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009: Protocol of aspirin production and system test
Aspirin Process:
- Reagents: Distilled water (DW), Sulfuric acid (H2SO4, 99%), ice, water, Salicylic acid, acetic anhydride, stainless cleaning solutions.
- Materials: Funnel, Filter paper or Fabric, vacuum pump, cleaning equipements, safety requirements (glasses, Lab coat, mask)
Protocol:
step 1:
- weighs 400g of salycilic acid and put it in the Reactor (Tank 1) using the funnel
- Add 1L of acetic anhydride using the funnel
- finaly add 20ml of concentrated sulfuric acid (H2SO4)
- Turn ON the heater in the Reactor bath (tank 1) - (the water should reach 65-70°C)
PS: Both sulfuric acid and acetic anhydride are DANGER and should take the needed safety while using it.
* Acetic Anhydride is a HIGHLY CORROSIVE CHEMICAL and contact can severely irritate and burn the skin and eyes with possible eye damage. * Breathing Acetic Anhydride can irritate the nose, throat and mouth.
* Sulfuric acid is a highly corrosive chemical that is potentially explosive in concentrated form *. It can cause severe skin burns, can irritate the nose and throat and cause difficulties breathing if inhaled, can burn the eyes and possibly cause blindness, and can burn holes in the stomach if swallowed.
Step 2:
- Start the reaction by turing ON the mixer of the reactor (tank 1)
- The reaction need 15-20 min to be completed
Step 3:
- Add water (at room temperature) in the bath of the cooler (tank 2)
- Transfer the mixture to the cooler (tank 2) to cooldown the temperature of the reaction (20-25°C)
Step 4:
- add 2L (cool distilled water from HOT WATER TANK) to destroy the excess of acetic anhydride
- transfer the mixture by pumping it in the crystallizer (tank 4)
Step 5:
- Put in the ice bath of the crystallizer 2 bags of ice, the crystals should form after 10min of this step
Step 6:
- Turn ON the vacuum pump and start the filtration in the filter (tank 5)
- Disconnect the vacuum pump add 2L of DW then reconnect it and wait 15min
Step 7:
- turn OFF the vacuum pump
- Add 1L of ethanol + 6L of warm distilled water from the HOT WATER TANK (tank 3) and wait till all crystals dissolve in it
Step 8:
- Retransfer the mixture to the crystallizer (tank 4) and follow the same steps (from step 5 to step 6).
|
Step |
Step Description |
Expected Results |
Results |
|
Precondition |
System is OFF |
- |
- |
|
TURNING ON the system |
Turn ON the control panel
|
The system is ON |
The system is ON |
|
Switch on the mixer 1 (tank 1: Reactor) |
Turn on the mixer 1 from the control panel (Reactor--->Mixer ON) |
Mixing the reagents to obtain the mixture in the reactor (tank 1) |
The reagents were mixed and the mixture was obtained in the reactor (tank 1) |
|
Open the valve V1 (tank1 : Reactor) |
Open the valve V1 to transfer the mixture from tank 1 (reactor) to tank 2 (cooler) (Reactor---->Reactor valve V1) |
Transferring the mixture to cooler (tank 2) |
The mixture is transferred to cooler (tank 2) |
|
Open the valve 6 (tank 3 : HOT WATER) |
Open the valve V6 to add water from HOT WATER TANK (tank 3) to the cooler (tank 2) (HOt WATER TANK---->HOT WATER TANK valve V6) |
Transferring the distilled water (HOT WATER TANK 3) to the cooler (tank 2) with the mixture |
The distilled water is transferred from (HOT WATER TANK 3) to the cooler (tank 2) with the mixture |
|
Open the valve V2 (tank 2: Cooler) |
Turn ON the pump 1 Open the valve V2 to transfer the Water from cooler (tank 2) to crystallizer (tank 4) (cooler---->cooler pump 1) (cooler---->cooler valve V2) |
Transferring the mixutre to the crystallizer (tank 4) and formation of crystals |
The mixture is transferred to the crystallizer (tank 4) but there isn't formation of crystals |
|
Switch on the mixer 2 (tank 4 : Crystallizer) |
Turn on the mixer from the control panel (Crystallizer--->Mixer ON) |
Mixer 2 is ON and start Mixing the mixture in the Crystallizer (tank 4) | Mixer 2 is ON and the mixture is mixed in the Crystallizer (tank 4) |
|
Open the valve V3 (tank 4: Crystallizer) |
Open the valve V3 to transfer the Water from crystallizer (tank 4) to the filter (tank 5) (crystallizer---->crystallizer valve V3) |
Transferring The mixture to the filter (tank 5) |
The mixture is transferred to the filter (tank 5) PS: there isn't any formation of crystals. there's a mixture with purple color. |
|
Switch on the vacuum pump |
Turn on the vacuum pump from the control panel (Filter---->Filter pump ON) |
Vacuuming The air in tank 6 (Waste tank) |
The air is vacuumed in tank 6 (Waste tank) |
|
Open the valve V4 (tank 5 : Filter) |
Open the valve V4: 1-the vacuum filtration begin 2-Aspirin crystals are now in the filter (tank 5) (Filter---->Filter valve V5) |
Transferring The filtrate transferred to the waste tank (tank 6) |
The filtrate transferred to the waste tank (tank 6) |
|
Open the valve V7 |
Open the valve V7 to add 30L warm water from WARM WATER TANK (tank 3) to vacuum filter (tank 5) (WARM WATER TANK---->WARM WATER Valve V7) |
Re-Dissolving the Crystals with 30L warm water after 20min in the vacuum filter (tank 5) |
We didn't do this step (No crystals) |
|
Open the valve V5 and pump 2 (tank 5 : Filter) |
Open the valve V5 The solution is pumped from tank 5 to tank 4 for the second crystallization (vacuum filter---->vacuum filter Valve V5) |
Transferring the Solution to the crystallizer (tank 4) and start the crystallization |
We didn't do this step |
|
Switch on the vacuum pump for the second filtration |
Turn on the vacuum pump from the control panel (Filter---->vacuum pump ON) |
Vacuuming The air in tank 6 |
We didn't do this step |
|
Open the valve V3 and V4 |
Open the valve V3 and V4: 1-the vacuum filtration begin 2-Aspirin crystals are now in the vacuum filter (tank 5) (1-crystallizer---->crystallizer valve V3) (2-vacuum filter---->vacuum filter valve V4)
|
Transferring The filtrate to the waste tank (tank 6) |
We didn't do this step |
|
switching OFF the system |
switch OFF the system |
the system is OFF |
the system is OFF |
|
Postcondition |
system is OFF |
Overview: the first test was donned with no formation of crystals.
the hypothesis is: that's we should extend the reaction time also the crystallization time in order to found the optimum time to the formation of the ASPIRIN.
In video 10 there's a liquid mixture with purple color, we should found the cause of this purple color.
video 1 (mixing SA and acetic anhydride) 08.01.2024
video 2 ( mixing SA and acetic anhydride) 08.01.2024
video 3 (mixing SA and acetic anhydride) 08.01.2024
video 4 (add sulfuric acid and start the mixing) 08.01.2024
video 5 (put the ice in the ice bath) 08.01.2024
video 6 (transfer the mixture from the cooler to the crystallizer) 08.01.2024
video 7 (reaction in the reactor + mixing) 08.01.2024
video 8 (add distilled water to cooler) 08.01.2024
video 9 (turn on the mixer in the crystallizer) 08.01.2024
video 10 ( transfer the mixture from crystallizer) test negative 08.01.2024