Mass flow rate (kg/hr.) Density (kg/m ) Volume (L/hr.)
Acetone 45.15 792.5 56.97
Water 181.05 1000 181.05
MO 927.35 858.0 1080.82
Total 1318.84
3
Density of H2O2 solution: 1440 kg/m
3
Density of 10 wt.% NaOH solution : 1111.1kg/m
8 wt.% H2O2 solution = 5.7 vol% solution.
10 wt.% NaOH solution = 8.9 vol% solution.
H2O2 solution required: 6.59 L
It contains 0.375 L i.e. 0.54 kg H2O2 and 6.215 L i.e. 6.215 kg water.
Thus total mass of the H2O2 solution added: (0.54 + 6.215) kg/hr. = 6.755kg/hr.
NaOH solution required: 6.59 L

It contains 0.586 L i.e. 0.651 kg NaOH and 6.004 L i.e. 6.004 kg water.
Thus total mass of the H2O2 solution added: (0.651 + 6.004) kg/hr. = 6.655 kg/hr. Thus total mass
of the aqueous phase: (181.05 + 6.755 + 6.655) kg/hr. = 194.46 kg/hr.

Feed stream Settling Aqueous Organic
[9] agent [9A] phase [9B] phase [10]
Acetone 45.15 45.15
Water 181.05 181.05
MO 927.35 927.352
H2O2 solution 6.755 6.755

NaOH solution 6.655 6.655
1153.55 13.41 194.46 972.502
Total 1166.96 1166.96

Assumption :
Same as earlier.
Calculation:
14
MIBK to be produced in the reactor: 8.4167 kmol/hr. =841.67kg/hr.
MO required: (8.4167/0.95) kmol/hr. = 8.8596 kmol/hr. = 868.24 kg/hr.
Excess MO in output: 868.24 × 0.05 = 43.412kg/hr.
H2 required: (8.4167/0.95) kmol/hr. = 8.8596 kmol/hr. = 17.72kg/hr.
Excess H2 in outlet: 8.8595 ×0.05 kmol/hr. = 0.4429 kmol/hr. = .8859 kg/hr.
MO in inlet: 927.25 kg/hr.
H2 used for reaction (7): .4429 kmol/hr.
Isopropanol formed: 0.4429 kmol/hr. = 26.56kg/hr.
Acetone required: 0.4429 kmol/hr. = 25.68kg/hr.
Acetone in inlet: (25.68 + 19.47) kg/hr.= 45.15 kg/hr.
Acetone in outlet: (45.15-25.68)=19.47kg/hr.
MO in outlet=102.52kg/hr.
Component Inlet (kg/hr.) [12 & 13] Outlet (kg/hr.) [14]
MO 927.35 102.52
Acetone 45.15 19.47
Hydrogen 17.72
MIBK 841.67
Isopropanol 26.56
Total 990.22 990.22
9. 1ST PURIFICATION COLUMN:

Assumption:

Isopropanol and acetone is separated completely as the distillate.
No intermixing of the top and bottom product occurs.
Calculation:
Top [14A] Bottom [15]
Acetone 19.47 19.47
Isopropanol 26.56 26.56
MO 102.52 102.52
MIBK 841.67 841.67
46.03 944.08
Total 990.18 990.18
15
10. FINAL PURIFICATION COLUMN:
Assumption:

1 wt.% of the total MIBK is lost with the residue.
The composition of the distillate is 99.8 wt.% MIBK and rest 0.2 wt.% water. 
Calculation:
MIBK at top: 4166.67 kg/hr.
Total distillate flow rate: (100/99.8) × 4166.67 kg/hr. = 4175.02 kg/hr.
Water at top: (4175.02 – 4166.67) kg/hr. = 8.35 kg/hr.
Top [17] Bottom [16A]
MO 102.41 1.67 100.74
MIBK 841.67 833.33 8.34
835 109.08
Total 944.08 944.08
11. ACETONE RECYCLED STREAM:

Assumption:
Make up acetone and recycled acetone ratio = 1: 9.23
Calculation:
Amount of acetone recycled (stream no. 20): (10837.67 + 4.96) kg/hr. = 10842.63 kg/hr. Amount
of acetone fed to the DAA reactor (stream no. 2): 12017.41 kg/hr.
Amount of make-up acetone (stream no. 1): (12017.41 – 10842.63) = 1174.78 kg/hr.
4. ENERGY BALANCE
1. ACETONE RECYCLED STREAM
Assumption:
Temperature of the make up acetone: 35 0C. 
Temperature of the recycled stream: 50 0C 
Reference temperature: 25 0C 
Calculation:
Heat content of the make up stream [1]: (1172.43 × 0.084 × (35-25)) + (2.34 × 4.188 × (35-25))
kJ/hr.= 1082.84 kJ/hr..
16
Heat content of the recycled stream [20]: (10820.944× 0.084 × (50-25)) + (21.68 × 4.188 × (50-
25)) kJ/hr.. = 24993.87 kJ/hr.
Heat content of the mixed stream [2]: (11993.37 × 0.084 × (T-25)) + (24.03 × 4.188 × (T-25))
kJ/hr.
Now,
Heat content of the mixed stream = Heat content of the make up stream + Heat content of the
recycled stream
Or, (11993.37 × 0.084 × (T-25)) + (24.03 × 4.188 × (T-25)) = 1082.84 + 24993.87 Solving we get
0
T = 48.53 C
0
Thus temperature of the mixed stream [2]: 48.53 C
2. DAA REACTOR:
Assumption:

Only the desired reaction is taken into account.
Specific heat, Cp is calculated at reference temperature. 
Cp is assumed constant over the temperature range. 
0 0 
Let chilling water is available at 5 C and 5 C increase in the outlet temperature is possible.
0
Reference temperature: 25 C
Calculation:
0
Reactor inlet temperature: 48.53 C
0
Reactor outlet temperature: 15 C
Compound mi (kg/hr.) niHi (kJ/s) mo (kg/hr.) noH0 (kJ/s)
Acetone 11993.37 ? 10895.01 ?
Water 24.13 ? 34.06 ?
DAA 1073 ?
MO 15.43 ?
nH values are calculated by the expression, n× H = m× Cp× ΔT

Heat content of the inlet stream: (11993.37× 0.084 × (48.53-25)) + (24.13× 4.188 × (48.53 -25))
kJ/hr.= 26082.99 kJ/hr..
17
Heat content of the outlet stream: (10895.01× 0.084 × (15-25)) + (34.06× 4.188 × (15-25)) +
(1073× 3.49 × (15-25)) + (15.43× 3.84 × (48.53-25)) kJ/hr. = - 49420.12 kJ/hr..
Extent of reaction, ξ: (no-ni)/γ = (10895.01-11993.37)/(-2 × 58) = 9.4686 kmol/hr.. = 9468.62
mol/hr.
The standard heat of reaction, ΔHr..o[4]: - 4.9 kcal/mol = - 20.58 kJ/mol Then the enthalpy change
of the reaction, ΔH = ξ×ΔHr..0 + ∑noHo - ∑niHi Putting all the values we get, ΔH = -270367.30
kJ/hr..
Energy balance: Q – Ws = ΔH + ΔEk + ΔEp
Q = ΔH = -270367.30 kJ/hr.
Where, Ws = shaft wok = 0 (no moving parts).
ΔEk = Kinetic energy change = 0 (neglected). ΔEp = Potential energy change = 0 (neglected).
So, 270367.30 kJ/hr..heat is to be removed from the reactor to maintain the desired conversion.
Flow rate of chilling water: 270367.30 /(4.188 × 5) = 12911.52 kg/hr.
Description Heat input (kJ/hr..) Heat output (kJ/hr..)
Inlet stream [2] 26082.99
Outlet stream [3] 49420.12
Reaction 293704.43
Chilling water 270367.30
Total 319787.42 319787.42
3. ACETONE RECOVERY COLUMN:
Assumption:


The solutions are ideal in nature.
Saturated liquid feed is introduced in the column. 

Vapour leaving from top of the tower is saturated vapour. 
Total condenser is used. 
Bottom product exits as saturated liquid. 
Heat loss from the column is negligible. 
Reflux ratio = 0.10 

Reference temperature: 25 0C
18
Calculation:
Component Feed [4] Top [4A] Bottom [5]
Massflow rate Massflow rate Massflow rate
Wt % Wt % Wt %
(kg/hr..) (kg/hr..) (kg/hr..)
Acetone 10822.87 90.66 10816.00 99.80 79.05 6.70
Water 27.64 0.23 21.66 0.20 6.01 0.51
DAA 1079.16 8.98 1079.44 91.49
MO 15.62 0.13 15.33 1.30
Saturation temperature of mixture is determined using the formula Tsat = ∑ Tisat × xi
Boiling point of feed: 66.53 0C
Boiling point of distillate: 56.59 0C Boiling point of residue: 157.85 0C
We know, R = L0/D or, L0 = R × D = 1083.760 kg/hr.. G1 = L0 + D = 11921.4 kj/hr..
HG = (11897.6 × 0.084 × (56.6-25)) + (23.844 × 4.188 × (56.6-25)) + (449 × 119.22) + (11897.6×
523) kJ/hr.. = 6310711.103 kJ/hr..
HL = (1081.6 × 0.084 × (56.6-25)) + (2.16 × 4.188 × (56.6-25)) kJ/hr.. = 5737.5 kJ/hr..
HD = (10816.00× 0.084 × (56.6-25)) + (21.66× 4.188 × (56.6-25)) kJ/hr.. = 31576.49 kJ/hr..
HW = (79.05× 0.084 × (157.9-25)) + (6.01× 4.188 × (157.9-25)) + (1079.16× 3.49 × (157.9-25)) +
(15.62× 3.84 × (157.9-25)) kJ/hr.. = 512736.08 kJ/hr..
HF = (10822.87× 0.084 × (66.5-25)) + (138.35 × 4.188 × (66.5-25)) + (1079.16× 3.49 × (66.5-25))
+ (15.62× 3.84 × (66.5-25)) kJ/hr.. = 220563.37 kJ/hr..
QC = HG - HL - HD = 6273397.11 kJ/hr..
QB = HD + HW + QC + QL – HF = 6687311.91 kJ/hr.
Description Heat input (kJ/hr..) Heat output (kJ/hr..)
Top Outlet stream [4A] 31576.49
Bottom Outlet stream [5] 512736.08
Reboiler 6687311.91
Condenser 6273397.11
Total 6907875.28 6907875.28

Assumption:
Vapour leaving from top of the tower is saturated vapour.
Total condenser is used.
19
Bottom product exits as saturated liquid.
Heat loss from the column is negligible.
Reflux ratio = 0.10
The reaction is completed at the feed tray .
Reactor inlet temperature [2]: 120 0C
Calculation:
Component Inlet (kg/hr..) Outlet (kg/hr..)
`Top Bottom
Mass flowrate
Wt % Massflowrate Massflowrate
(kg/hr..) Wt % Wt %
(kg/hr..) (kg/hr..)
DAA 1079.404 91.49
Acetone 70.01 6.70 50.106 4.33
MO 15.436 1.31 927.34 80.04
Water 5.998 0.50 181.066 15.63
Mesitylene 10.65 10.06
Phorone 10.67 9.99
Saturation temperature of mixture is determined using the formula Tsat = ∑ Tisat × xi

Boiling point of feed: 172.9 0C
We know, R = L0/D or, L0 = R × D =115.85kg/hr..
G1 = L0 + D = 6371.82 kg/hr..
HG = (275.9 × 0.084 × (121.5-25)) + (995.92 × 4.188 × (121.5-25)) + (5100 × 3.84 × (121.5-25)) +
(2245 × 195.92) + (275.9 × 523) + (5100.00 × 2001.93) kJ/hr.. = 14884564.65 kJ/hr..
HL = (25.08 × 0.084 × (121.5-25)) + (90.54 × 4.188 × (121.5-25)) + (463.64 × 3.84 × (121.5-25))
kJ/hr.. = 208607.58 kJ/hr..
HD = (50.106× 0.084 × (121.5-25)) + (927.34× 3.84 × (121.5-25)) + (181.066× 4.188 × (121.5-25))
kJ/hr.. = 417217.65 kJ/hr..
HW = (10.65× 1.16 × (181.6-25)) + (10.67× 1.50 × (181.6-25)) kJ/hr.. = 4441.02 kJ/hr..
HF = (1079.16× 3.49 × (120-25)) + (70.01× 0.084 × (120-25)) + (15.436× 3.84 × (120-25)) +
(5.998× 4.188 × (120-25)) kJ/hr.. = 366371.59 kJ/hr..
QC = HG - HL - HD = 14258739.42 kJ/hr..
Extent of reaction, ξ: (no-ni)/γ = (927.34-77.18)/(1 × 98) = 46.526 kmol/hr.
20
The standard heat of reaction, ΔHr..o is calculated from standard heat of formation using the
formula: ΔHr..o = ∑γi × Hfproduct - ∑γi × Hfreactant
The standard heat of reaction, ΔHr..o: - 56320 kJ/kmol
QB = HD + HW + QC + QL – HF - ξ ΔHr..o = 2049042.42 kJ/hr..
Description Heat input (kJ/hr.) Heat output (kJ/hr.)
Top Outlet stream [7] 41721.52
Bottom Outlet stream [6A] 4441.02
Reboiler 17024536.38
Reaction 524068.86
Total 2939635.63 2939635.63
5. MO RECOVERY COLUMN:
Assumption:

Saturated liquid feed is introduced in the column. 
Vapour leaving from top of the tower is saturated vapour. 
Total condenser is used. 
Bottom product exits as saturated liquid. 
Heat loss from the column is negligible. 
Reflux ratio = 0.20 

Calculation:
Component Feed Top Bottom
Wt % Wt % Wt %
(kg/hr.) (kg/hr.) (kg/hr.)
Acetone 50.106 4.33 4.94 99.80 45.158 3.91
Water 181.06 15.63 0.008 0.20 181.05 15.70
MO 927.35 80.04 927.35 80.39
Saturation temperature of mixture is determined using the formula Tsat = ∑ Tisat × xi Boiling point
of feed: 121.3 0C
21
We know, R = L0/D or, L0 = R × D = 4.96 kg/hr. G1 = L0 + D = 29.74 kg/hr.
HG = (5.99 × 0.084 × (56.6-25)) + (0.06 × 4.188 × (56.6-25)) + (2245 × 0.06) + (5.99 × 523) kJ/hr.
= 3291.31 kJ/hr.
HL = (4.95 × 0.084 × (56.6-25)) + (0.01 × 4.188 × (56.6-25)) kJ/hr. = 14.46 kJ/hr.
HD = (24.74 × 0.084 × (56.6-25)) + (0.04 × 4.188 × (56.6-25)) kJ/hr. = 70.96 kJ/hr.
HW = (45.158 × 0.084 × (121.6-25)) + (181.06 × 4.188 × (121.6-25)) + (927.35 × 3.84 × (121.6-
25)) kJ/hr. = 417611.13 kJ/hr.
HF = (50.10 × 0.084 × (121.5-25)) + (927.35 × 3.84 × (121.5-25)) + (181.06 × 4.188 × (121.5-25))
kJ/hr. = 417218.88 kJ/hr.
QC = HG - HL - HD = 3205.89 kJ/hr.
Reboiler 3291.31
Condenser 3205.89
Total 420756.98 420756.98
6. DECANTER:
Assumption:
Since the concentration of H2O2 and NaOH solution is very low, their specific heat is approximated
as of pure water.
Temperature of H2O2 and NaOH solution is 30 0C
Temperature of the feed stream is 40 0C
Temperature of the organic phase outlet is 40 0C
Calculation:
Heat content of the inlets: (45.158 × 0.084 × (40-25)) + (181.05 × 4.188 × (40-25)) + (927.35×3.84
× (40-25)) + (13.41 × 4.188 × (40-25)) kJ/hr. = 65692.02 kJ/hr.
Let the temperature of the aqueous phase outlet is T
Heat content of the outlets: (45.158 × 0.084 × (40-25)) + (927.35 × 3.84 × (40-25)) +
(183,76×4.188 × (T-25)) kJ/hr. = 267361.87 + 3847.51 × (T-25)
We know, Heat content of the inlets = Heat content of the outlets
Or, 324512.99 = 267361.87 + 3847.51 × (T-25)
22
Solving this equation, T = 39.8 0C
Description Heat Input (kJ/hr.) Heat Output (kJ/hr.)
Feed stream [9] 65692.02
Settling agent [9A] 56.16
Aqueous phase outlet [9B] 11430.22
Organic phase outlet [10] 53472.37
Total 64902.59 64902.59

Assumption:
Specific heat, Cp is calculated at reference temperature.
Cp is assumed constant over the temperature range.
Effect of pressure on Cp is neglected.
Temperature of the hydrogen stream: 115 0C
Pressure in the reactor: 20 atm.
Let chilling water is available at 5 0C and 5 0C increase in the outlet temperature is possible.
Calculation:
Reactor inlet temperature: 115 0C
Reactor outlet temperature: 116.80C
Compound mi (kg/hr..) niHi (kJ/s) mo (kg/hr..) noH0 (kJ/s)
MO 927.35 ? 102.41 ?
Acetone 45.158 ? 19.47 ?
Hydrogen 17.72 ? ?
MIBK 841.668 ?
Isopropanol 26.58 ?
nH values are calculated by the expression, n× H = m× Cp× ΔT

Heat content of the inlet stream: (45.158× 0.084 × (115-25)) + (927.35× 3.84 × (115 -25)) +
(17.72× 14.304 × (115-25)) kJ/hr.. = 343632.7 kJ/hr.
Heat content of the outlet stream: (19.47× 0.084 × (116.8-25)) + (102.41× 3.84 × (116.8-25)) +
(841.668 × 1.25 × (116.8-25)) + (26.58× 1.26 × (116.8-25)) kJ/hr.. = 135906.75 kJ/hr.
Extent of reaction, ξ: (no-ni)/γ = (841.668 -0)/(1 × 100) = 42.0834 kmol/hr. = 42083.4 mol/hr..
23
The standard heat of reaction, ΔHr.o is calculated from standard heat of formation using the
formula: ΔHr.o = ∑γi × Hfproduct - ∑γi × Hfreactant
The standard heat of reaction, ΔHr.o: -35.00 kJ/kmol
Then the enthalpy change of the reaction, ΔH = ξ×ΔHr.0 + ∑noHo - ∑niHi
Putting all the values we get, ΔH = -2511362.29 kJ/hr.
Energy balance: Q – Ws = ΔH + ΔEk + ΔEp
Q = ΔH = -2511362.29 kJ/hr..
Where, Ws = shaft wok = 0 (no moving parts).
ΔEk = Kinetic energy change = 0 (neglected).
ΔEp = Potential energy change = 0 (neglected).
So, 2511362.29 kJ/hr.heat is to be removed from the reactor to maintain the desired conversion.
Flow rate of cooling water: 2511362.29/(4.188 × 10) = 59965.67 kg/hr.
Inlet stream [12 & 13] 3436932.7
Outlet stream [14] 135906.75
Reaction 294583.8
Cooling water 502272.45
Total 638178.57 638178.57
8. 1ST PURIFICATION COLUMN:

Assumption:
Saturated liquid feed is introduced in the column.
Vapour leaving from top of the tower is saturated vapour.
Reflux ratio = 0.10
24
Calculation:

(kg/hr.) Wt % (kg/hr.) Wt % (kg/hr.) Wt %
Acetone 19.47 1.97 19.47 42.30
Isopropanol 26.56 2.68 26.56 57.70
MO 102.41 10.35 102.41 10.85
MIBK 841.66 85.00 841.66 89.15
of feed: 116.8 0C
We know, R = L0/D or, L0 = R × D = 4.60 kg/hr.
G1 = L0 + D = 253.24 kg/hr.
HG = (21.42 × 0.084 × (86.3-25)) + (29.22 × 1.26 × (86.3-25)) + (21.42 × 523) + (29.22 × 880.12)
kJ/hr. = 39286.96 kJ/hr.
HL = (1.94 × 0.084 × (86.3-25)) + (2.65 × 1.26 × (86.3-25)) kJ/hr. = 214.67 kJ/hr.
HD = (19.47× 0.084 × (86.3-25)) + (26.56× 1.26 × (86.3-25)) kJ/hr. = 2151.69 kJ/hr.
HW = (102.41× 3.84 × (118.30-25)) + (841.66× 1.25 × (118.30-25)) kJ/hr. = 134849.23 kJ/hr. HF =
(19.47 × 0.084 × (116.8-25)) + (102.41× 3.84 × (116.8-25)) + (841.66× 1.25 × (116.8-25)) +
(26.56× 1.26 × (116.8-25)) kJ/hr.. = 132831.34 kJ/hr.
QC = HG - HL - HD = 36920.6 kJ/hr.

Reboiler 36920.6
Condenser 184626.89
Total 173928.6 173928.6
9. FINAL PURIFICATION COLUMN:

Assumption:
25
Saturated liquid feed is introduced in the column.
Vapour leaving from top of the tower is saturated vapour
Reflux ratio = 2.33
The tower operates at 3 kg pressure
Calculation:

Wt % Wt % Wt %
(kg/hr.) (kg/hr.) (kg/hr.)
MO 102.41 10.85 1.67 0.20 100.74 92.36
MIBK 841.66 89.15 833.33 99.80 8.33 7.64
of feed: 161.9 0C
We know, R = L0/D or, L0 = R × D = 1945.56 kg/hr.
G1 = L0 + D = 13902.82 kg/hr.
HG = (2775.002 × 1.25 × (159.7-25)) + (5.56 × 3.84 × (159.7-25)) + (400.38 × 27.81) + (2775.002
× 462.94) kJ/hr. = 1765910.85 kJ/hr..
HL = (1941.66 × 1.25 × (159.7-25)) + (3.89 × 3.84 × (159.7-25)) kJ/hr. = 328939.09 kJ/hr. HD =
(833.33× 1.25 × (159.7-25)) + (1.67 × 3.84 × (159.7-25)) kJ/hr. = 141175.74 kJ/hr. HW = (8.33 ×
1.25 × (179.8-25)) + (100.74× 3.84 × (179.8-25)) kJ/hr. = 61494.93 kJ/hr.
HF = (841.66× 1.25 × (161.9-25)) + (102.41× 3.84 × (161.9-25)) kJ/hr.. = 197865.59 kJ/hr. QC =
HG - HL - HD = 1295796.02 kJ/hr.
26
Top Outlet stream [17] 141175.74
Bottom Outlet stream [16A] 61494.93
Reboiler 292836.23
Total 1498467.47 1498467.47
10. PRE-HEATER 1:
Assumption:

High pressure (12.5 bar) saturated steam of temperature 190 0C is available for heating.
Calculation:
Heat load: (1007922.47 – (- 242871.32)) kJ/hr. = 68732.72 kJ/hr.
Latent heat of vaporization of saturated steam [15]: 1977.4 kJ/kg
Steam required: (68732.72 /1977.4) kg/hr. = 34.758 kg/hr.
11. REBOILER 1:
Calculation:
Heat load: 6619328.626 kJ/hr.
Latent heat of vaporization of saturated steam: 1977.4 kJ/kg
12. CONDENSER 1:
Calculation:
Cooling water required: (6275974.58 /4.188 × 10) kg/hr. = 149856.12 kg/hr.
13. COOLER 1:
Calculation:
Heat load: (366524.344-513359.93) kJ/hr. = -146835.586 kJ/hr.
14. REBOILER 2:
Calculation:
15. CONDENSER 2:
27
Calculation:
Calculation:
Heat content of the outlet stream:
(53.38 × 1.16 × (30-25)) + (53.32× 1.50 × (30-25)) kJ/hr.. = 709.50 kJ/hr.
Heat load: (709.50 -22221.66) kJ/hr. = -21512.16 kJ/hr.
16. REBOILER 3:
Calculation:
17. CONDENSER 3:
Calculation:
18. COOLER 4:
Calculation:
Heat content of the outlet stream: (225.79 × 0.084 × (40-25)) + (905.29 × 4.188 × (40-25)) +
(4636.76 × 3.84 × (40-25)) kJ/hr.. = 64846.43 kJ/hr.
Heat content of the inlet stream: 417611.06 kJ/hr.
Heat load: (64846.43 - 417611.06) kJ/hr. = -352764.622 kJ/hr.
Cooling water required: (1763823.11/4.188 × 10) kg/hr. = 8423.22 kg/hr.
19. PRE-HEATER 2:
Calculation:
Heat content of the outlet stream: (45.158 × 0.084 × (115-25)) + (927.35 × 3.84 × (115-25)) kJ/hr..
= 320834.22 kJ/hr.
Heat content of the inlet stream: (45.158 × 0.084 × (40-25)) + (927.35 × 3.84 × (40-25)) kJ/hr.. =
53472.37 kJ/hr.
Heat load: (320834.22 – 53472.37) kJ/hr. = 267361.87 kJ/hr. Latent heat of vaporization of
saturated steam: 1977.4 kJ/kg Steam required: (267361.87 /1977.4) kg/hr. = 135.20 kg/hr.
20. REBOILER 4:
Calculation:
28
21. CONDENSER 4:
Calculation:
22. PRE-HEATER 4:
Calculation:
Heat content of the outlet stream: 134850.88 kJ/hr.
Heat load: (197868.01 – 134850.88) kJ/hr. = 63017.13 kJ/hr.
23. REBOILER 5:
Calculation:
Heat load: 1300599 kJ/hr.
Steam required: (1300599/1977.4) kg/hr. = 657.732 kg/hr.
24. CONDENSER 5:
Calculation:
25. COOLER 5:
Calculation:
Heat content of the outlet stream: (19.47× 0.084 × (30-25)) + (26.56 × 1.26 × (30-25)) kJ/hr. =
175.55 kJ/hr.
Heat content of the inlet stream: 2152.34 kJ/hr. Heat load: (175.55 - 2152.34) kJ/hr. = -1976.78
kJ/hr.
26. COOLER 6:
Calculation:
Heat content of outlet stream: (833.34 × 1.25 × (30-25)) + (1.67 × 3.84 × (30-25)) kJ/hr. = 5240.4
kJ/hr.
Heat load: (5240.4 – 141176.41) kJ/hr. = -135936.01 kJ/hr.
29
27. COOLER 7:
Calculation:
Heat content of the outlet stream: (8.33 × 1.25 × (30-25)) + (100.74 × 3.84 × (30-25)) kJ/hr. =
1986.33 kJ/hr.
Heat load: (1986.33 – 61496.89 ) kJ/hr. = -59510.56 kJ/hr.
28. COOLER 8:
Calculation:
Heat content of the outlet stream:
(10837.67 × 0.084 × (50-25)) + (4.95 × 4.188 × (50-25)) kJ/hr. = 23278.01 kJ/hr.
Heat content of the inlet stream:
(10837.67 × 0.084 × (56.6-25)) + (4.95 × 4.188 × (56.6-25)) kJ/hr. = 29423.40 kJ/hr.
Heat load: (23278.01 – 29423.40 ) kJ/hr. = -6145.39 kJ/hr.
29. COMPRESSOR 1:
Assumption:
Hydrogen is available at 3 atm. pressure and 30 0C temperature.
The hydrogen stream is to be pressurized upto 20 atm.
Adiabatic compression is done in the compression.
Heat capacity ratio, γ of hydrogen is 1.405
Calculation:
Let outlet temperature is T20C
The pressure-temperature relation for adiabatic compression is
P(1-γ/γ)T = constant Thus, T2 = T1 × (P1/P2) (1-γ/γ) = 30 × (3/20) (1-1.405/1.405) = 52 0C
30. PREHEATER 3:
Calculation:
Heat content of the outlet stream: (17.72 × 14.304 × (115-25)) kJ/hr. = 22812.01 kJ/h Heat content
of the inlet stream: (17.72 × 14.304 × (52-25)) kJ/hr. = 6843.60 kJ/hr. Heat load: (22812.01 –
6843.60) kJ/hr. = 15968.41 kJ/hr.
Latent heat of vaporization of saturated steam: 1977.4 kJ/kg Steam required: (15968.41 /1977.4)
kg/hr. = 8.07 kg/hr.
30
5. EQUIPMENT DEIGN
The mass transfer equipment which is selected for detailed design is the final purification column.
It is a distillation column which separates MIBK from MO and gives a product purity of 99.8 wt%
MIBK solution. The column handles 4720.4 kg/hr.. mixture of MIBK and MO having composition
89.15 wt% MIBK and 10.85 wt% MO. A sieve tray column operating at 3 kg pressure is to be
designed for this job.
5.1 LIST OF ITEMS TO BE REPORTED
1. Column sizing (diameter and height)
2. Tray hydraulic design
3. Tray support specification
4. Material of construction
5. Pressure drop
6. Roof and bottom specification
7. Shell, nozzle, bolt, and flange specification.
8. Other accessories and fittings.
9. Condenser –Reboiler setup.
10. Column support.
11. Drawing of the column.
5.2 AVAILABLE INFORMATION
1. Flow rate and composition of feed.
2. Top and bottom product specification.
3. Operating pressure of the column.
5.3 ADDITIONAL INFORMATION
1. Saturation temperature of MIBK and MO
2. Vapour-liquid equilibrium data at operating temperature and pressure
3. Relative volatility
4. Top and bottom temperature
5. Feed temperature at 3kg pressure
6. Complete material balance
7. Physical properties (density and surface tension) of distillate, residue and vapour
31
1. Saturation temperature of MO is determined by the help of Wagner equation [13]which is given
below.
*( ) ( )+
And the form of this equation which is used to determine the saturation temperature of MIBK is as
follows.
Minimum for these equations is triple point and the maximum is critical temperature (Tc). The
pressure is in bar and the temperature is in kelvin [13].The values of the constants: a, b, c, d are
given below [13]
Component Tc (K) A B C D Pc (bar) Tmax (K)
MIBK 605 -8.68118 3.99203 -4.81662 -1.73164 34.1465 605
MO 571.40 3.8222 1190.6904 195.45 571.40
Putting P= 3kg = 2.94 bar, saturation temperature and the saturation pressure is calculated. From
these values vapour-liquid equilibrium (VLE) data is calculated using Raoult’s law because we
assumed the mixture and the vapour phase ideal.
(Tsat)MIBK = 159.7 (Psat)MIBK = 2.94 bar
(Tsat)MO = 179.8 (Psat)MO = 2.94 bar
From the saturation temperature values it is clear that MIBK is more volatile than MO. So MIBK is
designated as component 1 and MO is designated as component 2.
2. The VLE data is calculated using –
( )
( ) ( )
( )
The calculated VLE data are given below.

T (o C) P1 sat (bar) P2 sat (bar) X1 Y1
159.7 2.940000 1.870336 1 1

160 2.957839 1.883699 0.983392128 0.989359
161 3.022597 1.928778 0.924487848 0.95046
162 3.088397 1.974686 0.866754293 0.910504
163 3.155251 2.021431 0.810153982 0.869469
164 3.223168 2.069026 0.754650685 0.827335
165 3.292157 2.117479 0.70020938 0.784081
166 3.362229 2.166802 0.646796194 0.739686
167 3.433394 2.217005 0.594378366 0.694128
32
168 3.50566 2.268097 0.542924197 0.647384
169 3.579038 2.320091 0.492403007 0.599432
170 3.653537 2.372995 0.442785099 0.550249
171 3.729168 2.426821 0.394041713 0.499812
172 3.80594 2.481579 0.346144996 0.448098
173 3.883862 2.537281 0.299067958 0.395081
174 3.962945 2.593936 0.252784443 0.340738
175 4.043198 2.651556 0.207269096 0.285044
176 4.12463 2.710151 0.162497327 0.227973
177 4.207252 2.769733 0.118445284 0.1695
178 4.291073 2.830312 0.075089821 0.109597
179 4.376103 2.891899 0.032408473 0.048239
179.77 4.442405 2.94 0 0
3.The relative volatility at top and bottom is determined by using the formula [14]
( )
( )
And = 1.572 = 1.511.
The geometric mean relative volatility, α = 1.541
4.The top and bottom temperature is nothing but the saturation temperature of the top and bottom
product respectively.
Top temperature = 159.7
Bottom temperature = 179.8
5.Feed temperature = (159.7 × 0.8915)+(179.8 × 0.1085) = 161.90
The overall material balance equation is-
F=D+W
Where, F= Feed rate, kmol/hr.
D= Overhead product rate, kmol/hr.
W= bottom product rate, kmol/hr.
Doing component balance for MIBK
FXf= DXd+ WXw
Where, Xf= mole fraction of MIBK in feed
Xd= mole fraction of MIBK in distillate
Xw= mole fraction of MIBK in residue
Given,
F = 944.08 kg/hr.. = 9.47kmol/hr..
Xf= 0.8891
Xd= 0.9980
Xw= 0.0750
33
So the equations becomes-
D+W = 9.47
9.47× 0.8891 = D × 0.998 + W × .0750
Solving these two equations we get, W= 1.116kmol/hr.and D= 8.354kmol/hr.
6. The liquid density is calculated by modified form of Rackett equation [15]-
( )
Density (g/ml) =
Where, A,B and n are regression coefficient. T and Tc are in Kelvin. The values of the coefficient
for MIBK and MO are given bellow [15]:
component A B n Tc
MIBK 0.26654 0.25887 0.28571 571.40
MO 0.27648 0.25438 0.28484 600.00
ρ(MIBK) at top temperature (159.7 )= 0.6567 g/ml

ρ(MIBK) at bottom temperature (179.8 )= 0.631 g/ml
ρ(MO) at top temperature (159.7 )= 0.7159 g/ml
ρ(MO) at bottom temperature (179.8 )= 0.6919 g/ml
So the distillate density becomes,
ρ(top) = 0.0019×0.7159 + 0.9981×0.6567 = 0.65689 g/ml = 656.89 kg/m3
Similarly the residue density becomes, ρ(bottom) = 0.68739 g/ml = 687.39 kg/m3
7. The vapour density is calculated by the following formula.
ρ= (PM/RT)
where, P=total pressure
M= molecular weight
R=universal gas constant
T= temperature
By calculating we get,
Vapour density at top, ρv(top) = 8.173 kg/m3
Vapour density at bottom, ρv(bottom) = 7.666 kg/m3
8. The liquid surface tension is determined by modified Othmer relation [15]
Surface tension (dyne/cm) = A×(1-T/Tc)n
The values of the constants are given below [15]
component A n Tc
34
MIBK 57.130 1.2040 571.4
MO 66.120 1.2560 600.0
The surface tension of distillate and residue is calculated applying same procedure for density
which gives the following value.
σ(top) = 10.394 dyne/cm
σ(bottom) = 11.115 dyne/cm.
5.4 DESIGN METHODOLOGY
STEP 1: TO FIND NUMBER OF THEORETICAL STAGES
To determine the number of theoretical stages, here we used the method of McCABE and THIELE
[16]. In this method what we need first is the equilibrium curve (x Vs y). The VLE data obtained by
Raoult’s lay is plotted. The operating line equations for both top and bottom section are determined
by appropriate mass balance. The equations of enriching section and stripping section operating
lines are respectively-
Yn+1 = (L/G) Xn+ (D/G) Xd……………………………………………………………(5.1)
=(R/R+1) Xn+ Xd/(R+1)
Ym+1 = (Lb/Gb).Xm– (W/Gb).Xw……………………………………………………….. (5.2)
= (Lb/Lb-W)Xm– (W/Lb-W)XW
Where, R = L/G = Reflux ratio.
L, G = liquid & vapour flow rate in top section respectively
Lb, Gb= liquid & vapour flow rate in bottom section respectively
The q-line equation is-
y = (q/q-1).x – (Zf/q-1)……………………………………………………………………….(5.3)
where, q = (HG-HF)/(HG-HL)
HG = enthalpy of vapour from any tray.
HF = enthalpy of feed
HL = enthalpy of liquid
Therefore if the feed is saturated liquid then q = 1 and q/q-1 = ∞. So q-line would be vertical.
The general procedure of finding number of equilibrium stage is as follows.
1. The distillate composition is marked on x-axis and travelled vertically upward upto the diagonal
line.
2. Travel vertically upward from the point of feed composition on the x-axis upto the diagonal.
Extend the line according to the slope of q-line and mark the point of intersection with the
equilibrium line.
35
3. Draw a line joining these two points and extend up to y-axis. The intercept on y-axis is
Xd/(Rm+1), from which we can find Rm.
4. Assume an operating reflux ratio 1.2-1.5 times of Rm and find the intercept (Xd/R+1) on y-axis.
5. Join the intercept and the corresponding point of the distillate composition on diagonal. This is
the enrichment section operating line.
6. By staircase construction we will get the number of theoretical stage in enrichment section.
7. Similarly we can find the number of theoretical stage in the striping section. Mark the position of
bottom product on x-axis and find the corresponding on the diagonal. Join this point with the q-line
intersection point on the equilibrium curve. This is the striping section operating line.
8. By staircase construction we will get the number of equilibrium stage in the striping section.
9. The feed point should be located closest to the intersection of two operating line.
10. The equilibrium curve is given below.
1.0
0.9
0.8
0.7
0.6
Y1
0.5
0.4
0.3
0.2
0.1
0.0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
X1
In this design problem the driving force for separation is very small. The equilibrium curve is very
close to the diagonal. Since the top and bottom product composition is very close to unity, it is very
difficult to mark the points on the graph. So determination of theoretical stage by graphical method
is difficult in this case.
Based on the basic logic of the McCABE and THIELE method, a computer program is written in
Turbo-C language. The logic is given bellow.
36
The equation of the equilibrium line is determined by polynomial curve fitting. The
equation and the R2 value is given above. The position of the points required for drawing
the graph were determined by solving equilibrium line equation and q-line equation.
The equation of the connecting lines between the two points (mentioned above in 1. & 2.)
was determined. The intercept of the line with y-axis was determined and from there the
minimum reflux ratio was calculated.
The actual reflux ratio was determined and the operating line equation was generated.
Then the values of L, G, q, L, G were calculated using the following equations and the
striping section operating line equation was stablished.
L=R.D ………………………………………………………………………………….(5.4)
G=D(R+1) ……………………………………………………………………………….(5.5)
L=qF+1 ………………………………………………………………………………….(5.6)
G=F(q-1)+G ……………………………………………………………………………..(5.7)
The mathematical logic behind staircase construction is employed in the program to
calculate number of theoretical stage separately in top and bottom section to get an idea
about the feed tray location. The program section for enrichment section will terminate
when calculated x value crosses the feed composition. Similarly program section for
striping section will terminate when calculated x value crosses the residue composition. The
program is shown below.
37
#include<stdio.h>
#include<conio.h>
#include<math.h>
main()
{
intn,b;
float m1,m2,c1,c2,a,x,y;
printf("\n enter the slope of the operating line of the enriching section:");
scanf("%f",&m1);
printf("\n enter the intersect of the operating line of the enriching section:");
scanf("%f",&c1);
printf("\n enter the slope of the operating line of the stripping section:");
scanf("%f",&m2);
printf("\n enter the intersect of the operating line of the stripping section:");
scanf("%f",&c2);
n=1;
y=0.9981;
x=0.9981;
while(x>0.8895)
{
x=(1.415-(sqrt((1.415*1.415)-(4*0.428*y))))/(2*0.428);
a=y;
y=(m1*x)+c1;
n=n+1;
}
y=a;
printf("\n the no of top tray is= %d",n);
b=n;
while(x>0.0755)
{
x=(1.415-sqrt(1.415*1.415-(4*0.428*y)))/(2*0.428);
y=(m2*x)+c2;
n=n+1;
}
printf("\n the calculated theoritical stages are= %d",n);
n=n-b;
printf("\n the no of bottom tray is= %d",n);
getch();
}
38
STEP 2: DETERMINATION OF NUMBER OF ACTUAL TRAY
We have to determine or assume the overall column efficiency to calculate the number of actual
stage. If the efficiency is η, then number of actual tray is given by,
Actual tray = (theoretical tray / η) ……………………………………………………………..(5.8)
STEP 3: COLUMN SIZING [17]
Determination of column diameter: (All the calculations are done on the basis of operating
conditions ) 1. Maximum liquid rate (Lw) in Kg/sec.
Lw = (liq flow rate in Kgmol/hr.. *Molecular Weight) / 3600 …………………….......(5.9a)
2. Maximum vapour rate (Vw) in Kg/sec.
Vw = (Vapour flow rate in Kgmol/hr.. *Molecular Weight
)/3600……………………………….(5.9b) 3. Assume tray spacing in meter
4. Flow Factor (Flv).
√ ……………….(5.10)
5. Assume:
a. Hole diameter (dh)
b. Hole Area= (3.14*dh2)/4.
c. Plate thickness.
d. Weir height (hw).
e. Downcomer area (Ad).
6. Find Fair’s co-efficient (K), From graph find k1,then K = k1 ( Ϭ
/.02)0.2……………………..(5.11)
7.Find flooding velocity
Flooding velocity (uf) = K [(ρv-ρl)/ρv]0.5……………………………………………………..(5.12)
8. Assume % flooding.
9. Find actual velocity assuming % flooding.
a. Actual velocity (ut) = uf* % flooding
b. Volumetric flow rate = Vw/ρv.........................(5.13)
c. Net flow area = (Flow rate/actual velocity)
……………………………………………………(5.14) d. Column area = (Net area * 100 ) / (
100%- allowance) …………………………………(5.15)
e. Diameter = [(column area *4)/3.14]0.5 ……………………………………………………(5.16)
10. The column diameter is rationalized with respect to that available in the market
11. Recalculate:
39
a. Column area (Ac) = (3.14*d2)/4 …………………………………………………….(5.17)
b. Net area (AO) = Ac* % allowance ……………………………………………………(5.18)
c. Down comer area (Ad) =Ac *% down comer area ……………………………………(5.19)
d. Active area (Aa)= Ac – 2Ad
e. Hole area (Ah) = Ac* % hole area.
f. Superficial velocity (uo) = (volumetric flow rate / net area) ……………..……………(5.20)
g. Find Lw/Dc from the graph
Weir length, lw =value from graph *Dc …………………………………………………(5.21)
Step 3: Calculation of %flooding
% flooding = (uo /ut)*100
STEP 4: ENTRAINMENT CHECKING
Read the value of from the graph . For sieve tray, it must be less than 1. If entrainment is large, increase
the tray spacing & lower the vapour velocity & recalculate. If % flooding > 95% or < 70% , change the
tray spacing ,active area and recalculate.
STEP 5: WEEPING CHECKING
a) Find weir liquid crest (how): how = 750 [Lw/(ϼl*lw)]2/3 ………………………………….(5.22)
b) Assume hw.
c) Find K from the graph.
d) Find minimum vapour velocity (Uh):Uh = [K- 0.9 (25.4-dh)] / (ϼv)0.5………………(5.23)
e) Check whether uh > uh (min). If uh < uh (min),decrease the hole area & recalculate.
STEP 6: CALCULATION OF TRAY PRESSURE DROP
a) Find Co from fig.
b) Find dry tray pressure drop, hd.
hd =51(uh/Co)2*(pv/pl) ….............................(5.24)
c) Find residual head, hr.. = (12.5* 103)/pl……………………………………….(5.25)
d) Find total pressure drop, ht = hd + ( hw + how) +
hr..………………………………………..(5.26) e) Check whether it is acceptable or not. If the
pressure drop is beyond the tolerance level, increase the tray spacing and recalculate.
STEP 7: CHECK DOWN COMER BACK UP
a) Assume apron height, hap = (hw-10)
b)Calculate the clearance area (Aap) under the down comer.
Aap=hap×lw ……………………………………………………………(5.27)
c) Find head loss for flow thr..ough this clearance ,hdc.
hdc = 166 [Lwd/(ϼl* Aap)]2…………………………………………..(5.28)
d) Find down comer back up, hb
40
hb= (hw+how)+ht+hdc………………………………………………..(5.29)
STEP 8: CALCULATION OF FROTH HEIGHT
To be on the safer side, it is taken as twice the down comer back up. Thus, Fb= 2*hb…(5.30)
STEP 9: CALCULATION OF DOWNCOMER RESIDENCE TIME
Down comer residence time, tr= (Ad*hb*ϼl)/Lwd…………………………………….(5.31)
To get most efficient design, all the calculations are to be repeated to get minimum column
diameter and minimum tray spacing.
5.5 DESIGN COMPUTATION (PROCESS)
S/L No Variables Top portion Bottom portion

1 Temperature ( ) 159.7 179.8
2 Pressure (kg) 3 3
3 Vapour flow rate (Kmol/hr.) 27.81 27.81
4 Liquid flow rate (Kmol/hr.) 19.46 28.93
5 Vapour Mass Flow rate, kg/s 0.7724 0.7724
6 Liquid mass Flow rate, kg/s 0.5404 0.7884
7 Vapour density (Kg/m3) 8.173 7.666
8 Liquid density (Kg/m3) 656.89 687.39
9 Surface tension (dyne/cm) 10.394 11.115
10 Surface tension (N/m) 0.010394 0.011115
STEP 1: CALCULATION OF THEORETICAL STAGE

The numbers of theoretical stages are calculated by computer programming which are given below.
No. of tray (top): 28
No. of tray (bottom): 16
Feed enters at 29th tray from top.
Total no. of tray: 45
The computer output is shown below.
41
STEP 2: DETERMINATION OF NUMBER OF ACTUAL TRAY
Overall column efficiency is assumed 85% [18]
From eqn. (5.8) Actual tray (top): 33
Actual tray (bottom): 19
Feed enters at 34th tray from tray.
Total no. of tray: 53
STEP 3: COLUMN SIZING
Determination of column diameter
1. From eqn. (5.9a) Maximum liquid rate (Lw) in Kg/s = 0.07724.
2. From eqn. (5.9b) Maximum vapour rate (Vw) in Kg/s = 0.7884.
3. Tray spacing is assumed 0.5 m.
4. From eqn. (5.10) Flow Factor (Flv),
Flv (top) = 0.07804
Flv(bottom) = 0.1077
5. Assumed:
a. Hole diameter (dh) = 5 mm
b. Fractional Hole Area= 0.1
c. Plate thickness = 5 mm
d. Weir height (hw) = 50 mm
e. Fractional Downcomer area (Ad) = 0.12
6. From graph k1 = 0.08 (top) and 0.079 (bottom)
Then from eqn. (5.11), K = 0.071 for both top and bottom.
42
7.From eqn. (5.12),
Flooding velocity (uf) (top) = 0.635 m/s,
Flooding velocity (uf) (bottom) = 0.667 m/s
8. Assume velocity as 75% of flooding velocity.
9. Actual velocity:
a. Actual velocity (ut) (top) = 0.476 m/s,
Actual velocity (ut) (bottom) = 0.50 m/s
b. Volumetric flow rate (top) = 0.0945m3/S,
Volumetric flow rate (bottom) = 0.100m3/S
c. From eqn. (5.14) Net flow area (top) = 0.198m2
Net flow area (bottom) = 0.201m2
d. From eqn. (5.15) Column area (top) = 0.2256m2
Column area (bottom) = 0.2290m2
e. From eqn. (5.16) Diameter (top) = 0.535 m
Diameter (bottom) = 0.54 m
13. The column diameter is rationalized with respect to that available in the market. And the
diameter is selected 0.55 m for both top and bottom.
Recalculation:
a. From eqn. (5.16) Column area (Ac) (top) = 0.2290m2
Column area (Ac) (bottom) = 0.2290m2
b. From eqn. (5.18) Net area (Ao) (top)=0.2290 m2
Net area (Ao) (bottom)=0.2290 m2
c. From eqn. (5.19) Down comer area (Ad) (top) = 0.0285m2
Down comer area (Ad) (bottom) = 0.0285m2
d. Active area (Aa) (top) = Ac – 2Ad = 0.172m2
Active area (Aa) (top) = Ac – 2Ad = 0.172m2
e. Hole area (Ah) (top) = 0.0180m2
Hole area (Ah) (bottom) = 0.0180 m2
f. Single hole area (top and bottom) = 19.635 mm2
Number of holes (top and bottom) = 920
g. From eqn. (5.19) Superficial velocity (uo) (top) = 0.452 m/s
Superficial velocity (uo) (top) = 0.482 m/s g.
Weir length, lw (top) = 0.42 m
Weir length, lw (bottom) = 0.42 m
STEP 3: CALCULATION OF %FLOODING

43
Actual % flooding (top) = 71.2 %
Actual % flooding (top) = 72.3 %
The % flooding is in between 95% and 70%, so the result is satisfactory
STEP 4: ENTRAINMENT CHECKING
From eqn. (5.10) Flow Factor (Flv),

Flv(top) = 0.078
Flv(bottom) = 0.107
The value of the fractional entrainment from the graph corresponding to flood% is determined.
Entrainment factor (top): 0.029 Entrainment factor (bottom): 0.018 So the entrainment is less than
0.1
STEP 5: WEEPING CHECKING
a) From eqn. (5.22)

Weir liquid crest (how) (top) = 11.73 mm liq.
Weir liquid crest (how) (bottom) = 14.64 mm liq.
b) Weir height hw is assumed 50 mm for both top and bottom.
c) From the graph, K (top) = 30.6 K (bottom) = 30.7
d) From eqn. (5.22) Minimum vapour velocity (uh) (top) = 5.23 m/s
Minimum vapour velocity (uh) (bottom) = 5.58 m/s
e) Actual hole vel - weep velocity (top) = 4.20 m/s
Actual hole vel - weep velocity (top) = 4.36 m/s
So uh is greater than uh (min) and therefore the result is satisfactory.
STEP 6: CALCULATION OF TRAY PRESSURE DROP
a) Co from fig. = 0.79 (for both top and bottom)

b) From eqn. (5.24) Dry tray pressure drop, hd(top) = 27.59 mm liq.
Dry tray pressure drop, hd(bottom) = 28.11 mm liq.
c) From eqn. (5.25) Residual head, hr..(top) = 19.09 mm liq.
Residual head, hr..(bottom) = 18.11 mm liq.
d) From eqn. (5.26)
Total pressure drop, ht(top) = 108.35 mm liq.
Total pressure drop, ht(bottom) = 110.94 mm liq.
e) The plate pressure drop is within the acceptable limit. So, further modification is required.
STEP 7: CHECK DOWN COMER BACK UP
44
a) Apron height, hap is assumed 45 mm for both top and bottom.
b) From eqn. (5.27)
The clearance area (Aap) under the down comer (top & bottom) = 0.0189 m2.
c) From eqn. (5.28) Head loss for flow thr..ough this clearance, hdc(top) = 0.314 mm liq.
Head loss for flow thr..ough this clearance, hdc(bottom) = 0.610 mm liq.
d) From eqn. (5.28) Down comer back up, hb(top) = 170.4 mm liq.
Down comer back up, hb(bottom) = 176.2 mm liq.
STEP 8: CALCULATION OF FROTH HEIGHT
From eqn. (5.28) Froth height (top) = 340.8 mm liq.

Froth height (bottom) = 352.4 mm liq.
Tray spacing – Downcomer backup (top) = 159.2 mm
Tray spacing – Downcomer backup (bottom) = 147.6 mm
So the design is safe to avoid flooding.
STEP 8: CALCULATION OF DOWNCOMER RESIDENCE TIME
From eqn. (5.28) Down comer residence time, tr(top) = 6.33 sec.
Down comer residence time, tr(bottom) = 4.4 sec.
This is greater than 3 sec. So the result is satisfactory
45
5.6 DESIGN METHEDOLOGY (MECHANICAL)
STEP 1: CALCULATION OF DESIGN PRESSURE AND DESIGN TEMPERATURE [19]
Design pressure= operating pressure + 20% allowance

Design temperature = operating temperature + 10% allowance
STEP 2: SELECTION OF MATERIAL OF CONSTRUCTION
STEP 3: CALCULATION OF SHELL THICKNESS [19]
Shell thickness, mm
( )
Where, P' = Design pressure

D=Shell inner diameter
S= Allowable stress
J= Weld joint efficiency
Set Corrosion allowance and determine final thickness,
t'=t+(corrosion allowance/1000) m
Rationalize the thickness obtained according to availability, t"
STEP 4: CHECK WHETHER THE THICKNESS OBTAINED CAN WITHSTAND THE LOAD OF
WHOLE TOWER [19]
Select insulation material & insulation thickness,i

Dead weight calculation
Outer diameter of the shell=D=d+(2*t") m
Outer radius of the shell=R=(D/2)
Inner radius of the shell= r =(d/2)
Dia including the insulation= D’= D+(2*i) m
Radius including the insulation=R’=(D’/2)
Density of the shell material=ρ
Density of insulating material=ρ’
Tray thickness, c = 0.005 m
Tray spacing, s = 0.5 m
Weight of torispherical top, w1 = ((π*D2/4)*t"*ϼ*1.7) kg
Weight of insulation, w2 = ((π*D’^2/4)*i*ρ’*1.7) kg Dead weight,
W = (w1 + w2) kg
Calculation of weight per unit length
Weight of shell/unit length= (π*(D^2-d^2)/4)*ρ
46
Weight of insulation/unit length=(π*(D’^2-D^2)/4)*ρ’
Weight of liquid/unit length= ((π*d^2)/4)*density
(use the larger density between water and the fluid handled)
Assume weight of external affixes/unit length
Weight of tray/unit length= ((π*d^2)/4)*c*ρ)/s
Actual tray weight/unit length= (Weight of tray/unit length)*1.3
Total weight /unit length, w= a) + b) + c) + d) +f)
Calculate total compressive force at a distance of x from top.
Compressive stress=( ) ( )
Calculation of axial stress

Axial stress= (r*(Pin-Pout))/(2*t)
Calculation of net tensile stress
Net tensile stress = axial stress – compressive stress
Calculation of wind load
Velocity of air = V= 300km/hr. = 83.33 m/s (assumed)
Density of air = ρ(air) = 1.126 kg/m3 (at 30oC & 1 atm)
Cd=0.44 in turbulent region Effective projected area,
A= 1.2*(D’*x) (allowing 20% excess for additional features)
Wind force, Fw= (Cd*A*ρ(air)*V^2)/2
Bending moment at a height x from top, BM=(Fw/2)*x^2
Moment of inertia, MI= π*r’*t
Where r’ = average column radius
Wind stress= (BM*R/MI)
Total compressive stress
Total compressive stress for windward side –
wind stress – net tensile stress = allowable stress
Total compressive stress for leeward side—
wind stress + net tensile stress = allowable stress
Find the distance x from top up to which the calculated thickness can be used by solving these two
equations. If the distance is less than the total column height, then the calculated is to be repeated
substituting x by (x-distance obtained from above solution)
STEP 4: CALCULATION OF SEISMIC LOAD [20]
Total height of the column, h = (no. of tray*s) + (1+1.5)m

Modulus of elasticity, E = 27990000 psi
47
Acceleration due to gravity, g = 32.2 ft/s2
Moment of inertia, m = π*((((D+d)/2)/2)^3)*t
Period of vibration, n = (2*π*((w8*h4))/(E*32.2*(m/(0.30484))))^0.5)/3.53 sec.
Seismic co-efficient, e = 0.08
Maximum bending stress, b = (8*e*w8*h2)/(π*R2*t) psi
Weight of column, w9 = w8*h kg Dead weight stress,
Ws = w9*9.81/(π*ds)
Seismic stress, S = (2*e*w9)/(3*π*R) psi
STEP 5: CALCULATION OF TORISPHERICAL HEAD[19]
Thickness of head=
Where C=corrosion allowance =0.118,

S=max. allowable stress=17114.51psi,
E=weld joint efficiency=0.85,
P= design pressure=42.67psi,
rc= crown radius=71.5
STEP 6: NOZZLE DIA CALCULATION [19]
Nozzle dia, Dopt (mm) =
Where,
G= Mass flow rate = volumetric flow rate × density
d= density, kg/m3
STEP 7: GASKET DESIGN
Design equation: √ ( )
Where,
d0 = outer diameter of the gasket
di= inner diameter of the gasket = 10 mm greater than the outside dia of shell
Y = minimum yield stress
m = gasket factor
P = design internal pressure
Actual gasket width N= (d0- di)/2
Basic seating width=N/2
G= diameter at location of gasket load reaction G= di+N
48
STEP 8: BOLT DESIGN
Determination bolt load due to design pressure:

Design equation: H = (3.142 G2 P)/4
Where,
H = total hydrostatic end force, P = design pressure
Determination of load to keep joints tight under operating condition:

Design equation: Hp = (3.14 G 2b m P)/4
Where,
HP = load to achieve adequate compression of gasket under operating condition
G = diameter of location of gasket load
2b= effective gasket pressure width
Total operating load:
Design equation: Wo = H + Hp
Determination of bolt load under bolting up condition :

Design equatio :Wg = (3.14 G b Y)
Where,
b = effective gasket seating width = 0.24 ft
Y = minimum gasket seating stress
Determination of minimum bolting area:

If A0 is the bolt area required under operating condition and Ag is the area required under bolting up
condition then,
Design equation: A0 = W0/S0 & Ag = Wg/Sg
Where,
S0 = allowable stress for bolting material at design temperature
Sg = allowable stress for bolting material at atm temperature
Among A0 and Ag , greater is selected.
STEP 9: FLANGE CALCULATION
Flange outside diameter (A) = [C + d +25] mm
Where,
d = bolt diameter
C = bolt circle diameter
Flange thickness can be calculated by,
49
Bs=2d+ 6t/ (m+0.5)
Where,
Bs= bolt spacing
d = bolt diameter
t= flange thickness
m=gasket factor
5.7 DESIGN COMPUTATIONAL (MECHANICAL)
STEP 1: CALCULATION OF DESIGN PRESSURE AND DESIGN TEMPERATURE
Design pressure= 3.48 atm

Design temperature = 1980C
STEP 2: SELECTION OF MATERIAL OF CONSTRUCTION
Material of construction: Grade 2B of IS 2002-1962 [21]

Specification of alloy steel: C% (max): 0.22
Si% : 0.10-0.35
S% (max): 0.050
P% (max): 0.050
Designation: Grade 2B
STEP 3: CALCULATION OF SHELL THICKNESS
Allowable stress, S = 118000000 N/m2 = 1.18 × 1014N/mm2

Weld joint efficiency=0.85 (for double welded butt joint with full penetration)
Shell thickness, t = 1mm
Corrosion allowance = 3mm
Final thickness, t' = 4 mm
Rationalized thickness, t"= 6 mm
STEP 4: CHECK WHETHER THE THICKNESS OBTAINED CAN WITHSTAND THE LOAD OF
WHOLE TOWER
Insulation material & insulation thickness, i

Felt wool is selected as insulating material and insulation thickness is 5 cm.
Dead weight calculation
Outer diameter of the shell=D=0.562 m
Outer radius of the shell=R= 0.281 m
Inner radius of the shell= r = 0.275m
50
Dia including the insulation= D’= 0.656 m
Radius including the insulation=R’= 0.0.328 m
Density of the shell material=7850 kg/m3
Density of insulating material=332.31kg/m3
Tray thickness, c = 0.005 m
Tray spacing, s = 0.5 m
Weight of torispherical top, w1 = 19.44 kg
Weight of insulation, w2 = 9.5 kg
Dead weight, W = 28.94 kg
Calculation of weight per unit length
Weight of shell/unit length= 40.91 kg/m
Weight of insulation/unit length= 31.63 kg/m
Weight of liquid/unit length= 237.6 kg/m
(Density of water is used since it is more than that of process fluid handled)
Weight of external affixes/unit length= 50 kg/m is assumed
Weight of tray/unit length= 88.74 kg/m
Actual tray weight/unit length= 18.65 kg/m
Total weight /unit length, w= 467.53 kg/m
Calculation of total compressive force at a distance of x from top.
CS area without corrosion allowance= 0.008 m2
Compressive stress, kg/m2= 3617.5 + 58411.25x
Calculation of axial stress
Axial stress, kg/m2= 359223.57
Calculation of net tensile stress
Net tensile stress, N/m2 = 355606.07 – 58411.25x
Calculation of wind load
Velocity of air = V= 300km/hr.. = 83.33 m/s (assumed)
Density of air = ρ(air) = 1.126 kg/m3 (at 30oC & 1 atm)
Cd=0.44 in turbulent region
Effective projected area,m2/m, A= 0.285 (allowing 20% excess for additional features)
Wind force/unit length,N/m, Fw= 1961
Bending moment at a height x from top, Nm, BM= 980.5x2
Moment of inertia, m4, MI= 0.0008
Wind stress, N/m2= 340723x2
Total compressive stress
Total compressive stress for windward side 340723x2+58411.25x -355606.07 = 118000000
51
Total compressive stress for leeward side – 340723x2-58411.25x +355606.07 = 118000000
Solving these two equations we get the lowest possible real solution of x
x= 18.5 m.
Since the value obtained is less than total column height, we have to repeat the procedure. The
recalculation shows for rest of the tower we can use next higher shell thickness of 8mm. So the final
inference is we will use 6mm thick shell from top to 19m. After that up to the bottom 8mm shell
thickness is to be used.
STEP 5: CALCULATION OF SEISMIC LOAD
Total height of the column, h = 27.5 m

Modulus of elasticity, E = 27990000 psi
Acceleration due to gravity, g = 32.2 ft/s2
Moment of inertia, m = 8.6×10-5
Period of vibration, n = 35 sec.
Seismic co-efficient, e = 0.08
Maximum bending stress, b = 34979.37 psi
Weight of column, W9= 41676.83 kg
Dead weight stress, WS= 325.41 N/mm2
Seismic stress, S = 3.83psi = 26406.9 N/m2
So the seismic stress is less than the allowable stress.
STEP 6: CALCULATION OF TORISPHERICAL HEAD
Head Type: Torispherical Thickness (top) =12mm

Thickness (bottom) =16mm
STEP 7: NOZZLE DIA CALCULATION
Top nozzle dia. for vapour outlet = 120 mm,

Thickness = 8 mm
Top nozzle dia. for reflux inlet = 26.64mm,
Thickness = 6.88 mm
Bottom nozzle dia. for reboiler inlet =120 mm,
Thickness = 8 mm
Bottom nozzle dia. for residue outlet = 26.64 mm,
Thickness = 6.88 mm
Nozzle dia for feed inlet= 15.8 mm,
Thickness = 5.54 mm
52
The written values are rationalized [19]
STEP 8: GASKET DESIGN
Material of construction: compressed asbestos sheet and various metallic reinforced sheets and
clothes (IS-2825-1969)
Y=25x106N/m2
m=2.75
P= 2.941x105N/m2
d0/di=1.0614
di= 0.566 m
d0= 0.570 m
Actual gasket width N= 2 mm
Basic seating width= 1 mm
Diameter at location of gasket load reaction= 0.568 m
STEP 9: BOLTING CALCULATION
Material of construction: Hot rolled carbon steel

Determination of bolt load due to design pressure:
Total hydrostatic end force, H= 3.58×105 N
Determination of load to keep joints tight under operating condition:
Load to achieve adequate compression of gasket under operating condition, Hp=6923.45N.
Total operating load:
Minimum bolt load under bolting up condition, W0=3.64×105 N
Determination of bolt load under bolting up condition:
Wg= 89176 N.
Minimum theoretically bolt area:
A0 =0.006 m2
Selection of bolts:
Bolt size =M 20×2
Root area=0.0002 m2
Flange thickness =20mm
Hub thickness =0.5x20mm=10mm
Bolt spacing=50 mm
No. of bolts=32 nos. (To achieve uniform tightening, the no of bolts should be in multiple of 4).
Bolt circle diameter, C = 0.509 m
53
Optimum bolt diameter = 20 mm
STEP 10: CALCULATION OF FLANGE
Material of construction: carbon steel Specification: IS-2856-1964

Flange thickness, t= 5.41 mm
Rationalized Thickness of flange =20mm [19]
STEP 10: SUPPORT DESIGN
Type of support: Skirt support
ASPECTS NOT ADDRESSED
1. The detailed process and mechanical design of the condenser and reboiler is not included in this
design report.
2. Control and instruments for the equipment is not discussed here.
3. Safety and environmental aspects is not discussed.
4. Operational features are not discussed.
5. Detail support and foundation design is not included.
54
6. DESIGN DATA SHEET
Column Tray Data Sheet Equipment no.(tag)
Description(func.)
Sheet no.
Operating Data TOP BOTTOM OR TOP AND BOTTOM
TOWER INSIDE DIAMETER(mm) 550 550 550
TRAY SPACE(mm) 500 500 500
TOTAL TRAYS IN SECTION 33 19
Internal Conditions at Tray Number
VAPOR TO TRAY
RATE(kmol/hr.) 27.81 27.81
DENSITY(kg/m3) 8.173 7.666
PRESSURE(atm.) 3.48
TEMPERATURE (K)
LIQUID FROM TRAY
RATE(kmol/hr.) 19.46 28.93
DENSITY(kg/m3) 656.89 687.39
TEMPERATURE
VISCOSITY
NUMBER OF LIQ FLOW PATHS
Technical / Mechanical Data
TRAY MATERIAL Carbon steel
TRAY THICKNESS (mm) 5
CAP MATERIAL Carbon steel
HOLDDOWN MATERIAL Carbon steel
NUTS AND BOLTS MATERIAL Hot rolled Carbon steel
SUPPORT RING MATERIAL Carbon steel
SUPPORT RING SIZE 60
DOWNCOMER BOLT BAR THICKNESS
CORROSION ALLOWANCE nil
TRAYS
TOWER ATTACHMENTS
TRAYS NUMBERED FROM TOP TO
BOTTOM
TRAY MANWAY REMOVAL FROM
DATE OF ENQUIRY DATE OF ORDER

ORDER NO. DRG NO.
MANUFACTURER `
NOTES
(1) INTERNAL VAPOUR AND LIQUID LOADINGS AT THE LIMITING SECTION ARE REQUIREDTO ENSURE
PROPER TRAY DESIGNS.
DENSITIES ARE REQUIREDAT ACTUAL INSIDE TOWER CONDITIONS OF TEMPERATURE AND PRESSURE.
VISCOSIY IS NOT REQUIRED UNLESS GREATER THAN O.7 Cp.
(2) CROSS OUT DIMENSION UNITS WHICH DO NOT APPLY TRAY SUPPLIES TO ADVISE
REMARKS
55
7. NOMENCLEATURE
A= area
Aa= Active area
Ac = column area
Ad = down comer area
Aeff= effective area
Ah = tray deak full open hole area
An = net area
Cp=specific heat
d = diameter
D, ρ = density
Fdl= Stress due to dead load
Flv = flow factor
g = gravitational constant
G, L = gas and liquid flow rate
Hi = enthalpy of ith stream.
hw= weir height
Lwi= weir length n=number of moles
Pc, Tc = critical pressure and temperature
Psat, Tsat = saturation pressure and saturation temperature
Pvp = vapour pressure
QB= reboiler load
Qc = condenser load
r = radius
R= optimum reflux ratio.
R= reflux ratio
Rm= minimum reflux ratio.
t = actual thickness of the plate
th= skirt thickness
W= residue flow rate
Wex= weight of external connections
Wh= weight of head
Wh= weight of head
Wint= weight of column internal
Wl= weight of liquid inside the column
56
Ws= weight of shell
Wtot = total weight to be supported
X1 = liquid mole fraction
Y1= equilibrium vapour mole fraction
α = relative volatility
η = overall column efficiency
ν = stoichiometric coefficient
σ = surface tension\
57
8. REFERENCES
1.Ullmann’s ―Encyclopedia of Industrial Chemistry‖, Vol. 18, p. 735, 6th edition (2003), Wiley-
VCH
2. J.J. McKetta, ―Encyclopedia of Chemical Processing and Design‖, Vol. 30, p. 50, 1st edition
(1989), Marcel Dekker Inc.
3. K. Schmitt, ―New acetone chemistry in Germany‖, Chem. Ind. Int., p. 204 (September 1966)
4. S.I.D.A. U.S. Patent 3,802,999 (October 31, 1961); Shell Development Co., U.S. Patent
2,344,226 (March 14, 1944)
5. Esso Research and Engineering Co., U.S. Patent 3,361,828 (January 2 , 1968)
6. Nippon Sekiyu, British Patent 968,151 (July 2, 1964)
7. McAllister et al., Shell Development Co., U.S. Patent 2,130,592 (September 20, 1938)
8. Esso Research and Engineering Co., U.S. Patent 3,153,068 (September 13, 1964)
9.Kgowa Hakko Kogyo, U.S. Patent 3,449,435 (June 10, 1969)
10.Scholven-Chemie, U.S. Patent 3,361,822 (January 2, 1968)
11. Shell Oil, U.S. Patent 3,374,272 (March 19, 1968)
12.R.M. Felder, R.W. Rousseau, ―Elementary Principles of Chemical Process‖, 3rd edition (2000),
John Wiley & Sons. Inc.
13. B.E. Pouling, J.M. Pransnitz, J.P. O’Connell ―Properties of Gases and Liquids‖ , 5th edition
(2000), McGraw-Hill.
14.J.M.Smith, H.C.Van Ness, M.M. Abbott, ―Chemical Engineering Thermodynamics‖, 6th
Edition, Tata-McGraw-Hill Edition.
15.C.L.Yaws, ―Chemical Properties Handbook‖, 5th edition, 1999
16. Robert .E. Treybal , ― Mass Transfer Operation‖,3rd edition.
17.Sinnot, R. K., ―Coulson Richardson’s Chemical Engineering‖, Vol-6,2nd Edition, Asian books
Private Ltd.
18. Perry R.H. Chemical Engineers Handbook – McGraw Hill Ltd. 5th Edition.
19. B.C Bhattacharya, ―Introduction to Chemical Equipment Design‖, 1st edition, Reprint, CBS
Publishers.
20. L.E. Brownell and E.H. Young, ―Equipment Design‖, Wieley Eastern Limited, New Delhi.
21. IS 2002-1962
22. Kirk Othmer, ―Encyclopedia of Chemical Technology‖, Vol. 1, p. 190, 3rd edition (1978), John
Wiley & Sons. Inc.
58

Plant Design of MIBK

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Plant Design of MIBK

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Table of Contents

1.1PHYSICAL PROPERTIES ........................................................................................................1

2. MANUFACTURING PROCESS ....................................................................................................4

2.1 PROCESS SELECTION ...........................................................................................................4

2.2 OVERALL PROCESS DESCRIPTION ...................................................................................6

3. MATERIAL BALANCE .................................................................................................................9

4. ENERGY BALANCE ...................................................................................................................16

5. EQUIPMENT DEIGN ...................................................................................................................31

5.1 LIST OF ITEMS TO BE REPORTED ....................................................................................31

5.2 AVAILABLE INFORMATION .............................................................................................31

5.3 ADDITIONAL INFORMATION ...........................................................................................31

5.4 DESIGN METHODOLOGY...................................................................................................35

5.5 DESIGN COMPUTATION (PROCESS)................................................................................41

5.6 DESIGN METHEDOLOGY (MECHANICAL) .....................................................................46

5.7 DESIGN COMPUTATIONAL (MECHANICAL) .................................................................50

6. DESIGN DATA SHEET ...............................................................................................................55

Dehydration of DAA to MO:

2.2 OVERALL PROCESS DESCRIPTION

Production rate of MIBK:

1. HYDROGENATION REACTOR (MIBK REACTOR):

H2 required: (8.4167/0.95)kmol/hr. = 8.8596 kmol/hr. = 17.19kg/hr.

Excess H2 in outlet: 8.8595 ×0.05 kmol/hr. = 0.4429 kmol/hr. = .8859 kg/hr.

MO in inlet: 868.24 + (84.68 – 43.413) kg/hr. = 910 kg/hr.

2. DEHYDRATING COLUMN (MO REACTOR):

4. ACETONE RECOVERY COLUMN:

8 wt.% H2O2 solution = 5.7 vol% solution.

10 wt.% NaOH solution = 8.9 vol% solution.

H2O2 solution required: 6.59 L

NaOH solution required: 6.59 L

of the aqueous phase: (181.05 + 6.755 + 6.655) kg/hr. = 194.46 kg/hr.

H2O2 solution 6.755 6.755

8. HYDROGENATION REACTOR (MIBK REACTOR):

9. 1ST PURIFICATION COLUMN:

11. ACETONE RECYCLED STREAM:

Compound mi (kg/hr.) niHi (kJ/s) mo (kg/hr.) noH0 (kJ/s)

Acetone 11993.37 ? 10895.01 ?

Water 24.13 ? 34.06 ?

nH values are calculated by the expression, n× H = m× Cp× ΔT

3. ACETONE RECOVERY COLUMN:

4. DEHYDRATING COLUMN (MO REACTOR):

Saturation temperature of mixture is determined using the formula Tsat = ∑ Tisat × xi

7. HYDROGENATION REACTOR (MIBK REACTOR):

nH values are calculated by the expression, n× H = m× Cp× ΔT

8. 1ST PURIFICATION COLUMN:

Component Feed Top Bottom

Description Heat input (kJ/hr.) Heat output (kJ/hr.)

Top Outlet stream [14A] 2151.69

Bottom Outlet stream [15] 132831.34

Total 173928.6 173928.6

9. FINAL PURIFICATION COLUMN:

Massflow rate Massflow rate Massflow rate

MO 102.41 10.85 1.67 0.20 100.74 92.36

MIBK 841.66 89.15 833.33 99.80 8.33 7.64

The calculated VLE data are given below.

159.7 2.940000 1.870336 1 1

ρ(MIBK) at top temperature (159.7 )= 0.6567 g/ml

4. Flow Factor (Flv).

5.5 DESIGN COMPUTATION (PROCESS)

S/L No Variables Top portion Bottom portion

STEP 1: CALCULATION OF THEORETICAL STAGE

STEP 3: CALCULATION OF %FLOODING

STEP 4: ENTRAINMENT CHECKING

From eqn. (5.10) Flow Factor (Flv),