Originally posted by bwz at https://www.hyperlab.info/inv/index.php?act=ST&f=17&...
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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.
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So.... As you can see, the most interesting question now is whether it is possible to use regular 95% EtOH in this preparation and how successfully it
can bee used. Anyone willing to find that out? |