Synthesis of Sodium Ethyl Sulfate

[Needtolearn]

Synthesis of Sodium Ethyl Sulfate

Molecular Formula: C2H5NaO4S
Appearance: White to Off-White Solid
Boiling point: 209 °C
Melting Point: N/A
Molecular Weight: 148.12 g/mol
CAS Number: 546-74-7



Glassware:

5L Round bottom Flask
5L two or three necked Round bottom Flask
5L beaker
Condensing column.
Pressure equalizing addition funnel
Vacuum filter


Reagents:

140g Ethanol (Anhydrous)
300g Sulfuric Acid (98%)
2000ml Distilled water
"≈" 260g Calcium Carbonate
"≈" 350g concentrated Sodium Carbonate solution (40g/100ml)
410ml Ethanol (Anhydrous) for purification



Part 1: Ethyl Hydrogen Sulfate
CH3CH2OH + H2SO4 = C2H5OSO3 + H20

Ethanol and sulfuric acid is put in freezer to cool down to 0 °C. water is put in fridge.
Ice water bath is prepared then Ethanol was added to a round bottom flask with a pressure equalizing drip funnel.
The Sulfuric acid is added SLOWLY drop by drop with strong stirring in the ice bath. The addition should take minimum 35 minutes from first to last drop.
After the addition is completed the reaction temperature should not be higher then 20 °C.
Let the solution stir vigorously in the ice bath for 60 minutes.
After 60 minutes the solution has turned yellow, the ice bath is removed and the reaction mixture is
Placed in a two necked flask and put in a heating bath that is heated to 50°C.
Heat reaction mixture to 50°C and keep it in water bath for 60 minutes then cool off to room temperature.
Put 2000ml cold water to 5L beaker then slowly add the cooled reaction mixture.


Part 2: Ethyl Hydrogen Sulfate into - Calcium Ethyl Hydrogen Sulfate
2C2H5OSO3H+CACO3 = (C2H50S03)2CA + H2O + CO2

Add calcium carbonate (≈260g) slowly with strong stirring to PH 7
The beaker is then heated to 60 °C in a water bath, also heat some rinse water 200ml.
Filter off the precipitate (Calcium sulfate) and rinse beaker and wash with the heated water.
Keep the filtered mixture.

Part 3: Calcium Ethyl Sulfate into - Sodium Ethyl Hydrogen Sulfate
(C2H50S03)2CA + NA2CO3 = 2C2H5OSO3NA + CaCO3

To filtered mixture add concentrated sodium carbonate solution (≈350g)
Calcium Carbonate will precipitate out of solution
Keep adding Sodium carbonate to it turns alkaline (PH 12-14)
Vacuum filter out the Calcium carbonate. Wash filtrate well with a little cold water
Boil solution until it becomes cloudy then filter (Precipitate this is Calcium Carbonate)
Continue to evaporate the filtrate till dry.
To dry mixture add 400ml Anhydrous ethanol and warm on water bath to most of the solids dissolves
Filter through a heated vacuum funnel, rinse Beaker with 10 ml Anhydrous ethanol.
When filtrate comes down to room temperature filter out the crystals,
Return filtrate to freezer to form second batch of crystals- then filter. Add crystals from batch one.

Yield is 235g – 51-65% of theoretical

 

[Needtolearn]

Is there a better way to do this? this kind of SUCKS

 

[woohoo]

Reaction with calcium carbonate makes a lot of foam.
Once i did it, i failed. But maybe try it again.

 

[Needtolearn]

Reaction with calcium carbonate makes a lot of foam.
add it slowly (A small amount at a time) yes this kind of sucks and takes some time but enjoy the magic of chemistry as you do it

 

[Mo0odi]

Cool
Have you tried making it yourself?