Ethyl hydrogen sulfate synthesis

[Konstantin91]

Hi, i need help to synthesize sodium ethyl sulfate, which i plan to use to make nitroethane which i plan to use as substitude for diesel in ANFO. I just want to compare results of ANFO made with diesel and ANFO made with nitroethane...

 

So i have googled procedure which i think is rly good just need some adjusting. I will copy full procedure and elaborate my thoughts about it, what i need is advice from someone experienced in this so i dont end up with diethyl sulfate which is toxic (only reason why i didnt already conducted few experiments on my own and find out correct way to sodium ethyl sulfate)

 

Procedure.
In 500 ml RB Flask was added 100 ml EtOH (97% is high enough ? ) 96% Sulphuric acid 100 ml (180g) in small portions was added carefully with cooling. Na2SO4 60 grams were then added and the mixture heated to 120C and kept at that temp for 1 hour. Na2SO4 was filtered off and gave 130 ml of pink ethylsulphuric acid.
In a 500 ml RB flask in 300 ml EtOH (its essential to use not less alcohol, you'll se why if you wont) were added 66g unhydrous K2CO3. 75 ml of ethylsulphuric acid were added dropwise with mixing. The ethanol is then distilled off. The wet salt was heated on a plate standing on a water bath removing the remants of ethanol .

 

OK first part of procedure ethanol and sulfuric acid, its fine... Na2SO4 (sodium sulfate) i think (correct me if i am wrong) is used as drying agent to absorb all water which might destroy our product in hydrolysis... i have also found some references which says mixing ethanol and sulfuric acid on room temperature, no need for refluxing on 120 C, so which is correct.. ?

 

Second part of procedure we use ethanol again (i think here it is as solvent) and in that ethanol we added K2CO3 (anhydrous cause again we dont want water here) , after that ethylsulfuric acid (i think it is other name for ethyl hydrogen sulfate) is added dropwise with mixing. Ok here my thoughts about that, ethyl hydrogen sulfate reacts with K2CO3 to produce potassium hydrogen sulfate and potassium bicarbonate (KHCO3) , thats why in my opinion procedure is not so good cause we need to use Na2CO3 to get sodium hydrogen sulfate and sodium bicarbonate (NaHCO3)

One other problem i can see here, through procedure we always try to avoid hydrolysis which happens when ethyl hydrogen sulfate comes in contact with water but when we use ethanol in second part of procedure even if it is 97% it still have some water in it so when we add ethylsulfuric acid (ethyl hydrogen sulfate, whatever) we expect it to react with carbonate (potassium, sodium) and not with little water we have in ethanol...

 

I made this post so someone with far more epxerience than i have help me and elaborate procedure to me. I am also worried end product of this procedure might not be sodium (potassium, whichever carbonate we use) ethyl sulfate but diethyl sulfate which is toxic and only reason why i didnt myself find out by conducting few experiemnts already...

 

BTW sry for my english, its not so good...

Edited September 19, 2014 by Konstantin91

[Enthalpy]

Hi Konstantin95, no worry with your English, I'm happy that we share a language. But are discussions about explosives manufacture permitted on ScienceForums?

[Konstantin91]

Hi Konstantin95, no worry with your English, I'm happy that we share a language. But are discussions about explosives manufacture permitted on ScienceForums?

 

I have to admit i never read forum rules. It is only for academic purpose and i do not require instructions about explosive manufacturing cause i already know very much about that i am just conducting experiments in which i compare results.. I didnt even asked help for sodium ethyl sulfate synthesis cause i can do research on my own, these days you can find everything you need on google. I only asked for someone with enough experience to elaborate this particular procedure for me. As i said i am only afraid i might end up with diethyl sulfate which is toxic and i want to avoid that by any possible means thats why i made this topic here asking for help.

 

If this topic breaking forum rules so much pls delete it and accept my apology for harm i might made to forum by making it..