xwinorb - 1-2-2010 at 02:19
I would like to know if someone has tried the method for making ethyl sulfate ( hydrogen ethyl sulfate ) as described in the US Patent Office
3,024,263.
It says ethyl sulfate can be made from ethyl alcohol and sodium bisulfate ( the author used the monohydrate salt of sodium bisulfate ). Reflux till
all the sodium bisulfate is consumed and only the finer sodium sulfate remains in solution. Cool down to form the Glauber salt ( decahydrate ).
Supposed to remove all water.
Filter out the sodium sulfate, distill out the ethyl alcohol and neutralize with sodium carbonate to obtain the sodium salt of ethyl sulfate.
Does this work as stated ?
I was thinking about another possible way : Painkilla has posted in this forum a very detailed procedure for making methyl sulfuric acid and then DMS.
It is attached to one of his posts, in PDF format, I have it.
I think that by using his method and replacing methanol with ethanol would produde ethyl sulfate.
EDIT by XW : ( I mean to make the ethyl sulfate only, then neutralize it with sodium carbonate to get the sodium salt of ethyl sulfate. NOT to follow
Painkilla's procedure completely, just the first part ).
Is this correct ? Any problems ?
I have also a few other methods as listed on the Rhodium nitroalkene FAQ, listed under sodium ethyl sulfate. Indeed, those are complicated, one of
them uses oleum. I would like something more OTC and simple if possible.
[Edited on 1-2-2010 by xwinorb]
Myfanwy - 1-2-2010 at 03:09
I tried it with EtOH and NaHSO4.
The most stuff,whats produced is Et2O, because NaHSO4 is a catalyst for the condensation of 2 EtOH
molecules.
I got nearly no EtHSO4, just Et2SO4.
No bubbles were produced, by adding Na2CO3.
Why not cool down Ethanol and Sulfuric acid below 0°C and give them both together.
This worked and i made Diethyl sulfide.
xwinorb - 1-2-2010 at 05:18
Many thanks.
FedeJuninArg - 19-3-2015 at 12:48
Hi I have tried this: https://www.erowid.org/archive/rhodium/chemistry/nitroalkane...
EtOH + concentrated H2SO4, boiled maybe half an hour under reflux. Some Et2O was produced..
When I add Na2CO3 to neutralize there's a lot of fizzing so it's working.. but at the end the mixture turns into a white milkshake and I don't know
what to do next.. Should I heat it on a water bath at 60ºC as the article says?
How can I isolate the product?
Thanks !!
Metacelsus - 19-3-2015 at 12:57
How does fizzing show that it's working? Couldn't it just be unreacted sulfuric acid getting neutralized?
Anyway, if it is working, then you should filter the solids out and collect the solution.