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Author: Subject: ETN synthesis problem
domstp
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[*] posted on 24-5-2010 at 08:35


thanks, that was what i was looking for.
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quicksilver
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[*] posted on 25-5-2010 at 05:51


hissingnoise 's response is possibly the most important however there is another significant issue. Often "sub-nitration" are produced such as "di & tri nitrates" and these may be soluble in water and lost to the final yield. They may play a role in that, they may be productive energetic materials if utilized WITH the final appropriate nitrated product. This is significant in nitric esters especially the solid alcohols.
Small yields of mannitol are the most obvious of these. Their occurrence in PETN has been documented by several chemists as well. Since Erythritol is very fast nitration, the possibility of various byproducts as sub-nitrations is very possible. Normally these would co-exist but with excess water it's possible they'd be washed away.
This is one of the reasons why scaling up is not always a case of multiplication of materials. What may be fine with 5gr of solid alcohol may have a lesser yield with a value of 30gr.




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gnitseretni
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[*] posted on 25-5-2010 at 06:04


Is a fast addition time a way to reduce sub-nitrations?

I've read posts where folks use long addition times. If after the last addition they let it react for 15 minutes, then the first addition has had a reaction time of one hour and 15 minutes, and the last addition only a mere 15 minutes. Is this large difference in reaction time a cause of sub-nitration?
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quicksilver
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[*] posted on 25-5-2010 at 11:55


Quote: Originally posted by gnitseretni  
Is a fast addition time a way to reduce sub-nitrations?

I've read posts where folks use long addition times. If after the last addition they let it react for 15 minutes, then the first addition has had a reaction time of one hour and 15 minutes, and the last addition only a mere 15 minutes. Is this large difference in reaction time a cause of sub-nitration?



It is very difficult to say that one specific method would result in a lack of sub-nitration because each nitration is a somewhat unique reaction. Great effort goes into making a nitric ester consistent on a plant-level.
For many purposes they are not a negative bi-product....but for a situation that demands consistency such as smokeless powder they certainly are. To answer the question (TTBoMK) it's a CONSISTENT addition (or rather exposure) that would make a difference. Say you find that adding your solid alcohol to a mixed acid milieu in weight of .25 gram every 3 minutes is appropriate to maintain reaction (or deflect run-a-way). If then you actually set a timer (wrist watch) to your additions, you may have the best chance to maintain a single-level nitration (see: Federoff).




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gnitseretni
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[*] posted on 27-5-2010 at 08:48


Made some ETN.





10g Erythritol
50g KNO3
150ml H2SO4

Yeah, I know.. that's a LARGE excess H2SO4 ;)
I recrystalized the ETN from acetone/methanol (50/50).
Anyways, I know it's nothing special.. I was just a little bored and felt like sharing :P
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Justin
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[*] posted on 27-5-2010 at 14:45


What was your final yeild?? i like the electric mixer idea!! may have to try that, however im a bit concerned about the acids corroding the metal mixers, my wife would be sooooo PISSED!!! LMAO
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gnitseretni
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[*] posted on 27-5-2010 at 16:17


Yield was kinda bad.. only 11 grams. I thought for sure I would have more than that when I drowned the mixture and saw a thick layer form at the bottom. Although it did look a little... fluffy. I left the mixer on for 20 minutes after the last addition. I'll make it 30 next time.

The mixers start rusting after just two uses. I just sand the rust off and reuse them.
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seppe
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[*] posted on 28-5-2010 at 08:23


hey i m new on this forum ... i need littel help ... etn how much dissolves in 61 degrees hot ethanol thx boys
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Jimbo Jones
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[*] posted on 28-5-2010 at 10:57


Based on my tests, the nitration of ETN is the easiest of all nitric esters (except EGDN I guess). Yields are excellent, even with the nitrate & acid combo. The biggest problem with the solid sugars is there slow rate of solubility. The electric mixer is not a bad idea, but manual stirring in every five minutes or so will give you the same results. 100 ml. 95 % sulfuric acid, 75 gr. AN (recrystallized) and 15 gr. E gave me around 21 – 22 gr. pure, recrystallized from methanol ETN. For maximum yields the E have to be ground to very fine powder, which speeds the nitration considerably. Add in little portions with good stirring to prevent the clumping. Some people left the mixture from 20 to 30 minutes after the last addition, but around 1 hour is good if you want to achieve maximum yields. The recrystallization from alcohol is also very simple. For every 10 gr. ETN I use around 100 ml. hot methanol (forget the acetone). The temperature must be below 60 °C, because of the ETN low melting point. Stir the crystals until everything dissolve, then test with litmus paper and add little portions sodium carbonate if this is necessary. The hot solution is filtered directly in container with ice cold water and 1 % urea. I use magnetic stirrer for the water, but manual stirring is also ok.
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seppe
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[*] posted on 28-5-2010 at 11:56


Thanks for your help .... But the information I need for ethanol ... is the solubility of methanol almost like ethanol
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Jimbo Jones
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[*] posted on 28-5-2010 at 12:04


Yes, but I prefer methanol. Pure.
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gnitseretni
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[*] posted on 28-5-2010 at 12:31


I've used the mixer for a long time, but I only used it with HNO3/H2SO4 mixtures. I just recently started using it with KNO3/H2SO4 mixtures. I used a large excess of H2SO4 in my last synth a few posts up, but the first time I did it I used the right amount of H2SO4 and found that the mixture was too thick... eventually the mixture became so viscous that the container itself began to turn instead of the mixture :P So if you're gonna use a mixer then either use an excess of H2SO4 or find a way to secure the container to keep it from turning. But best to use it with HNO3/H2SO4 mixtures in my opinion.

I like using the mixer because I have my hands free to do other stuff, like in between additions I can back away to avoid those nasty HNO3 fumes.

Btw, the electric mixer is best used with larger synths. With smaller synths you use smaller containers, obviously, which might create problems. For example, I used a canning jar in my last synth. The mouth of the jar was very narrow and some of the material to be nitrated hit the top of the metal mixer and flew against the walls of the jar, which I had to scrape off from time to time. I didn't have this problem with larger synths, because the mixture completely covered the metal mixer. This problem can be overcome by cutting the four 'blades' on the metal mixer in half.. leave the bottom half of the blades attached to the mixer but remove the top half so there's nothing there that will hit the material to be nitrated against the walls of the container. If I didn't explain that well enough, see picture below.

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JohnWW
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[*] posted on 28-5-2010 at 13:05


That mixer looks like an egg-beater! But, in view of its being used to agitate HNO3-H2SO4 nitration mixtures, what metal are the shaft and blades made of? Or are they fully coated with some acid and heat resistant non-metallic material like PTFE?
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gnitseretni
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[*] posted on 28-5-2010 at 13:35


Yeah egg-beater.. hand-mixers whatever you wanna call em. They're only 7 bucks or so at the Walmart. As for the material.. not sure, probably some shitty quality SS. They start rusting after just one or two uses. But just sand the rust off and/or dip them in HCl and they're good to go again.
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seppe
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[*] posted on 30-5-2010 at 08:46


is re-crystalization etn more sensitive to friction and impact than not re-crystalizion etn ?
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hissingnoise
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[*] posted on 30-5-2010 at 09:23


Crude, non-recrystallised explosives are usually more sensitive because their purity is questionable.
Recrystallisation of these compounds is always recommended. . .

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maxidastier
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[*] posted on 16-6-2010 at 09:49


....if you don't use it immediately or dissolve it in NG or whatever. ;)
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pjig
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[*] posted on 16-6-2010 at 22:18


As far as ETN goes,,, is there a way to indefinitely store it ? I'd assume that in a aqueous solution of alcohol or maybe h2o would work. I know this is how they store picric acid( in 10-30% h2o). Would it store in a solvent like nitromethane for a long period of time (few years)?
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[*] posted on 17-6-2010 at 04:41


I think acetone would be a good choice in this regard, as you know the ETN won't come out of solution.
By adding an excess of sodium/calcium bicarbonate with urea to fight off any acidity would be advantageous.

The bicarbonates would dissolve in the water, along with other impurities when recrystallizing your ETN.
Then just follow the 50/50 ethanol/acetone route to get finer crystals.




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hissingnoise
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[*] posted on 17-6-2010 at 05:53


If ETN is well neutralised and recrystallised a few times it should be pure enough for indefinite storage in a fridge. . .

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maxidastier
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[*] posted on 3-7-2010 at 09:57


Can someone help me with the equotation?
I'd like to use my distilled 98% HNO3 instead of KNO3..

What amounts are needed for 10 g Erythritol?

Can someone suggest me a chemistry calculator? I read about the gnome chem calculatur, but I don't have ubuntu.
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quicksilver
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[*] posted on 4-7-2010 at 11:00


If you really want one of the best suites then I'd suggest ChemOffice because then you could calculate, illustrate, & have a great deal of fun.
http://www.cambridgesoft.com/software/ChemOffice/

That and a strong undergrad textbook like ISBN 0-534-17035-8 (look that up on Amazon, they have used copies from about 30 large universities.)

[Edited on 4-7-2010 by quicksilver]




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maxidastier
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[*] posted on 9-7-2010 at 09:46


Well, thank you, but as I see, this programm as a little bit overseized.
I really just need a equotation programm, that knows molar mass and those things to calculate how many grams/mls are needed nitrate 10 g of ETN etc...
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[*] posted on 13-1-2012 at 18:45


help,
i cannot understand why my nitrations are going ary, with the proven 1;4;12 ratios and the nitrification appearing to go well, not very thick until it nitrates for an hour or so. beautiful crystals needle like come out of the freezer. but i can't know what i have here.... no bang
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sdodgen62
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[*] posted on 14-1-2012 at 06:31


maybe it has something to do with using a denatured alcohol instead of ethanol hmmmm
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