Keras
National Hazard
Posts: 937
Registered: 20-8-2018
Location: (48, 2)
Member Is Offline
|
|
Hydrazine sulphate with sodium bisulphate
Folks,
the traditional way to get hydrazine sulphate is to mix sulphuric acid with the products of the Hoffman rearrangement.
However, since sulphuric acid has become quite tedious to find (at least over here in Europe), I suppose substituting it with a solution of sodium
bisulphate, which is on tap, is a better option?
|
|
karolus28
Hazard to Self
Posts: 51
Registered: 14-4-2019
Location: EU's Brazil
Member Is Offline
Mood: zgrzyt
|
|
One would probably end up with a lot of sodium sulfate contamination when crystalising out the product. In theory adding enough hydrochloric acid
would make Hydrazine Dihydrochloride and it should be possible to crystalise it out with cooling(some websites say it's solubility is 5g/100g @idk *C,
cuz they didnt write that), though I assume the yield would suck ass
Hi, please read about exif data.
|
|
Σldritch
Hazard to Others
Posts: 310
Registered: 22-3-2016
Member Is Offline
Mood: No Mood
|
|
I have process in hydrazine sticky for you (using Calcium Hypochlorite, Sodium Bisulfate, Urea). You have my permission to copy the wierd letter in my
username into the forum search engine bar.
|
|
Keras
National Hazard
Posts: 937
Registered: 20-8-2018
Location: (48, 2)
Member Is Offline
|
|
Quote: Originally posted by Σldritch | I have process in hydrazine sticky for you (using Calcium Hypochlorite, Sodium Bisulfate, Urea). You have my permission to copy the wierd letter in my
username into the forum search engine bar. |
The sigma? Ok, thanks.
|
|
Keras
National Hazard
Posts: 937
Registered: 20-8-2018
Location: (48, 2)
Member Is Offline
|
|
Quote: Originally posted by karolus28 | One would probably end up with a lot of sodium sulfate contamination when crystalising out the product. In theory adding enough hydrochloric acid
would make Hydrazine Dihydrochloride and it should be possible to crystalise it out with cooling(some websites say it's solubility is 5g/100g @idk *C,
cuz they didnt write that), though I assume the yield would suck ass |
Well, solubility of hydrazine sulphate is given as 30 g/L whereas that of sodium sulphate is around 300 g/L at 25 °C (and increases slightly with
temperature). I’ll have to juggle with those figures to see what yield of almost pure product can be extracted.
|
|
Σldritch
Hazard to Others
Posts: 310
Registered: 22-3-2016
Member Is Offline
Mood: No Mood
|
|
BTW using Calcium Hypochlorite you save even more acid because you can just filter off the Calcium Carbonate. And to be clear I used hydrochloric acid
AND Sodium Bisulfate. It was a while ago though so I can't really remember the details. You are better of checking my notes in the thread. IIRC I got
25% yield or so without gelatin and only using tap water. It is really very low tech. And it has worked every time for me - just don't cool it down
too much or you'll get Sodium Sulfate.
|
|
Keras
National Hazard
Posts: 937
Registered: 20-8-2018
Location: (48, 2)
Member Is Offline
|
|
OK. Fine, I've got quite a lot of it. It’s quite messy to work with, though, especially because it is never pure.
I’ll check your notes, thanks for pointing me to them! And happy new year!
|
|