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I Successfully synthesized nitroethane but not pure can I make p2np with impure nitroethane.
HIGGS BOSSON
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Depends on how dirty your nitroethane is. Try putting a few grams in the microwave as an experiment.
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- By Manisj@1290
I used this method for making sodium ethyl Sulfate.
But after purify by ethanol my yield is very low quantity like 60g approx lots of sodium ethyl Sulfate not dissolved in ethanol. So I have throw undissolved Sodium ethyl Sulfate. I am very dispute how can I get maximum quantity of Sodium ethyl Sulfate??
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.
But after purify by ethanol my yield is very low quantity like 60g approx lots of sodium ethyl Sulfate not dissolved in ethanol. So I have throw undissolved Sodium ethyl Sulfate. I am very dispute how can I get maximum quantity of Sodium ethyl Sulfate??
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.
Add 215ml absolute ethanol
Add 108 ml (2 moles) of sulfuric acid slowly after the addition is complete. Heat to 80 degrees for 2.5 hours.
Turn off the heat and cool the mixture
Place it in a plate, then take 200 grams of sodium carbonate and add it until it equals the pH 8
After that, wait hours for the sodium carbonate to react well. Without adding water, there is a little ethanol. Allow it to evaporate into the air
The yield is 290 grams
Mixed moles of sodium ethyl sulfate
Mole of sodium sulfate
I used 2 moles of sulfuric acid, producing one mole of ethyl sulfate
One mole of sulfuric acid remains unreacted
Sodium sulfate, it doesn't matter, don't separate anything. Put everything and add 1 mole of sodium nitrite 103 grams with 50 ml of water and start distillation.
Add 108 ml (2 moles) of sulfuric acid slowly after the addition is complete. Heat to 80 degrees for 2.5 hours.
Turn off the heat and cool the mixture
Place it in a plate, then take 200 grams of sodium carbonate and add it until it equals the pH 8
After that, wait hours for the sodium carbonate to react well. Without adding water, there is a little ethanol. Allow it to evaporate into the air
The yield is 290 grams
Mixed moles of sodium ethyl sulfate
Mole of sodium sulfate
I used 2 moles of sulfuric acid, producing one mole of ethyl sulfate
One mole of sulfuric acid remains unreacted
Sodium sulfate, it doesn't matter, don't separate anything. Put everything and add 1 mole of sodium nitrite 103 grams with 50 ml of water and start distillation.