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Aspirin PDF

This case study involves the design of a continuous process to manufacture aspirin. Key aspects include: - Salicylic acid, acetic anhydride, and phosphoric acid continuously react and convert 99.5% of salicylic acid to acetylsalicylic acid in a stirred tank reactor. - Ultrapure water is then added and reacts with excess acetic anhydride, and the stream is cooled to crystallize the product acetylsalicylic acid. - Heat exchangers and pumps are used, and filtration separates the aspirin crystals from acetic acid byproduct. Material and energy balances along with equipment sizing and costs are analyzed to evaluate the process economics.

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375 views3 pages

Aspirin PDF

This case study involves the design of a continuous process to manufacture aspirin. Key aspects include: - Salicylic acid, acetic anhydride, and phosphoric acid continuously react and convert 99.5% of salicylic acid to acetylsalicylic acid in a stirred tank reactor. - Ultrapure water is then added and reacts with excess acetic anhydride, and the stream is cooled to crystallize the product acetylsalicylic acid. - Heat exchangers and pumps are used, and filtration separates the aspirin crystals from acetic acid byproduct. Material and energy balances along with equipment sizing and costs are analyzed to evaluate the process economics.

Uploaded by

Rayan Fuad
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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218 Chapter 14 Case Studies

In order to clearly identify the material for the two separate problems, each problem
is presented in its entirety within a labeled frame. Since there are similarities between the
two problems, some of the same information appears in both problem descriptions.

14.2 CASE STUDY 1: MANUFACTURE OF ASPIRIN

Project Description
In the manufacture of aspirin, acetylsalicylic acid (ASA, the active ingredient in aspirin) is synthesized using the reaction

salicylic acid + acetic anhydride → acetylsalicylic acid + acetic acid

The presence of phosphoric acid catalyzes the irreversible reaction, which proceeds with kinetics that are first-order with respect
to salicylic acid concentration (kreaction = 0.5 s−1 ). Further, the reaction is exothermic (∆Hreact = −85, 800 J/gmol of salicylic acid
reacted). A simplified process is described below:
The following three streams will be continuously fed to a reactor at 70◦C:

Feed Stream Component Flow rate


1 Crystalline salicylic acid 2000 kg/hr
2 Liquid acetic anhydride (pure) 5000 L/hr
3 Liquid concentrated (95%) phosphoric acid 1250 L/hr

The salicylic acid will enter the reactor as a crystalline solid but will dissolve in the acetic anhydride.
The reactor is a continuously stirred tank reactor, where 99.5% of the salicylic acid will be converted to acetylsalicylic acid
(also dissolved). Furthermore, the contents of the reactor will be maintained at 70◦C in the reactor by a cooling jacket around the
reactor (carrying cooling water as needed).
The outlet stream from the reactor will flow to a mixer where it will be joined by an additional stream of ultrapure water (22,000
L/hr, 25◦C). The water will react with the excess acetic anhydride to form more acetic acid, according to the reaction

acetic anhydride + water → 2(acetic acid)

This reaction proceeds to 100% conversion in the mixer, so the sizing of a “reactor” for this step is not necessary. Further, this
reaction is also exothermic, but the extent of this reaction is small enough in this case to justify neglecting the heat of the reaction.
The mixed product stream leaving the mixer will enter a centrifugal pump, which will boost the pressure to the value needed to
pass through the remainder of the process (leaving the final filtration sequence at atmospheric pressure).
The stream leaving the pump will enter a product cooler (a heat exchanger) in which it will be cooled to 25◦C using cooling
water as the other stream in the exchanger.
The water addition and cooling step will promote the crystallization of the acetylsalicylic acid (and any unreacted salicylic
acid), and the stream will then enter a filtration sequence to separate the crystals (aspirin stream) from the other byproducts (acetic
acid byproduct stream, which is sold).

Technical Details

1. Individual Properties

Salicylic Acetic Phosphoric Acetylsalicylic Acetic Water


Acid (liq) Anhydride Acid Acid (liq) Acid
Formula C 7 H6 O3 C 4 H6 O3 H3 PO4 C 9 H8 O4 C 2 H4 O2 H2 O
M.W. 138.1 102.1 98.0 180.2 60.1 18.0
M.P. (◦C) 159 –73 21 135 17 0
B.P. (◦C) 211 139 158 140 118 100
Density (g/cm3 ) 1.44 1.08 1.68 1.35 1.05 1.0
14.2 Case Study 1: Manufacture of Aspirin 219

Case Study 1 Manufacture of Aspirin (continued)

2. Treat the concentrated phosphoric acid (95% PA, 5% water) as pure phosphoric acid.
3. Assume the following stream heat capacities:

reactor outlet stream 1.67 J/g ◦C


ultrapure water and cooling water streams 4.184 J/g ◦C
mixer outlet stream 3.41 J/g ◦C
4. To determine the mixer outlet temperature, construct separate heat balances on the ultrapure water stream and reactor outlet
stream. The outlet temperatures of both streams must be the same, and the heat needed to cool the reactor outlet stream from
its entering temperature must equal the heat to raise the ultrapure water temperature from its entering temperature.
5. Cooling water is available at 18◦C and has a maximum return temperature of 40◦C. In selecting the actual return cooling
water temperature, assume that you want to minimize the cost of cooling water (even though this will affect the size and
cost of the heat exchanger). However, a second and overriding constraint is the rule of thumb that the minimum temperature
difference (either ∆T1 or ∆T2 , see Figure 10.11) for a heat exchanger is 5◦C.
6. Assume countercurrent, single-pass heat exchangers.
7. Assume that the separation system is isothermal (operates at constant temperature).
8. For the purposes of sizing the pump, the pressure drop due to friction in each of the units downstream of the pump is esti-
mated to be as follows:

heat exchanger 22 psi


filtration sequence 260 psi

9. The separation system uses a complex scheme of multiple steps. For this preliminary design, simply represent the separation
system by a box labeled “Separation System.”
10. The cost of the separation system can be approximated as $2.9 million (delivered price).
11. The following market costs/values apply:

Salicylic acid $1.33/lbm


Acetic anhydride $0.49/lbm
Phosphoric acid $0.34/lbm
Ultrapure water $0.03/lbm
Acetylsalicylic acid (aspirin) $3.97/lbm
Acetic acid byproduct stream $0.013/lbm
12. The following utility costs apply:

cooling water $0.03/1000 gal


electricity $0.05/kW -hr

13. The total operating cost per year can be estimated as 1.55 times the sum of the feed cost, cooling water costs, and electricity
costs (excluding the filtration sequence, for which these values are not known). In other words,

Operating cost = 1.55(Feed cost + Cooling water cost + Electricity cost)

14. The direct capital costs for the reactor, heat exchangers, and pump can be estimated from the formulas in Table 13.2 and
using the current value of the M&S Index (look in the back of a current issue of the magazine Chemical Engineering2 ).
15. The current tax rate is 35%; we are allowed to depreciate our equipment over 10 years; and our company requires a minimum
ROI of 0.15. In our case, 85% of the capital investment can be depreciated.
220 Chapter 14 Case Studies

Case Study 1 Manufacture of Aspirin (continued)

Assignment

1. Draw a PFD for the process.


2. Perform material balances on the process, one unit at a time, to determine the component flows for each stream.
3. Perform energy balances to determine the unknown temperatures of the streams and/or the heat duties for the heat exchangers
and reactor.
4. Calculate the amount of steam and cooling water needed for the heat exchanger(s) and reactor(s).
5. Design the reactor(s) – determine the reactor volume(s) needed to achieve the specified conversion.
6. Determine the work required for the pump assuming that the pump is 85% efficient (only 85% of the energy added to the
pump is transferred to the fluid).
7. Size all heat exchangers using approximate values of Uo from Table 10.4.
8. Complete a stream table showing, for each stream, the mass flow rates of all components, the temperature, and the pressure.
The stream table would be as follows:

Process Reactor Mixer Pump Cooler Separator Outlet


Feed Outlet Outlet Outlet Outlet #1 #2
Flows (kg/hr):
salicylic acid
acetic anhydride
phosphoric acid
acetylsalicylic acid
acetic acid
water
Total
Temp. (◦C)
Pressure (kPa)

9. Complete an equipment specification list containing the following kinds of information:


Pumps: For each pump, provide the required horsepower.
Heat exchangers: For each exchanger, provide the heat duty (Btu/hr), area, Ao ( f t 2 ), and required steam (lbm /hr) or cooling
water (lbm /hr).
Reactor: For each reactor, provide the volume (liters), heat duty for the heating/cooling jacket (Btu/hr), and required flow
(lbm /hr) of steam or cooling water for the jacket.

10. Determine the ROI for this project.


11. Suggest three ways to potentially improve the economics of this process. Explain why you believe your suggestions may
make a significant improvement.

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