golfpro
Banned
Posts: 179
Registered: 18-5-2013
Member Is Offline
Mood: Cap Sensitive
|
|
Erythritol powdered or coarse (ETN)
I have made ETN multiple times before and I've always got around the same amount of Erythritol TetraNitrate as Erythritol I used or in other words
around a 45% yield, I am starting to think the Erythritol must be finely powdered in order to get a good yeild, I usually grind for a few minutes the
erythritol down to a grainy powder w/ a mortar and pestle but never made the effort to make it into a fine powder.
This would make sense seeing how the Erythritol doesn't dissolve well in sulfuric acid/nitric acid mix as far as I can see.
I have tried using sulfuric acid/AN as well as sulfuric acid/HNO3, different temperatures, different amount of time etc.
[Edited on 11-11-2013 by golfpro]
|
|
|
VladimirLem
Hazard to Others
Posts: 204
Registered: 24-5-2010
Member Is Offline
Mood: Have no fear <Vlad> is here.
|
|
Quote: Originally posted by golfpro  | I have made ETN multiple times before and I've always got around the same amount of Erythritol TetraNitrate as Erythritol I used or in other words
around a 45% yield, I am starting to think the Erythritol must be finely powdered in order to get a good yeild, I usually grind for a few minutes the
erythritol down to a grainy powder w/ a mortar and pestle but never made the effort to make it into a fine powder.
This would make sense seeing how the Erythritol doesn't dissolve well in sulfuric acid/nitric acid mix as far as I can see.
I have tried using sulfuric acid/AN as well as sulfuric acid/HNO3, different temperatures, different amount of time etc.
[Edited on 11-11-2013 by golfpro] |
its defenitly better to use very fine powders...a really strange example is nitrating fructose...when the crystals are huge, then you can see, that
the surface of them become slighly yellow when nitrating and the core stays white crystalline (unnitrated/undernitrated)...and the yield is
horrible...
i've seen a patent that said that good results are able with the H2SO4/HNO3 version with 88% HNO3...so maybe use more H2SO4 when not having high
concentrated HNO3 and boil the mixed acids after the nitration to get the H2SO4 back (without nitrated stuff left in there, of course  )
another idea (carefull to handle and you should first look if there are patens that agrees with this) could be warming up (<35C) the nitration bath
after all erythrol is in it...acids are "stronger" if they are warm....BUT first go and search if this way could be used
!
|
|
|
golfpro
Banned
Posts: 179
Registered: 18-5-2013
Member Is Offline
Mood: Cap Sensitive
|
|
This can be used, I've done it this one says to allow the ETN to rise up to 40*C and then keep it at 45*C at the very end with continued stirring,
then cool down to 10*C. This method was done and got 90% yield (350g) but used a heavy excess of anhydrous Nitric Acid and sulfuric acid.
http://www.wydawnictwa.ipo.waw.pl/cejem/vol-10-03-2013/Kunze...
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
