ASPRIN (Plant Design)
ASPRIN (Plant Design)
ADDIS ABABAINSTITUTEOFTECHNOLOGY
There are different methods of production of aspirin (acetyl salicylic acid). The most common method of
production is by the reaction of salicylic acid and acetic anhydride. The manufacture of aspirin is based
on the synthesis of salicylic acid from phenol. The process has two step processes.
The raw materials for the production of aspirin are salicylic acid, acetic anhydride and either toluene or
sulphuric acid (H2SO4). For economic reason we prefer to use sulphuric acid. The process is based on the
reaction between salicylic acid and 20% stoichiometric excess of acetic anhydride and 10% by weight
concentrated sulphuric acid (based on the mass of salicylic acid).
The first step in the production is dissolution of salicylic acid. Salicylic acid is dissolved by sulphuric acid
in mixing tank. Then both salicylic acid solution and acetic anhydride are feed into reactor. The reaction
takes place in glass-lined or stainless-steel batch reactor for 3houres, in which the temperature is
90°C.In addition to acetyl salicylic acid acetic acid is also formed from the reaction.
At the end of the reaction period the liquid product mixture is transferred to crystallizer where it is
cooled from 90°C to 0°C. The aspirin crystallizes from the acetic acid/acetic anhydride mother liquor.
The resulting suspension is transferred to a filter or centrifuge for removal of acetic acid and solvent.
After washing with solvent, the aspirin crystals are slurried and filtered again. The aspirin crystals are
then dried and sent to sifting, granulation and tableting. Acetic acid, which is formed as a by product, is
recovered for sale.
Assumptions Made
It is required to produce 1,200,000kg of acetyl salicylic acid (aspirin). From specification of the product,
the final product must be min. 99.5% pure (1,194,000kg of aspirin). The rest 0.5% is water. Sulphuric
acid (H2SO4)is used as catalyst and it is not part of the reaction. Salicylic acid and acetic anhydride react
according to:
C7H6O3 = 7*12+6*1+3*16=138g
C4H6O3 = 4*12+6*1+3*16=102g
and products:
C9H8O4 = 9*12+8*1+4*16=180g
C2H4O2 = 2*12+4*1+2*16=60g
The reaction is carried out at a temperature of 90°C.The reaction delivers a 95% yield of acetylsalicylic
acid. Therefore 5% of the initial mass of reactants remains after the reaction is completed.
Acetic anhydride
102 g of Acetic anhydride = 180 g of aspirin
X (95% of reactant) = 1,194,000kg
Solving for X
X= (102/180)* 1,194,000kg
= 676,600 kg
95% of reactant = 676,600 kg
100% (Required reactant) = Y
Y= (676,600*1)/ 0.95 = 712,210kg
From process description 20% stoichiometric excess of acetic anhydride is feed to the reactor.
= 854,652kg
Salicylic acid
138g of Salicylic acid = 180 g of aspirin
X (95% of reactant) = 1,194,000kg
X (95% of reactant) = (138/180)* 1,194,000kg = 915,400
Annual requirement of Salicylic acid (100%) = 915,400/0.95 = 963,579kg
Amount of Acetic acid
60g of Acetic acid = 180 g of aspirin
From process description 10% by weight concentrated sulphuric acid (based on the mass of salicylic
acid) is required.
= 963,579kg * 0.1
= 96,358kg
Reactor
The reaction cycle is 5 hour, in which 3 hours of reaction and 2 hours of loading of reactants ,removing
outputs and cleaning time.
S1S2
H2SO4H2SO4
Crystallizer
The reaction is carried out at a temperature of 90°C and takes 5 hours, after which the products are
transferred to crystallizer and cooling takes place from 90°C to 0°C at a rate of 0.1 °C per min. The
crystallization process will take 15 hours and this is three times longer than reactor step. To avoid a
delay before the next batch is started, 3 crystallizers will be required. Crystallizer should be free every 5
hours to take feed from the reactor. The mass delivered to the crystallizer is fed out completely to the
centrifuge. It is assumed that all the aspirin is recovered at crystallization.
S2
C7H6O3 , C9H8O4
C4H6O3 , C2H4O2
H2SO4
S4 C7H6O3 , C9H8O4
C4H6O3 , C2H4O2
Centrifuge
After the wash the 2% mother liquor present is replaced with the same weight of water. It is considered
that a kilogram of washing solvent (water) should be used for each kilogram of product. So there is
additional water stream (stream 4) going into the centrifuge and as a result of the washing process the
aspirin is split in two streams (stream 7 and stream 6).The aspirin stream containing water (stream 7) is
delivered to a drier. S4 H2O
H2O
C7H6O3 , C9H8O4S 3
C4H6O3 , C2H4O2
S7 C9H8O4 , H2O
Y = 1,194,000 kg/0.98
= 1,218,367.3 kg
Mass of liquer left in with asprin first = total mass after first centrifugation - mass of asprin
= 24,367.3 kg
Total mass of liquer = 42732 + 48179 + 96,358 + 398,000 = 585,269 kg
Mass of C7H6O3 in s6 = Mass of C7H6O3 left after first centrifugation = 0.073 * 24,367.3 = 1778.kg
Mass of H2SO4 in s6 = Mass of H2SO4 left after first centrifugation = 0.164 * 24,367.3= 3898.8kg
Mass of C4H6O3 in s6 = Mass of C4H6O3 left after first centrifugation= 0.083 * 24,367.3 = 1998.1kg
Mass of C2H4O2 in s6 = Mass of H2SO4 left after first centrifugation = 0.68 * 24,367.3 = 16,691.6kg
It is stated that the water leaving with asprin in stream 7 have the same mass as Mass of liquer
Water in s7 = 24,367.3kg
= mass in S3 - mass in S6
MATERIALS IN stream 3 (kg) IN stream 4 (kg) Out stream 5 Out stream 6 Out stream 7 (kg)
(kg) (kg)
day year day year day year day year day year
Dryer
It is recommended that the final product (stream 9) must be 99, 5% pure. It has been assumed
that the 0.5% impurity remaining with the aspirin prior to drying is water. So the 1,194,000
aspirin must be accompanied by no more than 1,194,000*0.005/0,995 = 6000kg of water. The
remaining 18367.3 kg (24,367.3– 6000) water is evaporated off during the drying process (stream
8)H2O
S8
S7 S S S9S9 s9
SALICYLIC ACID - - -
ACETIC - - -
ANHYDRIDE
SULPHURIC - - -
ACID
ACETIC ACID - - -
vapour liquid
Distillation
We assume that acetic acid is completely separated from the liquor. Stream 11 carry acetic acid
and the other component of liquor is carried by stream 10.
S11 C2H4O2
C7H6O3 , H2SO4 S5
C4H6O3 , C2H4O2
,
C7H6O3
C4H6O3
H2SO4 S10
Sizing of reactor
The reaction period is five hours (sum of time of feeding, reaction, removing and cleaning).
The sum of mass of outlet stream of reactor = 128.2 + 144.5 +289.1 + 3582.4 +1194.1 =5338.3
Volume of reactor per day = (3582.4/1390) + (289.1/1830.5) + (128.2/1050) + (144.5/1443)
= 4.122 m3/day
If the reactor is 75% full on each batch or cycle the volume of the reactor needed
Energy balance
Kopp’s rule is a simple empirical method for estimating the head capacity C p of solid or
liquid at or near 20℃. According to this rule, Cp for molecular compounds is the sum of
contributions for each element of compound.
For example the head capacity for salicylic acid (solid ) calculated
The unit of the heat capacity must be changed to I since we are working in a
mass base
Heat capacity (J/kgoc) = [(heat capacity (J/ moloc ) / weight (g/mol)]X 1000
= 2262.5 J/kgoc
Heat of Reaction
QR = -n ∆HoR
= -85 X 4970
= - 422,450 kj
∆H = m Cp ∆T Where ∆T = 65 Oc
Qp = Hproduct - QR
= -289,684.6 kg
Let assume that from 3 hour of reaction time, heat is librated for 2 hours
Qp = 289684.6 kg/ 2 hr
= 144,842.3kJ/hr
Q = Mc Cp At
Mc = Q/CpAt
Cp = 4018 KJ/kg
4T = 10Oc = 10k
M = 144,842.3kJ/hr
4018 X 10Oc
M = 3465.1 kg/hr
Q = 3465.1 kg/hr
998kg/m3
= 3.5 m3/hr
90-30
= 64.9Oc
Q = U ∆Tlm A
A = Q
U ∆Tlm
= 9m2
A 1500 litter staired tank stainless steel reactor having approximately 9m2
Jacket area.
Q= m Cp ∆T ∆T = -90 Oc
= 11,947 kJ/hr
Mc Cp ΔT = Q
MC = Q/ΔTCP
= 285.8 kg/hr
Q=m/ρ
Capacity of crystalizer
= 1.02 m3/batch
V (With 90% full) = 1.02 / 0.9 = 1.14 The volume of the crystallized with 900 C
Percent full can be determined as follows.
= 1.02 m3/batch
The fore the capacity of the crystallizer is 1.4 m3 ≈ 1.2 The volume of the
crystallized with 900 C Percent full can be determined as follows.
= 1.02 m3/batch
Products from crystalliser are delivered to the centrifuge at 0℃.Product are assumed to remain at
0℃. No heat is actively added.
= 1.02 m3/batch
1.02 m3 = X
Heat is added to the materials in the drier. Initial temperature of acetylsalicylic acid is 0℃, while
the water content is at 10℃. To calculate in enthalpy ΔH of drier in stream 8 as
follows
Capacity of drier
The heat transferred to the drier is 142,672.75 KJ. Let the chance in
temperature of the air be 300C and heat supplied be for 5 hour. Let the
moisture content of the air be 0.01 kg/kg air.
To determine the capacity of drier
The amount of air that supply this amount of heat can be calculated by
Ma = Q/ΔTCP
= 28534.5 / 30 * 1 =951.15
Compound In put
Asprin 3582.4 kg/day
Water 73.1 kg
3655.4 kg/ day
The capacity of drier in kg/ hr
= 152.3 kg/h
in volume ,
in m3/ hr ,
V= 011 m3/ hr
Distillation
It is assumed that products delivered from the centrifuge process remain at 0℃ (except water).
There are three liquids present in the stream 5 going to the distiller; acetic acid, acetic anhydride
and sulphuric acid. Following are boiling points at atmospheric pressure for the components fed
into the distiller:
Material fed into the distiller is to be heated to 118.1 (°C) in order to boil off the acetic acid, while
leaving the remaining materials unevaporated. To Calculate enthalpy ΔH of distillation in
stream 10.
= 300,498 kj
≈ 1.5 m3/day
=62.5 l/hr
Capacity of condenser
=0.005 m3/hr
Storage Capacities depend on many things. One of the factors is the daily
requirement and to how many days we need to store our raw material.
Raw materials
Daily requirement
= 732 m3 ≈ 7.5 m3
V of stor for Sulpc acid = 0.16 m3/day X 3day
≈ 0.5 m3
For salicylic acid, since it is solid we need storage room. The storage room
capacity can be calculated As capacity of storage room
= 8673 Kg
We select bucket elevator to transport salicylic acid and aspirin water mixture
to temporary storage.
Temporary storage tank to feed the centrifuge the tank must hold the
crystallization out put for day therefore it has similar volume as crystallizer
which is volume per day
It should store one day centrifuged product for any delay in process . The
capacity is 2.673 m3/ day .
Storage tank for acetic acid acetic acid recovered per day is 1144 kg. we
prefer to prepare storage tank for 7 days.
=7.63 m3 ≈ 7.7 m3
Selection and determination of Capacity of pumps
The capacity of the pump for Acetic anhydride feed can be determined
= 2.44 m3
For both fluids we select centrifugal pump made from stain less steel
Equipment specification
Reactor
Jacketed, agitated
Glass lined carbon steel , atmospheric
320 gallon volume
Crystallizer
Stainless steel
320 gallon, atmospheric
Centrifuge
Dryer
Distillation
7.5 m3 volume
Glass lined carbon steel
Floating roof, API
Pump for feeding reactant (2) pump for reactant and product mixture feed to
crystallizer (1)
Stainless steel
Pipe diameter 2 in
Packing seal type
Stainless steel
0.9 gal/min flow rate
6 * 4 inch area
2 meter height
Condenser
Cost of equipments
We can estimate other costes from a given table of cost relation. Our plant solid
liquid processing.
Direct cost
Purchased-equipment installation(pe)
Pe = 0.39 * 6,863,900.4
= 2676921 birr
= 892307 birr
P = 0.31 * 6,863,900.4
= 2127809 birr
Ec = 0.1 * 6,863,900.4
= 686390.04 birr
B = 0.29 * 6,863,900.4
=1990531 birr
Y =0.1 * 6,863,900.4
= 686390.04 birr
S = 0.55 * 6,863,900.4
= 3775145 birr
L = 0.06 * 6,863,900.4
= 411834 birr
Indirect cost
Engineering and supervision (E)
E = 0.32 * 6,863,900.4
= 2196448 birr
= 2333726 birr
= 1235502 birr
Contingency (C)
C = 0.36 * 6,863,900.4
= 2471004 birr
= 8236680 + 13247246.0.8
= 21483926.08 birr
= 5079286.3 birr
Total capital investment (T.c)
= 5079286.3 + 21483926.08
= 26,563,212.08 birr
= 1,791,000 kg/year
Material Molecular
C7H6O 138 g
C4H6O3 102 g
C9H804 180 g
C2H4O2 60 g
of A.A by 0.95
0.95
= 1,068,315,79kg/year
= 1,281,978.947 kg AA / year
0.95
= 1445,368. 421 kg / year
= 144556.84 kg/year
Centrifuge
S4H2O
S3
Centrifuge Aspirin
S7
Acetic Acid H 2O
Aspirin
Acetic S5 S6
Anhydride Acetic
Acetic
Anhydride
H2SO4 Anhydride
H2SO4
Salicylic acid H2SO4
Salicylic acid
Salicylic acid
Acetic Acid
Acetic Acid
H 2O
Centrifuge is first separate S5 which don’t contain Aspirin from s3 and from the
process description the separate left from s5 is contain the martial found in the
streams is 2% which Called material liquor. The mother liquor is separated by adding
water (stream 4)
0.98
= 36,55.02 kg/year
from stream S3
= 72,268.42 = 0.082
877904.21
Reactor
S1 Reactor S2
H2So4
Salicylic acid
Crystallizer
S2 S3
Crystallizer
= 36551.02 kg /year
Amount ( kg/year )
Martial S6 S5 S7
salicylic Acid 3,008.85 69,259.57
Acetic anhydride 2,668.72 61,430.23
H2SO4 6,17.71 138,519.13
Acetic acid 24,855.74 572,144.26
H20 1,7754,448.77 - 36551.02
Aspirin - - 1,7,791.00
Dryer
S7 S8
H20
Aspirin
H 2O S 9
1.0 X
X = 1,791,000 / 0.995
= 9,000 kg /year
= 27551.02 kg/year
From stream 2
Distillation
We assume that acetic acid is completely separated from the liquor. Stream 11
carry acetic acid and the other component of liquor is carried by stream 10.
S11
Distillation
S5
S10
S5 S10 S11
Salicylic Acid 69,259.57 69,259.57 -
Sizing of reactor
Reaction period is five hour (sum of time of feeding, reaction,
0.75
Energy balance
Kopp’s rule is a simple empirical method for estimating the head capacity Cp of solid or
liquid at or near 20℃. According to this rule, Cp for molecular compounds is the sum of
contributions for each element of compound.
A calculated
= 161.1 J/mol 0C
= 231J/mol 0C
The heat cap by k/g is found by dividing heat capacity in mole by molecular weight
and multiplying by 1000
Weight ( g/mol )
0.1802 kg/mol
QR = -n∆H0R
= -85 X7454.9
= -633667.45 kJ
QP = H product + QR
= 190,277.8 -633667.45 KJ
= -443,389.65 KJ
Let assume that from 3 hour of reaction time heat is librated for 2 hours
Qp = - 443,389 .65 KJ
2 hr
Mechanism to cool it. We prefer to cool it by using water and Jacketing the reactor. Let
the temperature change of cooling water be 10 0c from initial temperature
Q= mc Cp ∆T
mc = Q/CP∆T
∆T = 10 0C = 10 M
4.18X10 0C
= 5,303 .7 kg /hr
We select the material of construction to be glass lined. Stirred tank reactor. Assume
water in let temperature of 200C with 100c temperature rise. It is reasonable to
assume that a jacket to reactor with over all heat transfer coefficient.
(90-30)
Q = UA T min
A= Q = 221, 694, 82
A= 13.7 m2
Compound Input and out put kg/ batch Heat removed (kJ)
Sulicacid acid 54.2 -5689.2
Acet Anhydrid 48.08 -5774.2
sulpheric Acid 108.4 -16810.6
Asprin 1343.4 -142463.5
Acetic acid 447.8 -97970.1
Q= mcp ∆T ∆T= - 90 0c
=17541.2 kg /her
The cooling water can be calculated as
mc Cp ∆T=q
mc = Q/∆T Cp
4.18X10k
The volume of the crystallizer with 90 0C percent full can be determinate as follows
V= 1.534 m3
Capacity of centrifuge
The volume of Mixtures to be centrifuged is
V= 1.14 m3
1m3 = 264.2gal
1.14m3 = X
X= 301.2 gal
Assume that the volumetric flow rate of 301 gal / batch or 60.2 gal /hr
= 213906.6 KJ
Capacity of drier
The heat transferred to the drier is 213906.6 KJ. The amount of air that supply this
amount of heat can be calculated by assuming
Let the change in temperature of the air be 30 0C and heat supplied be for 5
hour. let the moisture content of the air be 0.01 kg/kg air
ma∆T Cp = Q ,
∆TCp t 5
3 0 0C
Compound Input
Aspirin 5373.54
Water 109.66
Total 5483.2 Kg/day
Day 24 hr
= 228.46 kg/hr
In volume
V= 3.975 m3 /day
Distillation
It is assumed that products delivered from the centrifuge process remain at 0℃ (except water).
There are three liquids present in the stream 5 going to the distiller; acetic acid, acetic anhydride
and sulphuric acid. Following are boiling points at atmospheric pressure for the components fed
into the distiller:
Stream II contains reflux 42.915 kg of acetic acid will be cooled from acetic acid will be
cooled from 118 .1 0C to 250C and then returned to distiller for re- distillation as
follows
= 299068,246 KJ
The mass of water required to condenses the vapor can be calculated, if ∆T =350C
mc = Q 269642.15
The storage capacity depend on many things one of the reactors is the daily
requirement and to how many days we need to store our raw material raw material
= 0.474 m3
≈ 0.5 m3
= 130009.6 kg
1443 kg/m3
= 9 m3 volume of house
Acetic anhydride feed pump the capacity of the pump for acetic anhydride feed can be
determined.
= 1050 kg/m3
Batch day
Q= 3.66 m3 /day
45min X 4batch
= 0.02 m3 /min
Q=433.65 kg/day
1830,5 kg/m3
= 0.237 m3/day
= 11.85 X 10 -3 m3/min
= 11.8 l/ Min
For both fluids are select centrifugal pump made from stainless steel pump used
to pump reactor mixture
20min /batch
Storage tank temporary feed to centrifuge the tank must hold the crystallization
out put for day therefore it has similar volume of crystallizer which is volume per day
.
Day
We should have the same capacity tank like that feed centrifuge. It should store one
centrifuged product for any delay. The capacity is 6.136 m3
Acetic acid recovered per day is 1716.9 kg. We refer to prepare storage tank for 7
days.
1049 kg/m3
= 11.5 m3
In volume
= 91 L/hr
Capacity of condenser
We know that the mass of Acetic anhydride to be condense is 28.6kg/ batch or 114.4
kg/day
1050 kg/m3
Equipment specification
Reactor
Jacketed, agitated
Crystallizer
Stainless steel
Centrifuge
20 inch diameter
Stainless steel
Dryer
Area of 20 ft2
Stainless steal
Distillation
7.5 m3 volume
Pump for feeding reactant (2) pump for reactant and product mixture feed to
crystallizer (1)
Stainless steel
Pipe diameter 2 in
Stainless steel
Stainless steel
Bucket elevators 1 for transport salicylic acid and 1 to transport centrifuged aspirin to
temporary storage tank
6 * 4 inch area
2 meter height
Cost of equipments
Reactor 61250
Crystallizer 1559550
Centrifuge 1169200
Dryer 262700
Distillation 500000
Total 7771336.8
We can estimate other costes from a given table of cost relation. Our plant solid liquid
processing.
Direct cost
Purchased-equipment installation(pe)
Pe = 0.39 *7771336.8
= 3007421 birr
Ic = 0.13 * 7771336.8
= 1002473.78 birr
P = 0.31 * 7771336.8
= 2390514.41 birr
Ec = 0.1 * 7771336.8
= 771133.68 birr
=2236287 birr
Y =0.1 * 7771336.8
= 777133.68birr
S = 0.55 * 7771336.8
= 4241235.24 birr
L = 0.06 * 7771336.8
= 462680 birr
Indirect cost
E = 0.32 * 7771336.8
= 2467627 birr
= 2621854 birr
= 1388040.62 birr
Contingency (C)
C = 0.36 * 7771336.8
= 2776081.25birr
= 24136484.15 birr
= 5706389.23 birr
= 5706389.23+ 21483926.08
= 29,842,873.38 birr
Plant Flow Diagram
Salicylic acid
store
Crystallizer 1 Intermediate
Reactor storage tank
Reactor
Washed
Crystallizer 2 stream
Centrifuge
Temporary
Crystallizer 3
Storage tank
C4H6O3
storage
tank
H2SO4
storage
Tank
Distillation
column
Drier
Conveyor
Packing