lab and pilot plant tours scaling up
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Lab and pilot plant toursScaling upwww.abpischools.org.uk
•Pear shaped flask•Bunsen burner•Reflux condenser•Vacuum filtration
Preparation of Aspirin (typical A level procedure)
1. Weigh out 2g of 2-hydroxybenzoic acid and place it in a pear shaped flask. (The starting material is a fluffy irritant white solid.)
2. Add 4.0cm3 of ethanoic anhydride. (A colourless liquid with a pungent smell.)
3. The reaction mixture will get slightly warm so cool it by swirling the flask under running water.
4. When it is cool, add two anti-bumping granules.
5. Heat under reflux for 30 minutes.
6. Cool the mixture.
7. Pour into 100cm3 of cold water containing 10cm3 of dilute sulphuric acid. Stir and allow the resulting suspension to stand for 15 minutes.
8. Filter off the crystals that form. Dry and weigh the product.
Preparation of Aspirin (typical A level procedure)
The chemistry used to make aspirin
COH
O
O
COCH3
COH
O
OH
CH3C O
O
C
CH3
O
2-hydroxybenzoic acid
ethanoicanhydride
aspirin
1. Weigh out 2g of 2-hydroxybenzoic acid and place it in a pear shaped flask. (The starting material is a fluffy irritant white solid.)
How would you do this for 20kg - 10,000 times the scale?
Preparation of Aspirin (typical A level procedure)
1. Weigh out 2g [20kg] of 2-hydroxybenzoic acid and place it in a pear shaped flask. (The starting material is an irritant fluffy white solid.)
Preparation of Aspirin (typical A level procedure)
2. Add 4.0cm3 [40 litres] of ethanoic anhydride.(A colourless liquid with a pungent smell).
Temperatureprobe
Preparation of Aspirin (typical A level procedure)
2. Add 4.0cm3 [40 litres] of ethanoic anhydride.(A colourless liquid with a pungent smell).
Preparation of Aspirin (typical A level procedure)
3. The reaction mixture will get slightly warm so cool it by swirling the flask under running water.
Preparation of Aspirin (typical A level procedure)
3. The reaction mixture will get slightly warm so cool it by swirling the flask under running water.
Preparation of Aspirin (typical A level procedure)
3. The reaction mixture will get slightly warm so cool it by swirling the flask under running water.
Preparation of Aspirin (typical A level procedure)
4. When it is cool, add two anti-bumping granules.
5. Heat under reflux for 30 minutes.
Preparation of Aspirin (typical A level procedure)
Heat under reflux for 30 minutes
20
40
60
80
100
120
140
°C
30 60 90 120 150 180Time in minutes
5. Heat under reflux for 30 minutes.
Condenser
The maximum transfer of heat from the fluid in the jacket to the reaction mixture is 2° per minute
Preparation of Aspirin (typical A level procedure)
Heat under reflux for 30 minutes
20
40
60
80
100
120
140
°C
30 60 90 120 150 180Time in minutes
6. Cool the mixture.
7. Pour into 100cm3 [1000 litres] of cold water containing 10cm3 [100 litres] of dilute sulphuric acid. Stir and allow the resulting suspension to stand for 15 minutes.
Condenser
8. Filter off the crystals that form. Dry and weigh the product.
Preparation of Aspirin (typical A level procedure)
8. Filter off the crystals that form. Dry and weigh the product.
Preparation of Aspirin (typical A level procedure)
Filter off the crystals that form
Dry and weigh the product
