Laurelium
Harmless
Posts: 11
Registered: 10-5-2023
Member Is Offline
Mood: Methylated
|
|
Sulfamine to Ammonium Ethyl Sulfate question
To begin with, sorry if this post is separated from its original thread. I wasn't able to securely login on the page in order to post this reply.
Following the discovery of the thread below started by Antoncho, I was left to question what "sulfaminic acid" was. I UTSE as well as Science
Madness's Wiki & Forum to no avail.
When translating bwz's post below from russian, I get "sulfamine" instead. Would I be wrong to assume that sulfamine/sulfaminic acid
is ammonium sulphamate made from the hydrolysis of sulfamic acid with aqueous ammonia ?
The 10th post of the first page by Antoncho ~ ~ ~ Thread: https://www.sciencemadness.org/talk/viewthread.php?tid=15837
Quote:
Originally posted by bwz at https://www.hyperlab.info/inv/index.php?act=ST&f=17&... [Page 1, 18th post] *[Page 1, 19th post which speaks of this process gets
translated as sulfamine; 200g сульфаминовой or 1Kg сульфаминки]*
200 g sulfaminic acid pulverized w/a coffee grinder (Note 1) and 300 mls anhydrous EtOH (which was grudged) was refluxed for 3 hrs in a 2 l flask
(Note 2). The most part of HSO3NH2 dissolved and a pool of melted NH4EtSO4 is formed on the flask's bottom under the layer of alcohol. EtOH is then
removed - first with an aid of slight vacuum, then - at 15 mmHg. The residue of melted NH4EtSO4 crystallized slowly, one has to catch the moment when
it gets completely solid, but is still soft. After ir crytallizes fully, it is very hard to recover from the flask. Finally it was obtained 270 g of
white crystalline agregates.
295-270=25 g -- EtOH not reacted with sulfamic acid = 52 g unreacted acid
52/270*100=19,3% -- sulfamic acid content in the final product
(270-52)/295*100=73,9% - the yield of ammonium ethyl sulfate.
The product was then neutralized with Na2CO3 and evaporated to sp. gravity of 1,34 g/cm3. It still had a weak smell of ammonia due to the present
ammonium sulfamate. After filtering out the crystallized salts the volume of the solution constituted 275 mls.
It was reacted with :
60 mls water
12 g K2CO3
137 g NaNO2
1 mls polymethylsiloxane
...to yield 29 g (34% on NaEtSO4) of clear colorless liquid.
Note 1. It's probably not necessary to pulverize the acid since almost all of it dissolves anyway.
Note 2. The flask should have a bottom surface as large as possible since beecause of the alcohol economy there's a layer of NH4EtSO4 on the bottom
that partially retains sulfamic acid. The author had to stir it with a knitting needle occasionally. Using a stirrer would allow to avoid this
problem.
[Edited on 19-5-2023 by Laurelium]
|
|
|
Laurelium
Harmless
Posts: 11
Registered: 10-5-2023
Member Is Offline
Mood: Methylated
|
|
Looking back at it, it seems that it would be 200g of Sulfamic acid which when refluxed with EtOH give a dissolved solution of NH4EtSO4...
This thread may go to Detritus but I still find it hard to believe that Antoncho would have made a mistake in the translation.
|
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
