Hello Sodium ethly sulfate synthetic

[TucoSalamanca.]

Welcome
200 ml of absolute ethanol
100ml of concentrated sulfuric acid
Sodium carbonate
distilled water
synthesis
Slowly add sulfuric acid to the ethanol, then reflux at a temperature of 90 degrees for 3 hours.
Then let the mixture cool down and add sodium carbonate to neutralize the pH7
Add 50 mL of filtered water and let the crystals dry at room temperature

----> someone wrote like this, is the molar calculation correct, sir? <-------

 

[G.Patton]

Do u wanna produce sodium ethyl sulfate or sodium ethyl hydrogen sulfate?

 

[TucoSalamanca.]

sodium ethyl sulfate

 

[TucoSalamanca.]

Is the calculation correct?

 

[TucoSalamanca.]

synthesis in reflux

 

[G.Patton]

Video doesn't work. Send a side link.

 

[TucoSalamanca.]

I will post a decent video in the next synth

 

[wael gano]

Yes, it is true, but this reaction produces sodium ethyl sulfate and produces sodium sulfate
It is recommended to do this reaction in large quantities since in a subsequent reaction with sodium nitrite a little nitro ethane is produced
I tried it a lot and got tired of it because of the low yield of ethyl sulfate

 

[G.Patton]

You take 3.43 moles of EtOH and 0.54 moles of H2SO4. You need the equimolar amount of H2SO4 (627.7ml).
For a what reason water is added? Sort of crystallization from water?

 

[TucoSalamanca.]

possibly to crystallize

 

[wael gano]

Because the ratio is
52.9 grams of sulfuric acid (0.54 mol)
139.9 grams of ethanol (3.4 mol)
I used a millimetric measure of acid and twice as much ethanol

 

[G.Patton]

Sorry, I don't know what do you mean here
The reaction is EtOH + H2SO4 => EtHSO4 + H2O. It means you need to take equimolar ratio. Then Na2CO3 reacts with EtHSO4 by following reaction:
EtHSO4 + Na2CO3 => EtNaSO4 + NaOH + CO2 neutral pH means that your reaction is completed.

 

[TucoSalamanca.]

Should I do the synthesis with this calculation or like the topic I opened above 200ml ethanol 100ml sulfuric acid

 

[wael gano]

Yes, you can use these ratios
An important note, which is the temperature, does not increase the temperature in any case, the reaction may change and produce diethyl ether. If you see bubbles floating during the reaction, lower the temperature immediately and it may produce a little ethyl sulfate

 

[wael gano]

Gentle heating at a temperature of 80/90, the sulfuric acid removes the hydroxyl group and takes the ethyl to form ethyl hydrogen sulfate, and the hydroxyl group also forms water EtOH + H2So4 = EtHSo4 + H2o
(So4 /96g)(29gCh3Ch2)H1g
So4 96 grams
C2H6 30g
As ethyl hydrogen sulfate
EtHSo4 126 g/mol
So4/96g/mol
C2H6/30g/mol

 

[wael gano]

After making ethyl sulfate, we add sodium carbonate, neutral ph7
To become sodium ethyl sulfate salt, but it takes with it a side product, which is sodium sulfate. This is the effect of the low yield of nitro ethane.
We want you to clarify this work, and we need to add water as a solvent, because the mass becomes thick during the addition of carbonates. Is it possible to substitute ethanol, for example?

 

[G.Patton]

You can try do separate them by their solubility in EtOH or MeOH. I haven't found accurate information about their solubility. NaSO4 is insoluble in ethanol while EtNaSO4 soluble. Check it.

 

[wael gano]

Yes, correct
I will try adding EtoH and recrystallization. This is good for purifying sodium ethyl sulfate

 

[G.Patton]

@TucoSalamanca. Found useful article about this synthesis

 

[wael gano]

Really useful as the reaction between ethyl alcohol and sulfuric acid results in three reactions in a row
Temperature plays an important role in synthesis
It also needs equal molecules of acid and alcohol
I will conduct some experiments on this synthesis and hope the team will help

 

[TucoSalamanca.]

should post neutral be filtered

 

[wael gano]

After filtration, place it at room temperature to dry to a constant weight

 

[TucoSalamanca.]

Got it, thank you sir.