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LardmanAttack
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[*] posted on 3-1-2020 at 21:47
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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[*] posted on 3-1-2020 at 22:01


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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[*] posted on 4-1-2020 at 06:24


Weak acid.



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XeonTheMGPony
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[*] posted on 4-1-2020 at 08:11


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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[*] posted on 4-1-2020 at 08:45


Do you actually use sulfuric acid? And if so, what concentration?
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LardmanAttack
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[*] posted on 5-1-2020 at 02:28


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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[*] posted on 5-1-2020 at 02:30


Quote: Originally posted by Tsjerk  
Do you actually use sulfuric acid? And if so, what concentration?


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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[*] posted on 5-1-2020 at 05:22


Nitrate, dissolved in sulfuric acid is a more powerful nitrating agent than usual mixed acid. much less water, savvy?



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XeonTheMGPony
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[*] posted on 5-1-2020 at 09:45


Quote: Originally posted by caterpillar  
Nitrate, dissolved in sulfuric acid is a more powerful nitrating agent than usual mixed acid. much less water, savvy?


this has all ways given best yield, or pure wfna.
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[*] posted on 5-1-2020 at 15:43


Quote: Originally posted by XeonTheMGPony  
Quote: Originally posted by caterpillar  
Nitrate, dissolved in sulfuric acid is a more powerful nitrating agent than usual mixed acid. much less water, savvy?


this has all ways given best yield, or pure wfna.


Assume, you have concentrated NA. Do not waste it nitrating erythritol- make HMX or RDX.




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LardmanAttack
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[*] posted on 6-1-2020 at 03:18


Quote: Originally posted by XeonTheMGPony  
Quote: Originally posted by caterpillar  
Nitrate, dissolved in sulfuric acid is a more powerful nitrating agent than usual mixed acid. much less water, savvy?


this has all ways given best yield, or pure wfna.


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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[*] posted on 6-1-2020 at 03:39


Quote: Originally posted by caterpillar  
Quote: Originally posted by XeonTheMGPony  
Quote: Originally posted by caterpillar  
Nitrate, dissolved in sulfuric acid is a more powerful nitrating agent than usual mixed acid. much less water, savvy?


this has all ways given best yield, or pure wfna.


Assume, you have concentrated NA. Do not waste it nitrating erythritol- make HMX or RDX.


I make it as I need it, no waste.
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XeonTheMGPony
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[*] posted on 6-1-2020 at 03:42


Quote: Originally posted by LardmanAttack  
Quote: Originally posted by XeonTheMGPony  
Quote: Originally posted by caterpillar  
Nitrate, dissolved in sulfuric acid is a more powerful nitrating agent than usual mixed acid. much less water, savvy?


this has all ways given best yield, or pure wfna.


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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[*] posted on 6-1-2020 at 16:32


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.




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LardmanAttack
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[*] posted on 6-1-2020 at 23:42


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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[*] posted on 7-1-2020 at 04:10


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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[*] posted on 7-1-2020 at 11:28


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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[*] posted on 7-1-2020 at 12:39


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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[*] posted on 8-1-2020 at 04:12


Tannerite is a good source for bone dry A.N.
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LardmanAttack
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[*] posted on 9-1-2020 at 23:49


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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[*] posted on 10-1-2020 at 00:55



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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[*] posted on 12-1-2020 at 13:49


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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[*] posted on 13-1-2020 at 04:16


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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[*] posted on 14-1-2020 at 18:32


Quote: Originally posted by XeonTheMGPony  
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]


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 gĀ·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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[*] posted on 15-1-2020 at 01:42


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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