Question about nitroethane synthesis

[TucoSalamanca.]

Preparation of Nitroethane by Gerard Desseigne & Henri Giral
The reaction flask is charged with:26.5 g (0.0625 * 3moles) of tech grade K2CO3 dissolved in 137 g of water320 g of 97% tech sodium nitrite
6 ml of cetyl-oleic alcohol or oleic alcoholm(antifoaming agent)Vol of the mixture is about 420 mls. The mixture is heated on a bath at 130C with stirring.
The addition funnel is charged with 750 ml of an aqueous solution of 444 g (3moles) sodium ethylsulfate.
The solution is added to the reaction mixture during 50-60 mins at asuitable rate to keep the reaction mixture at 125-130C, with vigorous stirring.The distillation of the nitroethane begins when the addition is started. When addition of NaEtSO4 is complete 100 mls of water is added during 10 mins.
The distillate separates into 2 layers. Can be distilled at 760mmHg with a distillation column. Distillation starts at 30C. All below 74C is discarded.
Temp should settle at 87C & distillation is stopped at 99.8C.
Yield of nitroethane:96 g (1.28 moles), 42.6% based on NaEtSO4
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Friends, I have tried making nitroethane many times, but I have never been able to distill it successfully. Can someone write in detail how to do this (I'm a rookie chemist)

 

[TucoSalamanca.]

I'm distilling 103.5 grams of sodium nitrite, 158 grams of sodium ethyl sulfate and 8.6 grams of potassium carbonate and it's not distilling, it's a really bad problem. During the reaction it turns into stone and is very difficult to clean, synthesis always fails.

 

[wael gano]

I'm distilling 103.5 grams of sodium nitrite, 158 grams of sodium ethyl sulfate and 8.6 grams of potassium carbonate and it's not distilling, it's a really bad problem. During the reaction it turns into stone and is very difficult to clean, synthesis always fails.

TucoSalamanca.Have you checked the sodium ethyl sulfate? You may be missing one of your reagents

 

[wael gano]

I'm distilling 103.5 grams of sodium nitrite, 158 grams of sodium ethyl sulfate and 8.6 grams of potassium carbonate and it's not distilling, it's a really bad problem. During the reaction it turns into stone and is very difficult to clean, synthesis always fails.

TucoSalamanca.This is the solution. After the CO2 comes out of the water, the nitroethane will fall to the bottom, be separated, and re-distilled. If you do not see this solution, go back to You are missing reagents.

 

[wael gano]

I'm distilling 103.5 grams of sodium nitrite, 158 grams of sodium ethyl sulfate and 8.6 grams of potassium carbonate and it's not distilling, it's a really bad problem. During the reaction it turns into stone and is very difficult to clean, synthesis always fails.

TucoSalamanca.

 

[wael gano]

I'm distilling 103.5 grams of sodium nitrite, 158 grams of sodium ethyl sulfate and 8.6 grams of potassium carbonate and it's not distilling, it's a really bad problem. During the reaction it turns into stone and is very difficult to clean, synthesis always fails.

TucoSalamanca.Start by making hydrogen ethyl sulfate, H2SO4+C2H5OH=C2H5HSO4+H2o.
One mole is 54 grams of H2SO4
Half a mole will produce 50% ethyl hydrogen sulfate.
50% H2so4 is unreactive
The reaction time is balanced at 2.5 hours
The temperature is 80 degrees C
Add 70 grams of sodium carbonate per mole of H2SO4
25 ml water
Stirring and waiting for the carbonation reaction
Now you have half a mole of sodium ethyl sulfate and half a mole of sodium sulfate with excess carbonate and water. Add 50 grams of sodium nitrite, with continuous stirring, raising the temperature, and distilling. You will produce 15 ml of nitrethane.

 

[TucoSalamanca.]

Start by making hydrogen ethyl sulfate, H2SO4+C2H5OH=C2H5HSO4+H2o.
One mole is 54 grams of H2SO4
Half a mole will produce 50% ethyl hydrogen sulfate.
50% H2so4 is unreactive
The reaction time is balanced at 2.5 hours
The temperature is 80 degrees C
Add 70 grams of sodium carbonate per mole of H2SO4
25 ml water
Stirring and waiting for the carbonation reaction
Now you have half a mole of sodium ethyl sulfate and half a mole of sodium sulfate with excess carbonate and water. Add 50 grams of sodium nitrite, with continuous stirring, raising the temperature, and distilling. You will produce 15 ml of nitrethane.

wael ganoCan you explain in more detail?

 

[G.Patton]

The simplest syntheses of nitroethane look at here, there are tutorials with video explanation.

 

[TucoSalamanca.]

The simplest syntheses of nitroethane look at here, there are tutorials with video explanation.

G.Patton

From sodium ethyl sulfate and a metal nitrite.​

1,5 mol sodyum nitrit (103,5 g), 1 mol sodyum etil sülfat (158 g) ve 0,0625 mol K2C03 (8,6 g) ile iyice karıştırılır. Karışım daha sonra 125-130 °C'ye ısıtılır; bu sıcaklıkta nitroetan oluşur oluşmaz damıtılır. Distilasyon akışı önemli ölçüde gevşediğinde ısıtma durdurulur ve ham nitroetan eşit miktarda suyla yıkanır, CaCl2 üzerinde kurutulur ve gerekirse bir miktar aktif karbonla rengi giderilir. Nitroetan daha sonra yeniden damıtılır ve fraksiyon 114-116 °C arasında toplanır. Teorik verimin %42-46'sı .
I tried this method you shared and it failed. I don't understand

 

[TucoSalamanca.]

upp

 

[wael gano]

upp

TucoSalamanca.Please read carefully you will understand
Do you have concentrated sulfuric acid and absolute ethanol? Contact me and we can start synthesis with you

 

[TucoSalamanca.]

Please read carefully you will understand
Do you have concentrated sulfuric acid and absolute ethanol? Contact me and we can start synthesis with you

wael ganoLook, I can make sodium ethyl sulfate, that's not the problem, the problem is making nitroethane.

 

[TucoSalamanca.]

Please read carefully you will understand
Do you have concentrated sulfuric acid and absolute ethanol? Contact me and we can start synthesis with you

wael ganoTell me in detail how to make nitroethane.

 

[TucoSalamanca.]

Or friends, how can you make it with diethyl sulfate? I also have this reagent.

 

[The-Hive]

Vapor phrase off Propane + nitric acid easy to do but tweaking the flow is hard

 

[Mo0odi]

Vapor phrase off Propane + nitric acid easy to do but tweaking the flow is hard

The-HiveI think it produces faster and bigger


But there will be a risk of explosion

 

[The-Hive]

Keep it at 400°c and you’ll be fine

 

[Mo0odi]

Keep it at 400°c and you’ll be fine

The-HiveHave you tried making it, or are you thinking about making it?

 

[The-Hive]

Have you tried making it, or are you thinking about making it?

Mo0odiIve done it cupple times on a small scale

 

[The-Hive]

I wasn’t goin to post this but it’s Christmas tomorrow

do not use a flame and use straight pipe not zigzag this was 1937 we more clever in this day and age. Obviously flow rate needs to be spot on and temperature not exceed over 400°c propane automatic flash is 420-450°c you will be seeing god

end product you’ll get 4 nitros simple distillation required for nitroethane

last time I done it was 5 years ago sketchy synthesis

 

[wael gano]

I wasn’t goin to post this but it’s Christmas tomorrow

do not use a flame and use straight pipe not zigzag this was 1937 we more clever in this day and age. Obviously flow rate needs to be spot on and temperature not exceed over 400°c propane automatic flash is 420-450°c you will be seeing god

end product you’ll get 4 nitros simple distillation required for nitroethane

last time I done it was 5 years ago sketchy synthesis

The-HiveEthane (C2H6)
Propane C3H8

 

[The-Hive]

Ethane (C2H6)
Propane C3H8

wael gano

 

[nitro]

I wasn’t goin to post this but it’s Christmas tomorrow

do not use a flame and use straight pipe not zigzag this was 1937 we more clever in this day and age. Obviously flow rate needs to be spot on and temperature not exceed over 400°c propane automatic flash is 420-450°c you will be seeing god

end product you’ll get 4 nitros simple distillation required for nitroethane

last time I done it was 5 years ago sketchy synthesis

The-Hive

Obviously flow rate needs to be spot on and temperature not exceed over 400°c propane automatic flash is 420-450°c you will be seeing god

You can be safe with the flash point of the propane because the rxn mixture is supposed to be oxygen free. No oxygen, no flash. So just ensure you have no oxygen in your reaction and everything will be your way. Besides, the industrial way of propane nitration envolves pressures way exceeding the normal (8 to 12 atm) thus increasing flash point temperature anyway.

 

[The-Hive]

You can be safe with the flash point of the propane because the rxn mixture is supposed to be oxygen free. No oxygen, no flash. So just ensure you have no oxygen in your reaction and everything will be your way. Besides, the industrial way of propane nitration envolves pressures way exceeding the normal (8 to 12 atm) thus increasing flash point temperature anyway.

nitroI keep it at 350-400 seems good takes hours as I run it verry slow