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LardmanAttack
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Awful ETN yields
So i've been using ETN as my explosive of choice for a few months now for testing as it just performs excellently 90% of the time, but the only
problem is, I can't seem to get good yields out of it, And its an absolute pain in the ass and waste of money/time to make a shit ton of nitric acid
from nitrate from cold packs, I have to wait until it's all distilled, and hope to god that something doesn't go wrong in that timespan, only to be
left with garbage yields for the time/money/effort I put into it (100mls of 70-80% nitric only gives me like 20-25g of ETN in the end, and don't get
me wrong, thats not a horrible yield, it's just not at all practical) the only main thing I can think that is going wrong is me using low quality
drain cleaner acids, but I get much higher yields comparatively with low quality acid with something like NG than I do ETN. I have distilled sulfuric
before, but frankly, it's a huge pain in the ass, it takes forever, is scary to deal with and just not fun overall, I remember that I did distill and
use pure sulfuric a few months ago, and my yields were better, but not as much as you'd expect. I assume I just must be screwing something up in the
synthesis that leads to such low yields, I would appreciate it if anyone could give me some tips on how to improve this.
[Edited on 4-1-2020 by LardmanAttack]
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LardmanAttack
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Also to clarify before anyone asks, yes my erythritol is pure, that was a big problem for me in the beginning but just recrystallized and recently
I've found a pure source, also I can't exactly remember how much of an increase you are supposed to get out of the synthesis but I think it was
something like 2x the amount of erythritol at 100% yield? correct me if i'm wrong, at the very least i'd be satisfied with a 1.5 increase.
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caterpillar
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Weak acid.
Women are more perilous sometimes, than any hi explosive.
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XeonTheMGPony
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Some actual information would be nice, like how long, temps maintained, total volumes, stirring method.
There is two massive threads on here dedicated to ETN.
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Tsjerk
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Do you actually use sulfuric acid? And if so, what concentration?
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LardmanAttack
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Quote: Originally posted by XeonTheMGPony  | Some actual information would be nice, like how long, temps maintained, total volumes, stirring method.
There is two massive threads on here dedicated to ETN. |
Usually I keep the temp between 10-15C and add the Erythritol in over a period of around an hour and a half.
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LardmanAttack
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Yes, It's crappy drain cleaner acid, but i've measured the conc. to be about 93% and many people have used drain cleaners that are very similar using
just the nitrate salt method and have gotten much higher yields than me.
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caterpillar
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Nitrate, dissolved in sulfuric acid is a more powerful nitrating agent than usual mixed acid. much less water, savvy?
Women are more perilous sometimes, than any hi explosive.
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XeonTheMGPony
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this has all ways given best yield, or pure wfna.
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caterpillar
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Assume, you have concentrated NA. Do not waste it nitrating erythritol- make HMX or RDX.
Women are more perilous sometimes, than any hi explosive.
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LardmanAttack
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Really? I assumed that the extra impurities added from this method would lower yields even more than normal.
I guess I can try it to see how well it performs. If it does work well it would save me a lot of time.
[Edited on 6-1-2020 by LardmanAttack]
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XeonTheMGPony
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I make it as I need it, no waste.
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XeonTheMGPony
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| Quote: Originally posted by LardmanAttack |
Really? I assumed that the extra impurities added from this method would lower yields even more than normal.
I guess I can try it to see how well it performs. If it does work well it would save me a lot of time.
[Edited on 6-1-2020 by LardmanAttack] |
The impurities are all soluble in cold water, where the ETN is not, the water is what really makes for crap results, Ammonium Nitrate is the best
stuff, Potassium works but it pays to chill the mix and filter out the solid potassium sulfate, or use more Sulfuric acid to thin it.
With the Ammonium nitrate the mixture remains very stirrable.
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caterpillar
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| Quote: Originally posted by XeonTheMGPony | | Quote: Originally posted by LardmanAttack |
Really? I assumed that the extra impurities added from this method would lower yields even more than normal.
I guess I can try it to see how well it performs. If it does work well it would save me a lot of time.
[Edited on 6-1-2020 by LardmanAttack] |
The impurities are all soluble in cold water, where the ETN is not, the water is what really makes for crap results, Ammonium Nitrate is the best
stuff, Potassium works but it pays to chill the mix and filter out the solid potassium sulfate, or use more Sulfuric acid to thin it.
With the Ammonium nitrate the mixture remains very stirrable. |
AN most likely works well if you wanna make ETN- its preparation doesn't require hi temp. But I got runaway reaction, trying to use AN dissolved in
sulfur acid, nitrating phenol. KNO3 worked well- no runaway.
Women are more perilous sometimes, than any hi explosive.
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LardmanAttack
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So I tried the ammonium nitrate/sulfuric method, and it was marginally better than normal, seeing how little work compared to before this method is,
i'll definitely stick with doing it this way in the future, also I probably didn't get a great yield due to my ratios being off, does someone have
some that works well for them?
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XeonTheMGPony
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start keeping notes, try to go longer nitrating time, I do my additions at 5c I add at a rate to maintain that in an ice bath, after all additions I
allow to warm to room temp under stirring then dwell there for 30m befor quenching in ice water.
I Thoroughly powder and sift the Erythritol, I leave the A.N. as prilled addition of that takes longer but I can go at a faster rate as the
dissolution is slowed hence so is the exotherm (That and if you go too slow you end up with a puddle *Damned humidity*)
the rest scales to the planned batch size
Erythritol Tetra Nitrate E.T.N So we need 4 nitrate groups for each Erythritol Mol,
So 4:1 ratio + % excess for good measure.
So how many Mol of Erythritol are you using? how many Mol of Ammonium nitrate are you using, what is your % excess of NO3 group you have in solution?
I was a slave to the recipe method my self, it was a weakness that annoyed me so I learned about Stoichiometry.
https://www.khanacademy.org/science/chemistry/chemical-react...
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Tsjerk
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Baking your ammonium nitrate, I always used powder, in an oven at 180 degrees for a couple of hours is adviced. When making PETN I think I let the
nitration go at room temperature for about an hour after the ice bath melted. Doesn't hurt, even if unnecessary.
Using 50% excess nitrate doesn't hurt when using a cheap one like ammonium nitrate, just use enough sulfuric to keep it stirrable. If you don't have
one yet, get yourself a magnetic stirrer, you will love it.
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Pyro_cat
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On Ice baths in general,
Glue some cross beams into the ice bath container so you can freeze water in the container and the cross beams stop the ice from floating up when you
add water. This way the bottom of the beaker is directly on the ice instead of getting cooled just on the sides.
Putting stones in the water before freezing works too.
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XeonTheMGPony
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Tannerite is a good source for bone dry A.N.
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LardmanAttack
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I've always wondered if the ETN is slightly soluble in an acidic solution and if fully neutralizing it would give me a higher yield, is this true?
It's hard for me to tell.
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Microtek
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| Quote: |
Glue some cross beams into the ice bath container so you can freeze water in the container and the cross beams stop the ice from floating up when you
add water. This way the bottom of the beaker is directly on the ice instead of getting cooled just on the sides. |
Another way to solve this problem is called a raised shelf. The term is rather self explanatory - it is a shelf usually made of metal that you place
on the bottom of your water bath. There is room enough for a stirrer magnet under the shelf, and an ordinary magnetic stirrer is easily capable of
driving two magnets (one in the beaker and one in the bath). This ensures circulation in the bath as well as in the beaker. If you are using a flask,
you can suspend it with a clamp instead if you prefer.
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LardmanAttack
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So in summary: you want as little water as possible, use an excess of nitrate/nitric, start cold, then heat up slowly to around 20c to ensure full
nitration, and make sure erythritol is finely powdered. Anything else?
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XeonTheMGPony
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Spend more time learning about the reaction, why it does what it does.
1h of study will save you pounds of wasted chemicals and hours in wasted time and effort
Take notes of the reaction, then each one there after making particular notes of changes and how they effected the yield, change one variable at a
time.
Mixing, never enough mixing!
Use a slight excess of H2SO4 to facilitate easier mixing if needed.
http://www.sciencemadness.org/talk/viewthread.php?tid=83358
http://www.sciencemadness.org/talk/viewthread.php?tid=7209
[Edited on 13-1-2020 by XeonTheMGPony]
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LardmanAttack
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I know how the reaction works, I know chemistry, i'm not a complete amateur. I was just initially annoyed at how it wasn't working correctly, its not
like if you know the chemistry, your yields will automatically be perfect.
If I really need to prove it to you then fine.
Erythritol is a sugar alcohol with a molar mass of 122.120 g·mol, when added to a solution of nitric acid and sulfuric acid in the correct ratios, a
reaction called a nitration takes place, whereby the hydroxyl groups of the Erythritol are replaced with Nitro groups (NO2) thus creating a new,
explosive compound named Erythritol tetranitrate, Its explosive properties coming from the newly created NO2 groups and their ability to explosively
decompose while oxidizing any reductive elements (mainly carbon and hydrogen) in the chemical structure, thus creating a large amount of gases in a
short time
There. I know chemistry, although I can admit I'm a little rusty at stoichiometry.
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Tsjerk
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Not exactly, you form nitrate groups, not nitro groups. Despite confusing naming all around, they are quite different.
Being "rusty" at stoichiometry sound a bit strange to me. You get it or you don't, it is secondary school stuff for 14 year olds..
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