INTRODUCTION
Lactic acid, 2-hydroxyopropanoic acid, is the simplest
hydroxycarboxylic acid with asymmetric carbon atom:
CH3-CH-OH
COOH
Lactic acid occurs widely in nature, as the racemic form and as the
optically active acid. The primary uses of lactic acid are in foodstuffs
and in pharmaceutical products; a relatively small volume is used in
industrial applications. The main use of food-grade lactic acid is in the
manufacture of calcium and sodium stearoyl-2-lactylates for the
baking industry. It is also used as a preservative and a pickling agent.
It is used widely to adjust pH in diary products, beer, jams and jellies.
Technical-grade lactic acid has long been in use in the leather tanning
industry and in vegetable tanning.
Other non-food uses of lactic acid include applications in adhesives,
cleaning and polishing formulations, electroplating and
eletropolishing, insecticides and fungicides, plastics and resins and
textiles.
Some of the important physical properties of Lactic acid are listed as
below:
m.p. (pure optical isomers) = 53
o
C.
It is hygroscopic in nature and is normally obtained as a concentrated
1
solution, upto 90% (w/w) which is virtually colorless and odorless. It
is completely soluble in water, ethanol, diethyl ether.
This report is a pre-preliminary feasibility report on a project
involving the setting up of a plant to manufacture 10,000 TPA Lactic
acid from acetaldehyde.
2. EXECUTIVE SUMMARY
Product: Lactic Acid
Installed Capacity: 10,000 TPA
Location: Vadodara, Gujarat.
Raw Materials:
Material Requirement
(tons /ton of
product)
Cost
(Rs./ton)
Acetaldehyde 0.5316 20000
Acetone Cyanohydrin 0.94 95000
Utilities:
Utility Requirement
(per ton of
product)
Steam 1.00 ton
Cooling Water 57.77 m
3
Chilled Water 20.31 m
3
Project Cost Estimates:
2
Total Project Cost 531.02
Term Loan @ 14% p.a. interest 265.51
Total Equity 265.51
(All figures are in Rs. lakhs)
Product Price: Rs.1, 13,000/- per ton
Estimated Working Results:
Return on Investment = 77.95%.
Payback period = 15.4 months.
3. PROCESS SELECTION
The methods for the preparation of lactic acid fall in two groups:
1) Biochemical and
2) Chemical.
Lactic acid has in the past been available by fermentation processes
utilizing carbohydrates as raw material. This has been the major route
for production of lactic acid. Recently, a few chemical methods have
been developed for manufacture of lactic acid. These chemical
methods include hydrolysis of lactonitrile, carboxylation of
acetaldehyde, the alkaline degradation of sugar and a new method
from propene and nitrogen oxides with lactic acid nitrate as
intermediate.
The present report deals with manufacture of lactic acid from
acetaldehyde; so we will concentrate only on those routes for
manufacture of lactic acid that use acetaldehyde as the starting
3
material. Following 4 different routes are available for manufacture of
lactic acid from acetaldehyde:
1) The first process uses hydrogen cyanide as raw-material along with
acetaldehyde, resulting into the formation of lactonitrile, which is then
hydrolysed in presence of hydrochloric acid or PTSA as catalyst to
form lactic acid.
2) This route is similar to the first one, except that acetone
cyanohydrin is used as the raw-material instead of hydrogen cyanide.
The reaction between acetone cyanohydrin and acetaldehyde results
into the formation of lactonitrile as in the previous process, which is
then similarly hydrolysed to lactic acid, the final product.
3) Another route for lactic acid manufacture is through carboxylation
of acetaldehyde. This involves reaction of acetaldehyde with carbon
monoxide and water.
4) One more route starting from acetaldehyde employs an ion-
exchange catalyst. The reaction involves carbonylation of
acetaldehyde on ion-exchange catalyst like Lewatit-100.
Comparison between available routes:
While the first route employing hydrogen cyanide is useful and less
costly than the older fermentation process, it will be recognized that
there is danger and expense associated with the use of hydrogen
cyanide, and an alternate route is therefore desirable. Lactic acid is
widely used as a food ingredient. In particular, this route involves
4
cyanide which is highly poisonous and great care must be taken in the
manufacturing process to ensure that no cyanide remains in the final
product before it can be used as a food ingredient.
The reaction conditions, however, are not severe and the conversions
and selectivity resulting from the process are also very high:
Conversion = 97%.
The second route involving acetone cyanohydrin is comparatively
safer, as it does not involve hydrogen cyanide. Further, the
conversions resulting from the process are similar, and the process
conditions are also ambient. Conversion = 95%. However, there still is
some danger associated with the process, as acetone cyanohydrin has
tendency to dissociate into acetone and hydrogen cyanide.
The third route involving carboxylation of acetaldehyde has not yet
been commercialized. The first 2 routes are already being used for
manufacture of lactic acid. The main reason for the failure of this
route is the low conversion resulting
from the process. Attempts in the laboratory to use this particular
process have resulted only in traces of lactic acid. So, although the
process is very safe and easy to handle, it is not viable to be carried
out on an industrial scale.
The final route using ion-exchange catalyst is carried out at 60
0
C and
60-90 atmospheres to give lactic acid. However, the conversion from
5
this process is still lower than the previous one- only 2-3%.
Thus, considering all these aspects of the processes listed above, we
come to the conclusion that the second process involving the reaction
between acetone cyanohydrin and acetaldehyde is the best process for
manufacture of lactic acid.
4.PROCESS DESCRIPTION
The process selected for manufacture of acetaldehyde involves three
6
main steps:
1) In the first step, acetaldehyde is reacted with acetone cyanohydrin
to give lactonitrile.
2) In the second step, this lactonitrile is hydrolysed with the help of a
catalyst to give lactic acid.
3) The final step is the purification step, in which the crude lactic acid
obtained after second step is purified. This is done by esterification of
crude lactic acid to methyl lactate using methanol. Methyl lactate is
recovered, purified by distillation and hydrolysed by water in presence
of acid catalyst to produce lactic acid, which is further concentrated,
purified and methanol is recovered.
The final product is food grade 90% (w/w) lactic acid.
Reactions and details:
1) The reaction taking place in first step is:
Acetaldehyde + Acetone Cyanohydrin Lactonitrile
+ Acetone.
The above reaction takes place at 15
0
C and atmospheric pressure. It is
a liquid phase homogeneous reaction. A base catalyst can be used for
this reaction; however if acetone cyanohydrin dissociates into acetone
and hydrogen cyanide, then presence of hydrogen cyanide along with
base catalyst (NaOH) may create problems. Also, acetaldehyde is
known to be highly unstable in presence of NaOH, so use of NaOH
should be avoided. Hence, catalyst is not used in the present report; in
7
absence of catalyst, good conversion (95%) is obtained. The residence
time is approximately 25 minutes.
This reaction is carried out in a continuous stirred tank reactor, R101.
It is exothermic reaction with heat of reaction equal to 0.48 kJ/mol.
Acetone is formed as by-product, which can be recovered and then
sold.
The raw-materials acetaldehyde and acetone cyanohydrin are easily
available. Acetaldehyde is available in storage tanks equipped with
cooling facilities in order to keep the temperature below 15
0
C. So, we
can directly use acetaldehyde from the day tank to the main reactor,
through insulated pipeline. For acetone cyanohydrin, a heat exchanger
E101 is required in order to cool it to 15
0
C before feeding it to the
reactor.
Acetaldehyde is used in excess, while acetone cyanohydrin is the
limiting reactant. The output stream contains lactonitrile, acetone and
unreacted acetaldehyde.
This stream is then fed to distillation column D101 where
acetaldehyde and acetone are obtained as top products, while
lactonitrile is obtained as bottom product. The top stream is further fed
to another distillation column D102, in which acetaldehyde and
acetone are separated; recovered acetaldehyde is recycled.
2) Lactonitrile obtained from D101 is fed to the reactor R102. Water
is also fed to the reactor. PTSA (Paratoluene sulphonic acid) is used as
8
catalyst in this reaction. Reaction taking place is:
Lactonitrile + Water Lactic acid +
Ammonia.
Reaction is carried out at 60
0
C and atmospheric pressure. It uses
stirred tank reactor, R102. The output stream from R102 contains
lactic acid, water and solid catalyst. It is assumed that conversion of
lactonitrile is 100%. Ammonia from the reactor is fed to an ammonia
scrubber. The stream containing catalyst is fed to filter F101, where
the catalyst is separated.
3) This is the purification stage. Methanol is used for esterification of
lactic acid to methyl lactate. Lactic acid and methanol run in
countercurrent manner and the ester is carried out of the packed
column by the excess of alcohol vapors, which then are recirculated. It
is an exothermic reaction; heat liberated in reaction is used to vaporize
methyl lactate. The output stream from packed column,R103, contains
methyl lactate, water and excess of methanol. This stream is fed to
distillation column, D103,for separation. Methyl lactate and water,
coming as bottom product from this distillation column, are fed to the
next reactor, R104. Here, hydrolysis of methyl lactate takes place to
give pure lactic acid.
Stream coming out from R104 contains lactic acid, methanol and
water. It is fed to distillation column, D104. Lactic acid and water
9
come from bottom of the distillation column, and are fed to evaporator
so that required amount of water is vaporized and 90% (w/w) lactic
acid is obtained.
4. SITE SELECTION
Proposed Site: Vadodara, Gujarat.
The selection of site affects profitability as well as productivity of the
project. The following factors deciding site selection were examined:
1. Location with respect to marketing area:
Lactic acid is widely used as a food ingredient. The general use
pattern of lactic acid worldwide can be summarized by the following
table:
Used in: Percentage Use
Food and Beverage Industry 55
Chemicals (lactates, adhesives) 25
10
Plastics and textiles 15
Leather Processing 5
Total 100
As seen from the above table, it is clear that lactic acid is mainly used
in food and beverage industry. The present report hence deals with the
manufacture of food grade lactic acid.
Food industry is the main consumer of lactic acid. Due to the presence
of large number of food and beverage industries in Gujarat, setting up
of this plant in Gujarat naturally becomes a commercially viable
option.
In fact, there are already a few lactic acid manufacturers across India,
and food industries in Gujarat are dependent on these industries for
their demand of lactic acid. These manufacturers are:
i) Lactochem Limited, Chennai.
ii) Niphad Sahakari Sakhar Karkhana Limited, Nashik.
iii) Sangita Biochem Ltd., Mumbai.
However, transportation charges are incurred if lactic acid is bought
from one of these manufacturers for a food/beverage industry in
Gujarat. Hence, rather than setting up the plant in Mumbai or
elsewhere in Maharashtra, it would be wise to set up the plant in
Gujarat.
The next question is: where exactly in Gujarat should this plant be set
up?
2 Raw material supply :
11
The basic raw materials required are Acetaldehyde and Acetone
cyanohydrin.
Acetaldehyde is manufactured all over India, and will be easily
available.
However, acetone cyanohydrin has only one major manufacturer in
India: Gujarat State Fertilizers and Chemicals Limited, Vadodara,
Gujarat.
Also, Allied Chemical Corporation (ACC), Vadodara can easily
supply acetaldehyde.
Thus, raw-materials are available in plenty as well at reasonable prices
in Vadodara.
3. Transportation facilities:
The area is reasonably well connected by roadways and railways due
to the extensive development of infrastructure by the GIDC authorities
for the industrial belt. Facilities for the transportation of equipment
and for the travel of plant personnel are available. Several new
projects have received government approval for the improvement of
the transportation system.
4. Availability of labor :
Labor for plant construction and operation is available locally and
cheaply.
12
5. Availability of utilities :
The utilities water and power are supplied by the GIDC at reasonable
rates.
6. Availability of suitable land
There is no problem for acquiring land as it is an industrial zone. The
terrain is flat and the soil has a good bearing capacity. The topography
and meteorology of the site also permit normal dispersion of the air
borne pollutants.
8. Local community considerations :
Adequate housing, educational, recreational facilities are available
near the site.
9. Climate :
The region has a suitable climate and experiences moderate seasonal
rainfall. It is not prone to high winds.
10. Political and strategic considerations :
There are no restrictions on development of industry at the location as
it is allotted for industrial development. Besides above factors,
communication, industrial infrastructure, medical, fire-fighting
services are well available.
Thus, taking into consideration all the above factors, it is decided that
Vadodara, Gujarat would be the best site for the proposed project of
manufacture of lactic acid from acetaldehyde.
13
6. MATERIAL BALANCE
Basis: 1 hour.
1) R101:
Reaction:
Acetaldehyde + Acetone Cyanohydrin Lactonitrile
+ Acetone.
Conversion = 95%.
Component In(kg/hr) Out(kg/hr)
Acetaldehyde 578.95 28.95
Acetone Cyanohydrin 1062.5 0.0
Lactonitrile 0.0 887.5
Acetone 0.7 725.7
Total 1642.15 1642.15
2) D101:
Component In (kg/hr) Top Product
(kg/hr)
Bottom Product
(kg/hr)
Acetaldehyde 28.95 28.95 -
Acetone 725.7 724.75 0.95
Lactonitrile 887.5 - 887.5
Total 1642.15 753.7 888.45
3) D102:
14
Component In(kg/hr) Top Product
(kg/hr)
Bottom Product
(kg/hr)
Acetaldehyde 28.95 28.95 -
Acetone 724.75 0.7 724.05
Total 753.7 29.65 724.05
4) R102:
Component In(kg/hr) Out(kg/hr)
Lactonitrile 887.5 -
Lactic Acid - 1125
Water 645.54 195.54
PTSA (catalyst) 1.5 1.5
Ammonia - 212.5
Acetone 0.95 0.95
Total 1535.49 1535.49
5) F101: It is assumed that there are no losses across the filter. Even if
in practice, there are some losses, they are too small to be considered
in calculations.
Component In (kg/hr) Out(kg/hr)
Lactic acid 1125 1125
Water 195.54 195.54
PTSA 1.5 1.5
Total 1322.04 1322.04
6) R103:
Component In(kg/hr) Out(kg/hr)
Lactic acid 1125 -
Water 195.54 420.54
Methanol 498.5 98.5
Methyl lactate - 1300
Acetone
0.95 0.95
Total
1821.49 1821.49
7) D103:
15
Component In(kg/hr) Top Product
(kg/hr)
Bottom Product
(kg/hr)
Methyl lactate 1300 - 1300
Water 420.54 0.421 420.12
Methanol 100 99 1
Acetone 0.95 0.95 -
Total 1821.49 100.371 1721.12
8) R104:
Component In (kg/hr) Out (kg/hr)
Methyl lactate 1300 -
Water 645.12 420.12
Lactic acid - 1125
Methanol 1 401
Total 1946.12 1946.12
9) D104:
Component In(kg/hr) Top Product
(kg/hr)
Bottom Product
(kg/hr)
Lactic acid 1125 - 1125
Water 420.12 0.42 419.7
Methanol 401 396.99 4.01
Total
1946.12 397.41 1548.71
16
7. ENERGY BALANCE
Specific heat is considered as a function of temperature, while doing
calculations.
Heats of reaction are calculated using group contribution method, as
the heats of reaction and heats of formation of a few compounds were
not reported in literature.
1) E101:
This heat exchanger is required to cool acetone cyanohydrin, one of
the raw-materials to cool from 27
0
C to 15
0
C. Chilled water is used
for the same.
Heat required to be removed from acetone cyanohydrin = m x C
p
x
( 27-15)
= 1.71 x 10
4
kJ/hr.
Inlet temperature of chilled water = 10
0
C.
Outlet temperature of chilled water = 13
0
C.
So, mass flow-rate of chilled water required = 1362 kg/hr.
2) R101:
17
The reaction taking place in this reactor is exothermic; the value is
0.48 kJ/mol.
The rate of production of lactonitrile = 887.5 kg/hr
= 12500 moles/hr.
Rate of evolution of heat = 6 x 10
6
J/hr.
This heat is to be removed using chilled water, so that reaction
temperature of 15
0
C is maintained.
We use chilled water at an inlet of 10
0
C, which goes out at 12
0
C.
So, flow-rate of chilled water required = 653.4 kg/hr.
The stream going out of R-101 is at 15
0
C and contains lactonitrile,
acetone and unreacted acetaldehyde.
3) D101:
Component In (kg/hr) Top Product
(kg/hr)
Bottom Product
(kg/hr)
Acetaldehyde 28.95 28.95 -
Acetone 725.7 724.75 0.95
Lactonitrile 887.5 - 887.5
Total 1642.15 753.7 888.45
Average relative volatility is calculated for this system using the
correlation given by Wagle:
( )
'
,
_
2 1
2 1
1 1
25164 . 0 exp
b b
T T
where,
T
b1
and T
b2
are the boiling points of the 2 components in K and
18
1
and
2
are latent heats of vaporization in kcal/kmol.
Substituting the appropriate values, we get = 17.50.
Now, R
min
is calculated using the following formula:
( )
( )
'
Fa
Da
Fa
Da
x
x
x
x
R
1
1
1
1
min
where, x
Da
and x
Fa
represent the molar fraction of more volatile
component in top product D and feed F, respectively.
So, we get R
min
= 0.1
Now, optimum reflux ratio is calculated by multiplying the minimum
reflux ratio by 1.5
R
optimum
= 0.15.
The condenser load is calculated by the following formula:
Q
c
= D (R+1)
In this case, = 7058 kcal/kmol.
D= 13.15 kmol/hr.
Q
c
= 1.06 x 10
5
kcal/hr.
For calculating the reboiler load, we have to calculate the enthalpies of
feed, top and bottom products.
For this, we take 15
0
C as the reference temperature.
Enthalpy of feed, H
f
= 0.0
19
Now, enthalpy of the top product , H
D
= Enthalpy of acetaldehyde +
Enthalpy of acetone.
H
D
= (724.75 x 1.376 x 1000 x 25) + (28.95 x 1410 x 25)
= 1.02 x 10
6
J/hr.
Now, enthalpy of bottom product, H
B
= 12.5 x 212.30 x 165
H
B
= 4.37 x 10
5
J/hr.
Finally, reboiler load, Q
R
= Q
C
- H
F
+ H
D
+ H
B
.
Q
R
= 4.69 x 10
8
J/hr.
4) D102:
Component In(kg/hr) Top Product
(kg/hr)
Bottom Product
(kg/hr)
Acetaldehyde 28.95 28.95 -
Acetone 724.75 0.7 724.05
Total 753.7 29.65 724.05
As described in energy balance shown for D101,
= 3.36.
From , R
min
= 8.375.
R
optimum
= 12.56.
20
The condenser load is now calculated as:
Q
c
= D (R+1)
= 13.56 x 29.65 x 133.86
Q
C
= 5.38 x 10
4
kcal/hr.
Now, to calculate the enthalpies of feed, top and bottom products.
Enthalpy of feed, H
F
= (724.75 x 1.376 x 1000 x 25) + (28.95 x 1410
x 25)
= 1.02 x 10
6
J/hr.
H
D
= (380 x 28.95 x 5) + (1310 x 0.7 x 5)
= 2.05 x 10
5
J/hr.
H
B
= 724.05 x 1.428 x 1000 x 41
= 4.24 x 10
7
J/hr.
Now, Q
R
= Q
C
- H
F
+ H
D
+ H
B
.
Q
R
= 2.42 x 10
8
J/hr.
5) R102:
The reaction taking place in this reactor is an endothermic one, and the
value of heat of reaction is 3444.5 J/mol.
Production rate of lactic acid = 1125 kg/hr = 12500 moles/hr.
Rate of supply of heat required = 3444.5 x 12500 = 4.306 x 10
4
kJ/hr.
The reaction takes place at 60
0
C; steam is required to be supplied in
the jacket to maintain the temperature at 60
0
C.
21
To calculate the flow-rate of steam:
m x = 4.306 x 10
4
kJ/hr.
m = 19.1 kg/hr.
6) R103:
The reaction in this reactor takes place at 60
0
C; it is an exothermic
reaction and the value of heat of reaction is 3500 J/mol.
Rate of production of methyl lactate = 1300 kg/hr = 12500 moles/hr.
Rate of evolution of heat = 4.375 x 10
4
kJ/hr.
This heat is used to vaporize methyl lactate and water, thus methyl
lactate and water vapors come out of the reactor along with excess of
methanol vapors.
7) D103:
Component In(kg/hr) Top Product
(kg/hr)
Bottom Product
(kg/hr)
Methyl lactate 1300 - 1300
Water 420.54 0.421 420.12
Methanol 100 99 1
Acetone 0.95 0.95 -
Total 1821.49 100.371 1721.12
As shown earlier, calculations are done and results obtained are:
= 11.58
From , R
min
= 1.03
R
optimum
= 1.54
The condenser load is now calculated as:
22
Q
c
= D (R+1)
= 1128.8 x 100.7 x 12.58
Q
C
= 1.43 x 10
6
kJ/hr.
Now, to calculate the enthalpies of feed, top and bottom products.
Enthalpy of feed, H
F
= (420.54 x 1000 x 1.0 x 45)
+ (1300 x 1000 x 0.7 x 4.184 x 45)
+ (100 x 1000 x 2.53 x 45)
= 2.62 x 10
8
J/hr.
H
D
= 100.7 x 1000 x 2.53 x 30
= 1.02 x 10
7
J/hr.
H
B
= 1720 x 1000 x 2.93 x 100
= 5.04 x 10
8
J/hr.
Now, Q
R
= Q
C
- H
F
+ H
D
+ H
B
.
Q
R
= 2.54 x 10
8
J/hr.
8) R104:
The reaction taking place in this reactor is exactly reverse of that
taking place in R-103, so it is an endothermic reaction with value of
heat of reaction equal to 3500 J/mol.
Rate of supply of heat required = 4.34 x 10
7
J/hr.
This heat is supplied by steam, the flow-rate of which is calculated
23
below:
m x = 4.306 x 10
4
kJ/hr. m = 19.4 kg/hr.
9) D104:
Component In(kg/hr) Top Product
(kg/hr)
Bottom Product
(kg/hr)
Lactic acid 1125 - 1125
Water 420.12 0.42 419.7
Methanol 401 396.99 4.01
Total
1946.12 397.41 1548.71
As described earlier, we calculate and it is obtained as:
= 9.84
From , R
min
= 0.3
R
optimum
= 0.45
The condenser load is now calculated as:
Q
c
= D (R+1)
= 1.5 x 396 x 1128.8
Q
C
= 6.71 x 10
5
kJ/hr.
Now, to calculate the enthalpies of feed, top and bottom products.
Reference temperature taken for doing enthalpy calculations is 60
0
C,
so enthalpy of feed will be zero.
Now, enthalpy of top product,
H
D
= (1125 x 1000 x 0.7 x 63 x 4.184) + (195. 34 x 1000 x 63 x
4.184)
24
= 2.59 x 10
8
J/hr.
H
B
= 396 x 1000 x 0.61 x 5 x 4.184
= 5.06 x 10
6
J/hr.
Now, Q
R
= Q
C
- H
F
+ H
D
+ H
B
.
Q
R
= 9.33 x 10
8
J/hr.
10) E106:
This heat exchanger is required to cool acetaldehyde, one of the raw-
materials to cool from 20
0
C to 15
0
C. Chilled water is used for the
same.
Heat required to be removed from acetaldehyde = m x C
p
x ( 20-15)
= 6.75 x 10
3
kJ/hr.
Inlet temperature of chilled water = 10
0
C.
Outlet temperature of chilled water = 13
0
C.
So, mass flow-rate of chilled water required = 537.8 kg/hr.
11) E107 (Used to cool feed to R102):
This heat exchanger is required to cool lactonitrile, the bottom product
of D101 and to be fed to R102.
Cooling water is used for the same.
Heat required to be removed from lactonitrile = m x C
p
x ( 184-60)
= 2.76 x 10
5
kJ/hr.
Inlet temperature of cooling water = 32
0
C.
25
Outlet temperature of cooling water = 45
0
C.
So, mass flow-rate of cooling water required = 8253.75 kg/hr.
12) E108 (Used to heat feed water to R102):
This heat exchanger is required to heat water from 27
0
C to 60
0
C.
Steam is used for the same.
Heat required to be supplied to water = m x C
p
x ( 60-27)
= 1.18 x 10
5
kJ/hr.
So, mass flow-rate of steam required = 52.23 kg/hr.
13) E111 (Used to cool the feed to R104):
This heat exchanger is required to cool the mixture of lactic acid and
water from 130
0
C to 60
0
C.
Cooling water is used for the same.
Heat required to be removed from the mixture = m x C
p
x (130-60)
= 1.48 x 10
6
kJ/hr.
Inlet temperature of cooling water = 32
0
C.
Outlet temperature of cooling water = 40
0
C.
So, mass flow-rate of cooling water required = 22108 kg/hr.
26
8. PROCESS DESIGN
I) R-101:
The reaction taking place in R-101 is:
Acetaldehyde + Acetone Cyanohydrin Lactonitrile
+ Acetone.
Material balance over this reactor can be shown as below:
Component In(kg/hr) Out(kg/hr)
Acetaldehyde 578.95 28.95
Acetone Cyanohydrin 1062.5 0.0
Lactonitrile 0.0 887.5
Acetone 0.7 725.7
Total 1642.15 1642.15
Total volumetric feed entering the reactor
= (550+28.95)/650 + (1062.5/680)
= 2.46 m
3
/hr.
We can use the typical values of residence time reported in the
patents.
The reaction is kinetically controlled.
The residence time reported in patent is 26 minutes.
Reactor Dimensions:
F
V
27
where,
V = volume of the reaction mixture (m
3
).
F = volumetric flow rate entering the reactor = 2.46 m
3
/hr.
is the residence time = 0.433 hours.
V = 1.066 m
3
.
Now, let us fix H/D = 1.0
Cylindrical Volume + bottom volume = Total volume
Hence
066 . 1 135 . 0 2
4
3 2
+ D H D
D = H = 1.003 m.
However, we must provide some extra height.
H = 1.003 x 1.2 = 1.2 m.
Impeller Design:
A standard pitch-blade type of impeller is used for this purpose.
Diameter of impeller = 0.4 x Diameter of Vessel
d = 0.4 x 1.003 = 0.4012 m = 40.12 cm.
Now, we have to calculate the speed at which the mixing of liquids
will be efficient.
As reported in the patent, the power consumed per unit volume of the
reaction mixture is constant and it is roughly 1.32 HP per m
3
of the
reactor volume. This much power is sufficient to mix the liquids
efficiently.
28
The reactor volume, as we have calculated is 1.066 m
3
.
Power required for the process = 1.408 HP.
The reynolds number is given as:
2
Re
75 . 10 d N S
N
where,
S is the specific gravity,
is the viscosity of mixture in centipoise.
N
Re
= 2926.83 N ----(1)
Power consumption is given by the following equation:
5 3
d N N P
P
In terms of HP,
( )
5 3
13
75 . 15 9 . 0
10 523 . 1
N
P
N
P
3
7
10 458 . 2
N
N
P
-----(2)
Solving equations (1) and (2) and by using the graph of power number
against reynolds number for pitch blade turbine, iterations are
performed as described below:
A value of speed is assumed; this value is substituted in equation (1)
to get a value of N
Re
. From graph of N
Re
against N
p
, power number is
found. Now, using equation (2) and the above obtained value of N
P
,
29
another value of speed is obtained.
The iterations are performed till the value of speed matches for both
N
Re
and N
p.
We first start our assumption from a value of speed of 50 rpm.
Following values are obtained in iterations:
N N
Re
N
P
(from graph) N (from eq.2)
50 146341.5 1.2 273.61
273.61 8 x 10
5
1.15 277.52
277.52 8.12 x 10
5
1.15 277.52
So, we will use an agitator speed of 280 rpm.
Now,
Impeller blade width = (diameter of vessel)/15.
= 6.67 cm 7.0 cm.
Impeller level above bottom = D/3
= 0.33 m = 33 cm.
Number of baffles = 4
Width of baffle = D/10
= 0.1 m = 10 cm.
Calculation of Heat Transfer Area:
The reaction taking place in this reactor is exothermic; the value is
0.48 kJ/mol.
30
The rate of production of lactonitrile = 887.5 kg/hr
= 12500 moles/hr.
Rate of evolution of heat = 6 x 10
6
J/hr.
This heat is to be removed using chilled water, so that reaction
temperature of 15
0
C is maintained.
The internal heat transfer coefficient is given as:
h
i
= k 0.54 (Re)
0.67
(Pr)
0.25
( /
w
)
0.14
-----------(1)
D
i
Using the speed of agitator, we calculate the Reynolds number.
N d
N
2
Re
N
Re
= 8.2 x 10
5
.
k
C
P
Pr
k = 0.195 J/m s K
= 0.82 cP = 0.82 x 10
-3
kg/m s.
C
p
= 1.56 J/g K
Pr = 6.56
Also, we have D
i
= 1.003 m.
Substituting the obtained values of N
Re
, Pr and D
i
in equation (1), we
get-
h
i
= 1324.76 kcal/hr m
2
K.
Typical values of h
o
in such cases range from 1700 J/s m
2
K to 2000
31
J/s m
2
K.
So, we assume h
o
= 1800 J/s m
2
K = 1548 kcal/hr m
2
K.
Now, overall heat transfer coefficient,
d
o i d
R
h h U
+ +
1 1 1
Employing dirt factor of 0.001, we get
U
D
= 434.65 kcal/hr m
2
K.
We use chilled water, with an inlet temperature of 10
0
C and an outlet
temperature of 12
0
C.
Reaction temperature = 15
0
C.
( T)
LMTD
= 3.92 K.
So, area required for heat transfer can be calculated as:
LMTD D
T U
Q
A
A = 0.8430 m
2
.
From this, we calculate the height of jacket required for heat transfer:
x D x h
j
= 0.8430
h
j
= 26.75 cm.
We can definitely provide this jacket height, as generally, jacket
height is 0.75 times the vessel height.
The vessel height in this case is 1.2 m, which makes use of 90 cm of
vessel height for jacket possible.
Further, if we use chilled water so that the outlet temperature of
32
chilled water is 13
0
C, then the area required for heat transfer by the
jacket will be still less.
The process control and instrumentation for this reactor is shown in
Chapter 10. Process Selection.
Detailed mechanical design of this reactor is done in Chapter 9,
Mechanical Design.
II) D-102:
This distillation column is used to separate acetaldehyde and acetone,
so that acetaldehyde can be recycled back and acetone can be
recovered and sold back.
Material balance over the distillation column can be shown as below:
Component In(kg/hr) Top Product
(kg/hr)
Bottom Product
(kg/hr)
Acetaldehyde 28.95 28.95 -
Acetone 724.75 0.7 724.05
Total 753.7 29.65 724.05
The feed is at its boiling point, hence q=1.
x-y data for acetaldehyde-acetone system is given below:
X
acetaldehyde
Y
acetaldehyde
0.05 0.1627
0.1 0.2916
0.15 0.3961
0.2 0.4825
0.25 0.555
33
0.3 0.6168
0.35 0.6699
0.4 0.716
0.45 0.7563
0.5 0.7919
0.55 0.8236
0.60 0.8518
0.65 0.8771
0.70 0.8999
0.75 0.9206
0.80 0.9394
0.85 0.9565
0.90 0.9722
0.95 0.9866
The x-y graph is plotted.
R
min
= 8.38
Generally, optimum reflux ratio is 1.5 times the minimum reflux ratio;
hence we take optimum reflux ratio as 1.5 times the minimum reflux
ratio.
R
optimum
= 12.56
Using the above graph of x Vs. y, the theoretical number of plates
required is calculated.
Theoretical number of plates = 10.
But, actually, plate efficiency is never 100%.
We assume a plate efficiency of 75%.
Actual no. of plates = 10/0.75 = 13.33 14.0
Let us calculate tower diameter:
The value of tower diameter will tell us whether to use plate column
or a packed column.
34
2 / 1 2 / 1
1
,
_
,
_
g
g
g l
g
l
R
R
G
L
= 0.027.
From the graph, G
/
is calculated. However, it is the flooding velocity.
Actual G
/
= 0.8 x 1.6625
= 1.33
Now, cross-sectional area of the column,
/
G
G
A
A = 0.5449 m
2
.
5449 . 0
4
2
D
D = 83.3 cm.
As the diameter is less than 1.0 m, we use packed column.
The packing used is Ceramic Intalox Saddle type of packing.
The diameter of the packing used is 25 mm.
Total height of the tower = HETP x Theoretical number of stages.
For the packing being used, HETP = 0.46 m.
Total height of the column = 10 x 0.46 m = 4.6 m.
Pressure drop in the column, P = P/Z x height of column
= 6300 N/m
2
.
Condenser Design (E104):
Condenser load, Q
c
= 5.38 x 10
4
kcal/hr = 2.25 x 10
5
kJ/hr.
35
Flow-rate of chilled water required:
T C
Q
p
m = 7685.7 kg/hr.
Hot Fluid
(Acetaldehyde)
Cold Fluid
(Chilled Water)
Difference
20 Higher
Temperature
17 7
20 Lower
Temperature
10 10
0 Difference 7 3
T
LMTD
= 5.81
0
C.
The condenser is in true counterflow, since the shell-side fluid is
isothermal. So, we need not provide any correction the log mean
temperature difference.
The condenser design is done by using trial method.
We first assume that U
D
= 976 kcal/hr m
2
K.
The tubes used in the exchanger have in. outside diameter, 16 BWG
on 15/16 in. triangular pitch.
The tubes have length of 8 feet.
36
LMTD D
T U
Q
A
37
= 120.77 cm
2
.
t
t
a
water chilled of rate flow mass
G
= 176.77 kg/ sec m
2
.
Now, velocity,
t
G
V
= 0.176 m/sec.
Now, the average temperature for the chilled water,
t
a
= 13.5
0
C.
At t
a
, = 0.663 x 10
-3
Pas.
Inside diameter of tube, D = 1.58 cm.
t
DG
Re
= 4155.93
From graph of h
i
vs. Re at 14
0
C, we get:
h
i
= 2272.74 kcal/hr m
2
K.
h
io
= 2272.74 x ID/OD
= 1878.8 kcal/hr m
2
K.
Hot Fluid-Shell Side:
Assume maximum baffle space.
Shell side flow area (a
s
),
38
Pitch
B C ID
a
s
/
where, C
/
B is the baffle spacing.
a
s
= 129.14 cm
2
.
s
s
a
rate flow Vapor
G
G
s
= 0.6227 kg/ sec m
2
.
Now, loading,
3 / 2
//
N L
Rate Flow Vapor
G
t
f
= 65.97
0
C 66
0
C.
At this temperature, the values of thermal conductivity, density and
viscosity are found as:
K = 0.2595 W/m K
= 0.21 x 10
-3
Pas.
= 780 kg/m
3
.
39
Now, from the graph of condensing coefficient against condensing
load, we get
h
o
= 4150 kcal/ hr m
2
K.
Clean overall coefficient U
c
:
o io
o io
c
h h
h h
U
+
U
c
= 1293.3 kcal/hr m
2
K.
Now, let us calculate the dirt factor and find out whether it is under
acceptable limits:
D C
D c
d
U U
U U
R
R
d
= 0.0002 hr m
2
K/kcal.
This value of dirt factor is acceptable; hence the first trial condenser is
satisfactory and will be:
Shell Side Tube Side
ID = 10 inches = 25.4 cm.
Baffle space = 25.4 cm (approx.)
Passes = 1
Number and length = 62, 8
/
0
//
OD, BWG, pitch = in., 16 BWG,
15/16-in. triangular pitch.
Passes = 1
40
Reboiler Sizing (E105):
Reboiler load, Q
R
= 2.42 x 10
5
kJ/hr.
T
LMTD
= 35
0
C.
Typically, overall heat-transfer coefficient for reboilers ranges from
1000 to 1500 kcal/hr m
2
K.
So, we take U
D
= 1100 kcal/hr m
2
K.
Reboiler area, A = 1.5 m
2
.
9. MECHANICAL DESIGN OF STIRRED TANK
REACTOR R101
In the stirred tank reactor a flanged joint connects the shell and
the head. The shell and the bottom head are welded together. A jacket
is provided for efficient heat transfer. The agitator system includes a
41
pitched blade turbine, a stuffing box and gland arrangement and a hub
and key arrangement.
The vessel is designed in the following steps
Shell:
Internal Diameter 1.003 m
Material of construction Stainless Steel
Reactor temperature 15C
Internal pressure 1.03 kg/cm
2
Permissible stress at 15C 1330 kg/cm
2
Youngs Modulus 2 x 10
6
kg/cm
2
Head and bottoms flanged and shallow dished:
Internal Diameter 1003 mm
Crown Radius 1003 mm
Knuckle radius 50.2 mm
Material of construction Stainless Steel
Flange for head:
Material of construction Stainless Steel
Permissible Stress 1330 kg/cm
2
Gasket Material Asbestos
Gasket Thickness 3.2 mm
Bolts:
Material of construction Low Carbon Steel
42
Permissible Stress 540 kg/cm
2
Nozzles: welded to head
Material of construction Stainless Steel
Jacket Design:
Material of construction MS
Allowable Stress 963.24 kg/cm
2
.
Agitator shaft design:
Material of construction Stainless Steel
Permissible elastic limit 1330 kg/cm
2
Design of Shell:
Design pressure = 1.03 x 1.1
= 1.133 kg/cm
2
The thickness of shell is found by using the formula
t
s
=
P 2f.J
P.D
=
133 . 1 85 . 0 2 1330
1000 003 . 1 133 . 1
= 0.503 mm.
But, minimum thickness for reaction vessel, being 6.0 mm, we
use 6.0 mm thick plates. So, further stress checking is done for
thickness of 6.0 mm.
Testing for other stresses
a) Circumferential stress:
43
2t
t) P(D
f
i
t
+
=
0 . 6 2
) 0 . 6 (1003 1.133
+
= 95.27 kg/cm
2
b) Axial stress
i) Due to internal pressure
t . 4
P.D
f
i
1
=
0 . 6 4
1003 1.133
= 47.35 kg/cm
2
(tensile)
ii) Due to weight of vessel and contents
) t (D t
W
f
s i s
2
+
= 0.145 kg/cm
2
(compressive)
iii) Due to wind or piping
s
2
i
3
t D
M
f
44
Assume M = 3500 kgm
f
3
= 18.54 kg/cm
2
(tensile)
Total stress in axial direction
f
a
= f
1
+ f
2
+ f
3
= 66.04 kg/cm
2
c) Stress due to offset piping or wind
t) (D D t
2T
f
i i
s
+
= 5.24x10
5
kg /m
2
f
s
=52.42 kg/cm
2
.
Combining the above stresses the equivalent stress is:
2
s
2
a a t
2
t R 3f f f f f f + +
2 2 2
3(52.42) (66.04) ) 04 . 66 )( 27 . 95 ( ) 27 . 95 ( + +
= 124.1 kg/cm
2
(tensile stress)
For satisfactory design the following conditions must be
satisfied
f
R
(tensile) f
t
(permissible)
f
a
(tensile) f
t
(permissible)
We have found that
f
R
= 124.1 kg/cm
2
f
a
= 66.04 kg/cm
2
f (permissible for SS) = 1330 kg/cm
2
45
Therefore the shell design is satisfactory.
Head Design:
The head is to be flanged to the shell. The head is a
torispherical head.
Crown Radius R
c
= 1.003 m
Knuckle Radius R
I
= 5% of Rc
= 50.15 mm
The thickness of the torispherical head is given as
2f.J
.W P.R
t
c
h
where W = stress intensification factor
]
R
R
3 [
4
1
i
c
+
= 1.868
t
h
= 0.939 mm
For structural stability, the minimum head thickness must be
equal to the shell thickness.
t
h
= 5 mm.
Flange Design:
Gasket Design
Asbestos gaskets are provided of 3.2 mm.
Internal diameter of gasket = 1.003 mm
Gasket factor = 2
Minimum design seating stress (Y
a
) = 115 kg/cm
2
External gasket diameter is calculated as
46
1)P (m - Y
mP - Y
G
G
a
a
i
o
+
G
o
= 1033 mm
Basic gasket seating width is
b
o
=
) G - G (
4
1
i o
b
o
= 7.5 mm
as b
o
< 6.3 mm , b = b
o
+ 6 = 13.5 mm.
b = 14 mm (approximately).
Number of bolts
Under atmospheric conditions bolt load due to gasket reaction
is given by:
W
m1
= A
g
Y
a
= b G Y
a
Where G = (G
1
+ G
o
)/2
= 1018 mm
W
m1
= 7.35 x 10
4
kg.
A
m1
=
a
m1
f
W
Where f
a
is permissible stress under atmospheric
conditions
(1970
kg/cm
2
)
A
m1
= 37.34 cm
2
minimum no. of bolts is =
47
5 . 2
cm in diameter gasket mean
=
5 . 2
101.8
= 40.72
41
Bolt area =
N d
4
2
d = bolt diameter
N
A 4
m1
= 9221.8 kg
K = 1.58.
t
f
= 19.45 mm
20 mm
Nozzle Design:
We assume minimum nozzle diameter as 100 mm and proceed with
calculations for nozzle thickness.
The design procedure for all nozzles is the same
Minimum nozzle thickness
t
h
=
P - 2fJ
d P i
= 0.05 mm
Actual thickness taken = 3 mm
To check whether compensation is to be provided.
H
1
= 2.5 t
n
= 7.5 mm
The area for which compensation is required is
A = d t
s
= 600 mm
2
Area available for compensation
i) The portion of the shell or head as excess thickness
A
s
= d (t
s
t
s
`)
Where t
s
` = theoretical shell thickness = 0.615 mm
A
s
= 540 mm
2
ii) The portion of nozzle external to vessel
A
o
= 2 H
1
(t
n
t
n
`)
49
= 44.25 mm
2
Since area of compensation available is
A
s
+ A
o
= 584.25 mm
2
> A, compensation need not
be provided.
Jacket Design:
We use a plain jacket for heat transfer.
Internal pressure = 1.033 kg/cm
2
Design pressure = 1.133 kg/cm
2
Jacket internal diameter = 1003 mm
The thickness of jacket is calculated as
P - 2fJ
PD
t
t
j
= 0.694 cm
But, minimum jacket thickness = 5 mm, so we use jacket of 5mm
thickness.
Agitator System:
Diameter of agitator = 400 mm
Maximum Speed = 300 rpm
Width of blade = 70 mm
Power being used is 1.408 HP.
Shaft Design
Material of construction: Stainless steel
N 2
60 75 hp
Tc
= 3.36 kg m
50
T
m
= 1.5 x T
c
= 5.04 kg m
Z
p
=
s
m
f
T
= 0.379 cm
3
379 . 0
16
d
3
d = 1.25 cm
F
m
=
b
m
R 0.75
T
= 33.6 kg.
where R
b
is radius of blade =
2
40
cm = 20 cm
M = F
m
x L
Where L = effective length between agitator and
bearing = 1.4 m.
M = 47.04 kg m
M
e
=
) T M (M
2
1
2
m
2
+ +
= 47.17 kg m
Using this value, we calculate tension as:
3
) ( 32 /
100 17 . 47
d