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Author: Subject: Erythritol Tetranitrate
Brightthermite
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[*] posted on 18-11-2021 at 18:27


I see in the video you are getting around 50 percent yields with this method. Is that the best you are able to obtain using "The Column"?
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[*] posted on 18-11-2021 at 19:39


I'll watch the video in a bit. Right now I recrystalized my yield and I am astonished to see the dirt that got into my ETN. It is much more powdered than my previous attempt probably because I powdered the stuff before adding it to the mixture.

It will probably be equal to my first yield, but absolutely terrible overall since my first attempt (which went very, very smoothly) ended up with a final yield of 6.5 grams from 5 grams of Erythritol. I will probably end up with 6 grams starting from 15 grams.

I hope with my teflon seals, and the hole I created in my thermometer adapter now sealed again, I hope to get half-decent yields of nitric acid. Even if I need to let them temperature run up very high.

Edit: final yield after recrystalization is 4 grams. There is some mild discoloration as well, which is why I am not going to mix it with my first yield. I think there is something up with it since when I tried to pop some by burning it on aluminum foil and a lighter what happened is some of the stuff dissolved and let off a tiny bit of red fumes. Others popped fine. It isn't 100% worthless, but it's mostly worthless. I'll need to dispose of this batch ultimately.

[Edited on 19-11-2021 by ManyInterests]

[Edited on 19-11-2021 by ManyInterests]
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[*] posted on 19-11-2021 at 12:27


It was only attempt. Maybe is possible obtain 60% from Column device. But 90% sure not.



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[*] posted on 19-11-2021 at 18:55


Well I think my nitric acid situation should be fixed. With the teflon seals my latest attempt yielded 77ml or so of very, very clean acid with a specific gravity of around 1.425. So around 70%. I want to make a few more batches before making maybe one more batch of ETN before I do NHN and RDX. Then I'll consider my chemistry hobby good and solved and move onto another interest... :)

Quote:
It was only attempt. Maybe is possible obtain 60% from Column device. But 90% sure not.


I am not sure if I want to make that specific column, it is an interesting experiment, but I will pass.

Also while writing this comment, I made two batches of nitric acid, one before I quoted you and now this one. I hope it 70%. If it is, then I have enough 68-70% for everything I need. I'll need to get started on WFNA.
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[*] posted on 20-11-2021 at 03:29


HNO3/H2SO4 give always better yields than H2SO4 / nitrate salts for ETN.



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[*] posted on 20-11-2021 at 04:47


Quote:
HNO3/H2SO4 give always better yields than H2SO4 / nitrate salts for ETN.


And much easier and much more efficient. I should have enough HNO3 for my NHN, HDN, and one more ETN synthesis. I will dispose of my last batch since I don't like it. My first batch is still excellent but I will need to pulverize it as It is still a touch grainy. But I am gaining confidence in ETN's stability, so I will powder tiny bits at a time with a rubber spatula.

Edit: my second batch of HNO3 made yesterday appears to have dropped in concentration to around 65%. It's still useable for ETN, I'll need to use a bit more. One thing I learned is that you always must put an excess of sulfuric acid. That's probably why my first batch of that day was much better.

[Edited on 20-11-2021 by ManyInterests]

[Edited on 20-11-2021 by ManyInterests]
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[*] posted on 28-11-2021 at 19:57


As a final note on my latest ETN synthesis. The yield I got was 13 grams after recrystalization and drying. Starting from around 9.9 grams of erythritol. Seems like the slightly less HNO3 concentration didn't affect it that much.

If I have to put a note in, never add any sodium bicarbonate/carbonate into the water when extracting the ETN, it will form a bit of a foam that will make the extraction a bit harder to pull off. I originally thought I did not need to recrystalize this time, but I think it is always a good idea. My yield after the initial extraction was 16.5 grams, but after recrystalizing I got the 13 of very pure ETN.
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[*] posted on 10-11-2022 at 04:26


Quote: Originally posted by Brightthermite  
Would love to hear your yield. Sulfuric acid and ammonium nitrate is a much easer bath to handle btw. I still need to get around to trying KN03. Apparently the yield is pretty good and its much cheaper for me then AN.


Does anyone know why this is? I've only ever used AN/H2SO4 and using KNO3 that I recrystallized would be much cheaper per pound. I would assume since they're both nitrate salts it wouldn't be much of a difference but I'm not sure.
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[*] posted on 10-11-2022 at 05:46


Using KNO3 will probably not be cheaper as you need about 2x the sulfuric acid to render the mix thin enough to stir.



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[*] posted on 10-11-2022 at 23:02


In all honesty I found that using nitric acid is much easier than using any nitrate salt. Like I want to make picric acid, and while I could use potassium or sodium nitrate (which I have plenty) I would rather make nitric acid and use that instead. The end product is easier.

When I made ETN using KNO3 the result was barely usable and the yield abysmal. Speaking of which, I did improve my ETN synthesis by recrystallizing it not in acetone, but in methanol. Methanol will give you a fine, powder-like result while acetone will make it crunchy and chunky. This might still trap some of the acid within it.

The ones I made in 2021 (described here) were actually still quite acidic since I didn't wash my ETN with enough water. This resulted in it becoming highly degraded when I placed it in blasting caps. I solved it simply by continuously washing the ETN in the filters until the water passing through no longer contained any acid (either using pH paper to test, or simply using bicarbonate on the water to see if it reacts).

Also I will say it again, recrystalize with methanol and add a pinch of urea in both the methanol and the water you will dump it into. This will scrub out any and all acids and will leave you with a very decent product that you can store for years without issue.
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[*] posted on 12-11-2022 at 19:25


How do you get your methanol? I don't have access to lab grade methanol. Would I have to distill something like HEET or could I just recrystallize using HEET since it has such a high conc of methanol? I don't think they use any additives.

[Edited on 13-11-2022 by BlackPowderBoy]
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[*] posted on 13-11-2022 at 00:10


I buy my methanol as methyl hydrate from hardware stores. It is 99.9% pure.

Where do you live? Is methanol restricted where you live?

Edit:

About my previous comment for picric acid with nitric acid... I think it would be much easier (and cheaper) to use the nitrate salt with that one, and even more efficient. I made my first successful picric acid synth today with sodium nitrate. I will need to recrystalize everything however.

[Edited on 13-11-2022 by ManyInterests]
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[*] posted on 13-11-2022 at 00:44


No it's not restricted near me, it's sold in hardware stores as well. I just wanted to make sure I didn't have to purify it first even if it appeared pure and clear. I bought HEET antifreeze and the msds says it is 100% methanol. It's crystal clear and appears to have no additives except in the msds it says something about 2 other chemical names..."proprietary, 0.0006% TO 0.00120" not sure what that means but hopefully those aren't some sort of colorless chemicals they add that would ruin the ETN during recrystallization.

[Edited on 13-11-2022 by BlackPowderBoy]
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[*] posted on 13-11-2022 at 12:52


Quote: Originally posted by ManyInterests  
Speaking of which, I did improve my ETN synthesis by recrystallizing it not in acetone, but in methanol. Methanol will give you a fine, powder-like result while acetone will make it crunchy and chunky. This might still trap some of the acid within it.


This can happen both with methanol and acetone.
There are reasons to favor acetone over methanol: less toxic, usually more available and if you compare solubility in methanol and acetone the latter is much much better. It's therefore easier to pour into a large volume of water with stirring and avoid creating two layers. With both solvents, in room temperature water you are going to get a crunchy crust and a mess if you pour slowly without stirring.
Urea scavenges NOx, it doesnt neutralize the acids but improves stability. You still have to use a base to do that.




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[*] posted on 13-11-2022 at 16:06


That's what I'm trying to avoid, that crunchy mess. You're saying I should pour quickly with swift stirring? I've heard adding sodium bicarbonate to the water is a good neutralizer, is that true? Also I've read that heating up the acetone beforehand gives finer crystals but I'm very hesitant to do that after The Yamato71 story. Even though he used methanol.
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[*] posted on 13-11-2022 at 16:33


I've always used ethanol; I've never gotten acetone to work properly. When I poured the acetone/ETN into cold water, no matter how strong the stirring, the acetone layer settled out. After a few minutes the ETN precipitated out as soggy chunks.



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[*] posted on 13-11-2022 at 19:00


Quote: Originally posted by Herr Haber  
Quote: Originally posted by ManyInterests  
Speaking of which, I did improve my ETN synthesis by recrystallizing it not in acetone, but in methanol. Methanol will give you a fine, powder-like result while acetone will make it crunchy and chunky. This might still trap some of the acid within it.


This can happen both with methanol and acetone.
There are reasons to favor acetone over methanol: less toxic, usually more available and if you compare solubility in methanol and acetone the latter is much much better. It's therefore easier to pour into a large volume of water with stirring and avoid creating two layers. With both solvents, in room temperature water you are going to get a crunchy crust and a mess if you pour slowly without stirring.
Urea scavenges NOx, it doesnt neutralize the acids but improves stability. You still have to use a base to do that.


I think a double recrystalization would not be out of the question then. One with acetone, the other with methanol. Methanol isn't dangerous as long as you don't get it on your skin (and if you do, wash it off right away) or drink it.

I did notice that it did get me the recrystalized product in a nice powdery form. For the acid I did not use a base. All I did was wash it again and again and again with water until no more acids were left over. When I recrystalized I also washed it excessively. I did not use any bases, but it still works.

Quote: Originally posted by BlackPowderBoy  
That's what I'm trying to avoid, that crunchy mess. You're saying I should pour quickly with swift stirring? I've heard adding sodium bicarbonate to the water is a good neutralizer, is that true? Also I've read that heating up the acetone beforehand gives finer crystals but I'm very hesitant to do that after The Yamato71 story. Even though he used methanol.


I never had a case where acetone gave me a powdery result. But then again, I only worked with small quantities of acetone and it was room temperature acetone. Maybe if I was working with hot acetone it would give me something else.

[Edited on 14-11-2022 by ManyInterests]
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[*] posted on 14-11-2022 at 18:54


No matter how well you wash the product if you dont neutralize the acids at some point in your process you are inviting trouble.
It can be done with crude and still wet ETN. The idea is that the water will be enough to dissolve NaHCO3 and that this minimum amount of water will not hinder too much your solvent.
Then you can also add NaHCO3 to the water you are going to use to crash the solvent / ETN mixture. Note that an excessive amount of base will affect crystal shape and the properties of the product will suffer.
Doing both is probably not necessary if you do one or the other properly.
I have no opinion on what would be the best stabilizer (such as urea) but Rosco Bodine pointed out on one occasion that what is a good stabilizer (diphenylamine in the case of NC) for a product might not be good in other cases.

Double recrystallization from different solvents is definitely the way to go. First one for purity and the second one to get the shape or density you are after.
If it works for the industry with a boatload of compounds you can probably make it work for you ;)




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[*] posted on 14-11-2022 at 22:03


I'm probably going to make another ETN batch in a few months. When I do that, I will add an additional step after washing my ETN like I normally do, but I will add the step of washing it with dilute sodium bicarbonate water after I do that step.

I will also recrystalize it along with my other batch twice (during it's second recrystalization) and in addition to having the urea scavanger, I will also wash everything again with bicarbonate water. So it'll be the 2nd recrystalization for the last batch and the third for the stuff I already have. If that doesn't remove all acids then I don't know what will.


Right now I am working with picric acid synth and recrystalization. I ran into my first real complication. I used too much water so I still have most of my picric acid in the filtered water (very little actually were caught in the filter paper) so I just added everything back to the water, and added more water, and now I am boiling it down.

I had a starting amount of 50 ASA and the amount of water I used to dump it into was over 1600ml! Too much. Even if it was nice cold, it would contain all the picric acid. so I am just doing the recrystalization in the original liquid. Once it down to almost nothing I will be re-recrystalizing it since there is still a lot of acid in this stuff. From the fizzing I see when I stir it.
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[*] posted on 2-12-2022 at 23:14


Ok so methanol is definitely the answer. The difference between acetone and methanol is NIGHT AND DAY. However as previously stated on this site, you must use MUCH more methanol in your recrystallization than if you were to use acetone. It took me around 350ml to dissolve 10-11 grams of ETN and even then I should've bought more as there was a small pile that remained undissolved in solution.

The methanol didn't settle out the second I crashed it into water like acetone does. The whole water solution becomes milky and stays that way. I also used room temp methanol. I know you're supposed to heat up the methanol beforehand so you can dissolve more ETN in solution. But personally I'm not going to invole heat and ETN until I want to detonate it. Maybe when I get better equipment and more cojones.

The end result is a very nice, fine powder. MUCH better than the crunchy acetone mess. The texture reminds me of powdered sugar and the appearance almost reminds me of "Artifical Snow." Or "Dry Snow."

[Edited on 3-12-2022 by BlackPowderBoy]
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[*] posted on 3-12-2022 at 00:08


Quote: Originally posted by BlackPowderBoy  
Ok so methanol is definitely the answer. The difference between acetone and methanol is NIGHT AND DAY. However as previously stated on this site, you must use MUCH more methanol in your recrystallization than if you were to use acetone. It took me around 350ml to dissolve 10-11 grams of ETN and even then I should've bought more as there was a small pile that remained undissolved in solution.

The methanol didn't seperate out when I crashed it into the water like acetone does. The whole water solution becomes milky and stays that way. I also used room temp methanol. I know you're supposed to heat up the methanol beforehand so you can dissolve more ETN in solution. But personally I'm not going to invole heat and ETN until I want to detonate it. Maybe when I get better equipment and more cojones.

The end result is a very nice, fine powder. MUCH better than the crunchy acetone mess. The texture reminds me of powdered sugar and the appearance almost reminds me of "Artifical Snow." Or "Dry Snow."

[Edited on 3-12-2022 by BlackPowderBoy]


Did you heat your methanol? I was able to fully dissolve around 90 grams or so (forgot exactly how much) of ETN in around 500ml or so of methanol. I need to look up my (open) lab notes that I posted in another thread.

I heated the methanol to boiling point before dumping into the ETN for recrystalization. I actually didn't intend to recrystalize that much ETN, I wanted to do 30 grams at a time, but I did everything at once. It was a happy little accident.
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[*] posted on 3-12-2022 at 00:18


Experience says that hot methanol is the best for recrystallization of ETN. But it is work with poison, or rather with its vapors.



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[*] posted on 3-12-2022 at 00:25


Quote: Originally posted by Laboratory of Liptakov  
Experience says that hot methanol is the best for recrystallization of ETN. But it is work with poison, or rather with its vapors.


Yeah, I am aware of how nasty and smelly it is. I do it near my balcony door where air is rushing in and thus properly ventilates my apartment. The fumes aren't too much which is why I can do it this way, otherwise I would need to do it on my balcony.
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[*] posted on 3-12-2022 at 00:43


No the methanol was room temp. I'll try heating up the methanol to boil next recryst, I'm just sketched out even if I took all the precautions...

After reading "Life After Detonation" I would almost rather spend more and use up more methanol just to avoid heating it to a boil and putting ETN into it.

Also Lip, Is hot methanol best for recryst because it takes less to dissolve more? Or does it do a better job at dissolving overall? Does it open up the crystals more efficiently so more acid can escape? Or is it just that you use less methanol when it's heated?

[Edited on 3-12-2022 by BlackPowderBoy]
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[*] posted on 3-12-2022 at 02:14


Experienced researchers say, from many experiences, that acetone is too strong a solvent for ETN. Over many years of recrystallizations, methanol proved to be an ideal solvent for several reasons at once. Better neutralization, cleaner product, finer resulting fraction - the consistency of a fine powder. I don't remember the exact ratios between hot methanol and raw ETN.



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