Rhodanide
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ETN.exe has stopped precipitating
Good afternoon! I have had this happen to me twice, the past two tries that I have attempted it.
Food Grade Erythritol + Nitric/Sulfuric acid mix = Absolutely nothing upon precipitation in water. I nitrate it in an ice bath like all the other good
home chemists. Just thought I'd note that.
The first time I did it it worked, the only thing I can think of being a variable is that the past two times that I attempted this, I first dissolved
the Erythritol in Cold Concentrated H2SO4, THEN, added the HNO3.
Help?
Please?
Anyone?
Thanks!
~T
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hissingnoise
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Too much water in the mixed acid, the sugar was damp or the quantities were wrong . . . ?
BTW, you can delete surplus posts with the edit button!
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Daffodile
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Its probably your food grade Erythritol. Mine had other sugars and flavoring. Probably won't do much, but if your HNO3 already isn't that
concentrated, you'll get a water soluble, lower nitrate.
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OneEyedPyro
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Temp is a huge factor, 15C seems to be perfect for ETN. Then you have rate of addition and a host of other factors. If first dissolving in H₂SO₄
was really the only difference then that must be it but something tells tells me there's another reason.
With that said I've also had failures with certain synths when using the same exact procedure and chemicals that were successful before.
[Edited on 14-4-2016 by OneEyedPyro]
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TandemDwarf3410
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Did you figure out what went wrong? I'm having the same problem. I've tried twice (98% sulfuric acid from Rooto drain cleaner, 68% Nitric acid made
from that and KNO3, erythritol off of amazon that has no other listed ingredients) and nothing whatsoever crashes out when the reaction mix is added
to cold water.
I mostly followed Dugan Ashley's procedure from here https://www.youtube.com/watch?v=nayL7P1TztA
The first time, I added the nitric and sulfuric acid slow enough to keep them at a sane temperature, but let them get hot. I then chilled the mixed
acid. After that reaction failed I tried again. I mortar and pestled my granular Erythritol in to a fine powder and kept my acids under 5 degrees C
while mixing them just in case, but still nothing.
I'm a bit annoyed, as it seems like I'm somehow messing up a very straight forward procedure without making any mistakes that are obvious to me, and
I've burned through a lot of the Nitric acid that I spent a lot of last weekend making.
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Texium
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Thread Moved
14-4-2024 at 20:03 |
OneEyedPyro
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Quote: Originally posted by TandemDwarf3410  | Did you figure out what went wrong? I'm having the same problem. I've tried twice (98% sulfuric acid from Rooto drain cleaner, 68% Nitric acid made
from that and KNO3, erythritol off of amazon that has no other listed ingredients) and nothing whatsoever crashes out when the reaction mix is added
to cold water.
I mostly followed Dugan Ashley's procedure from here https://www.youtube.com/watch?v=nayL7P1TztA
The first time, I added the nitric and sulfuric acid slow enough to keep them at a sane temperature, but let them get hot. I then chilled the mixed
acid. After that reaction failed I tried again. I mortar and pestled my granular Erythritol in to a fine powder and kept my acids under 5 degrees C
while mixing them just in case, but still nothing.
I'm a bit annoyed, as it seems like I'm somehow messing up a very straight forward procedure without making any mistakes that are obvious to me, and
I've burned through a lot of the Nitric acid that I spent a lot of last weekend making. |
Continuous stirring and temperature control is important with ETN.
Are you certain that your reagents are at what concentration you say they are?
Adding that last nitro group is the hardest since the acids will be at their weakest while the final group is least willing to attach. It's possible
you're getting the mono/di/tri which will dissolve in water upon crashing.
Try carefully starting your addition of erythritol a little sooner after mixing your acids while temps are still warm to the touch (30C) would be my
only advice.
[Edited on 15-4-2024 by OneEyedPyro]
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dettoo456
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You don’t necessarily need to crush the erythritol to a fine powder - crystals are fine to nitrate since they dissolve in the rxn mix.
Just keep the reactor <10C, agitate with strong stirring, add the polyol very slowly and don’t allow the temp to rise very much at all during
additions, and stir for an additional 20-30min after all of the polyol has been added (the 20-30min stirring afterwards can be w/out active cooling,
to allow the rxn to come to around room temp). Sorry for the run-on sentence.
The general rules for nitrate esters can be applied to almost all polyols, but primary alcohols (like Et, Me, & IPr) require mild heating and more
dilute acid conc%s.
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