TurboZfreak
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UM..... Help "ETN"
Since my testing with ETN with my caps I decided to make a large batch. I started with 144ml of H2SO4 98% and 68ml HNO3 96%~. I started by cooling
both portions of acid to -5c and mixed them. Temp raised to a max of 29c. I cooled both back down to -5c. I made an ice bath and put the mixed acid
into a 500ml beaker in this ice bath. I started adding 24g 1.5g at a time over 10mins, temp never got above 5c. After final addition I stirred for 5
mins and let it nitrate for 60mins stirring every 10mins or so according to users advise on here which would give better yield. At the 15min interval
I pulled the beaker off the ice bath and let it slowly climb to 10c at the end of the hour. About at the 40min mark there was a separation of the acid
solution at the bottom and condensed erythritol and or etn at the top. At the end of 60 mins... and this is where it get crazy.. I crashed the stirred
mix into 750ml of cool water. A LOT of nitrogen dioxide started to form and the whole mix started to get hot. Climbed to 58c and brown sludge started
globing at the bottom. I immediately crashed that onto 1L of ice water. I stirred it around and ETN started to precipitate.... but unlike before where
it looks like snow, this time it started to crystallize into HUGE crystals along with some smaller snow like crystals. I have never seen crystals like
this before... Can someone help me to understand what happened... I washed them and neutralized them with sodium bicarb solution and they are drying.
I am not sure what to do with these and I am kinda scared of disturbing them.
  
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TurboZfreak
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UPDATE:
Been drying for a little while, still kinda wet. I took one of the tiny crystal chunks and put a hammer to it. It made a louder report and a small but
bright flash. I have hammered similar amounts but of powder and it has never been like that. I am pretty sure these are ETN crystals. Largest crystal
is almost the diameter of a quarter.
[Edited on 16-3-2014 by TurboZfreak]
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hissingnoise
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| Quote: | | A LOT of nitrogen dioxide started to form and the whole mix started to get hot. |
That would suggest that there was still unreacted erythritol in soln.!
At 0°C nitration proceeds slowly so that each addition is only partially nitrated before the next addition, allowing a build-up of erythritol in the
acid . . .
Nitration @ ~15°C with slow addition will allow a more complete, safer reaction!
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NeonPulse
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if the additions are done at too cold of a temp and too fast- then it is allowed to warm up and the built up un-reacted erythritol all want to react
at once causing problems. Your brown sludge could have been molten ETN as its MP is 61c so the thermometer may not have registered the spike up in
temp fully if you crashed it fast. Also you should crash the acids in more water to begin with 1L is a safe bet and have it ice cold for best results.
It sucks to filter so much liquid but you can be sure your ETN has fully precipitated. what was the final yield anyway? would be interested in seeing
how the problems you had affected the end result. you should also recrystallize it for safer keeping they will last alot longer and store pretty much
for years as long as it is well neutralized.
[Edited on 16-3-2014 by NeonPulse]
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Stortulling
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Do I need Sulfuric Acide?
'm sorry to bring up an old thread. The reason is that I've read many different syntheses for ETN, and no two are alike .. temperatures ranging from
+5 C to +45 C, and mixing ratio between SA and NA vary quite a bit. Of course, much of this is due to the concentration of NA, but then comes what I
wonder about. In a thread I read on this forum, someone wrote that you do not need SA if you have a high enough concentration of NA (>95%?), and
yield are better without SA. So what is high enough and does anyone know of the synthesis without SA?
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