Sciencemadness Discussion Board

ETN Synthesis - Not decanting

erick.wells - 4-12-2021 at 11:44

Hello everyone, everything good ?
This is my first post, I did some research here on the forum and I didn't find anything like the problem I'm facing.

I have no experience with chemistry, but I've managed to synthesize some things like Nitroglycerin, Nitrocellulose, HTMD.
I really like energetic materials and I'm trying to learn as much as possible.

I'm trying to synthesize ETN, using the following recipe I found on the internet using the bitchute video that I don't remember the link now.

erythritol
98% sulfuric acid
70% nitric acid
Bicarbonate and distilled water for washing.

I'm doing everything in a magnetic stirrer, I'm dissolving the erythriol in sulfuric acid refrigerated 5ºC keeping the temperature below 10ºC, after dissolving and turning a kind of paste I'm adding it in nitric acid also refrigerated and keeping it below 20ºC in a water/ice bath .

After adding the content of erythriol dissolved in sulfuric acid, the erythriol slurry with acid dissolves and becomes a more or less thick liquid.

The problem is that when I put the mixture in ice water it doesn't form crystals or something like that, it stays a clear solution and doesn't decant the erythriol.

Can anybody help me ? If you need to add more details like the measurements, I don't have them easily here.

I apologize for any errors here in this post, as my first post I still don't know how to do it correctly.

B(a)P - 4-12-2021 at 12:19

It is not going to be easy to help if you can't provide the concentration of your acids or the weight of the reagents that you used.
There is also a huge amount of really good information on this forum about ETN that you should make your way through if you are interested in learning more.
The synthesis of an energetic compound based entirely on a video is not a great idea of it isn't backed up with a lot of research, particularly if you don't have a lot of experience.

Edit - Your issue is one of formation not the ability to decant something so changing the title might get your more assistance as well.

[Edited on 4-12-2021 by B(a)P]

erick.wells - 4-12-2021 at 12:31

Quote: Originally posted by B(a)P  
It is not going to be easy to help if you can't provide the concentration of your acids or the weight of the reagents that you used.
There is also a huge amount of really good information on this forum about ETN that you should make your way through if you are interested in learning more.
The synthesis of an energetic compound based entirely on a video is not a great idea of it isn't backed up with a lot of research, particularly if you don't have a lot of experience.


I tried two times the process, here de concentrations:

1-Process:

Nitric Acid 70% -> 12ml
Sulfuric Acid 98% -> 18ml
Erythritol -> 3g

2 - Process:

Nitric Acid 70% -> 75ml
Sulfuric Acid 98% -> 93ml
erythritol -> 13g
Carbonated Water -> 150ml


This help ?

fredsci93 - 4-12-2021 at 15:23

Could you elaborate on the process a little more, specifically, how long was the erythritol reacted for, because if you simply reacted until the solution was a slurry nearly no ETN will be made, instead soluble lower nitrates will be produced (erythritol trinitrate, erythritol dinitrate and erythritol mononitrate) which is what I suspect may have happened.

try adding the erythritol to an iced mixed acid solution (Nitric and sulphuric) and mixing it every 10mins or so over 90 minutes, then you need to raise the temp to ~10-15C for 15 minutes to fully react away any impurities before quenching into ice water, should work although I have only personally performed this procedure on a sulphuric/ammonium nitrate nitrating mix.

ManyInterests - 5-12-2021 at 07:48

Quote:
I'm trying to synthesize ETN, using the following recipe I found on the internet using the bitchute video that I don't remember the link now.


Quote:
I'm doing everything in a magnetic stirrer, I'm dissolving the erythriol in sulfuric acid refrigerated 5ºC keeping the temperature below 10ºC, after dissolving and turning a kind of paste I'm adding it in nitric acid also refrigerated and keeping it below 20ºC in a water/ice bath .


Did you watch Darian Ballard's video? Here is the link that I used to synthesize ETN.

https://www.bitchute.com/video/78uQsxtKK3rE/

I used his method to great effect, but I had done my own modifications to it.

But I think I can see what's going wrong here. You're dissolving the erythritol in pure sulfuric acid. You need to add it to the nitrating mixture, not pure sulfuric acid. That will destroy your erythritol for sure.

Firstly, I kept the temperature much lower than 10 C. It never went above 4 C (because it's winter and I kept it outside) and I would avoid using carbonated water, as I noticed that when you add any carbonate or bicarbonate to the ETN it can form into a foam that will not go away, not matter how many times you wash it out with water.

My step by step process with the following proportions:
Quote:
1-Process:

Nitric Acid 70% -> 12ml
Sulfuric Acid 98% -> 18ml
Erythritol -> 3g


The most I did was 3 times this amount, 9.9 grams of erythritol, 42ml of 65% nitric acid (it got diluted, but it didn't affect the yield that much) and 55ml of sulfuric acid (around 95 or 96%).

1: Made the nitrating mixture and stirred it well, after which I covered the beaker with plastic wrap and put it in the freezer to cool down as much as possible. While in the freezer I also made a saltwater ice bath and placed the beaker in it and let it cool for several hours until the ice began to freeze.

2: I ground up 9.9 grams of granulate erythritol in a coffee grinder to powderize it and kept it aside. ALWAYS use granulated erythritol and always grind it. It will result in an end product in a powdered state instead of larger crystals. Purer and more stable.

3: After the saltwater bath has frozen (this will take hours and a cold freezer) the mixing can start. Do this outside or in a fumehood as there will be fumes. I did it outside with a fan running to suck away the fumes.

4: In very small portions (around 0.5 to 1 gram at a time) add the powdered erythritol to the mixture and stir for about a minute or two every time. What I did was use my thermometer along with a glass stir rod and periodically check the temperature. In my case it never went above zero as the mixture was ice cold

5: After all the erythritol is added continue to mix until everything is dissolved. I scraped the sides of my beaker to get any chunks in and kept stirring for another 10 minutes. The end mixture will be a milky white, thick liquid.

6: After this. I covered the nitrating mixture and kept it outside and as cold as possible. I know this is less than completely ideal, but I believe it does lower the risk of a runaway, and since it is outside, if a runaway does happen, the fumes won't harm you and you can wait until it cools down on its own before retrieving the beaker.

7: Darian said to wait 30 minutes to let it nitrate. He did this at a temperature of 10c. I let it nitrate for around 3.5 hours as the temperature never went above 4C.

8: While I was poured around 900 ml of distilled water and let it cool in the fridge. I don't know how much water you will need initially. for my proportion I would have used more than 1 liter, but I don't have any containers that hold that much. You should use glass jars when doing this, as I noticed that plastic loves to carry the stains and I think they become unusable after a bit for anything else. The plastic becomes much more opaque as well.

9: Once the nitration is complete, take the beaker and pour the contents into the water. Use more distilled water to remove what is stuck in the beaker. Give the contents of the container you poured them into a good stir for a bit.

10: The ETN is 100% insoluble in water, just as a reminder. Filter off the contents of the first jar into anther container. A simple funnel with coffee filters will work just fine. Once the coffee filter starts to get clogged with ETN (if you have that much) replace it with another filter and set the first to dry (but give the ETN in the filter several washes of distilled water to pull out as much of the acid as possible). While doing this, peroidically refilled the original jar with distilled water. This will help dilute acid in it.

If and when the jar you are using for filtering gets full, check to see if you have any errant bits of ETN in there. They can be neutralized with sodium hydroxide (lye). The water will still be acidic, so you would also want to want to neutralize with a carbonate or bicarbonate before pouring it down the drain.

Once you have filtered off all the ETN set the filters out to dry. I try to get them to dry faster by putting paper towels over and under them (with plastic cling film at the bottom) to draw out as much of the water as possible.

Once it is fully dry. Weigh the yield. The yield I received from the following method above was 16 grams of ETN. But I did use carbonate water that resulted in some fluff forming. I was certain the yield was too high and some contamination was there, as a small sample of the stuff refused to burn at all when I tried to test it on aluminum foil with a flame beneath it.

Recrystalization is simple. Put the ETN in a glass container and, dropwise, add acetone until all the ETN is in solution and the impurities are not. I added a slight excess of acetone until the solution was colorless, but be very careful when adding the acetone as ETN is VERY soluble in acetone.

After this, I got my 1 liter beaker, filled it with distilled water and got some strong stirring going on before dumping the ETN/acetone solution into it. Strong stirring is necessary as the ETN in this case will like to stick to the bottom. Stirring helps prevent that.

Once the ETN/acetone is added you should immediately see the ETN crystals forming. It will have a solid, chunky, crunchy consistency. You can then filter this off as previously into another container with a funnel and coffee filter. It should be easier to it this time around.

After this, let the recrystalized ETN dry. They will still be chunky and crunchy. But you can grind them up. Just be gentle with them and do them in small pieces at a time just to be safe. Once it is a powder again and dry, the ETN is ready for use.

My final yield after that was 13 grams. Not bad. I used up a lot of water and it was time consuming, but the result is very pure ETN to make all the blasting caps I could ever want!

[Edited on 5-12-2021 by ManyInterests]

[Edited on 6-12-2021 by ManyInterests]

Raid - 30-3-2023 at 05:44

If you or anyone is still wondering about this, I'm guessing that it's because the product is not getting properly nitrated. I have had this same problem but when I used KNO3 In place of HNO3. If anyone is still having this issue I would recommend nitrating it for longer, maybe leaving it overnight.
If DB's method is not working then I would try the stoichiometric equivalents for each of the chemicals, that might help.

karolus28 - 30-3-2023 at 06:53

Quote: Originally posted by ManyInterests  

But I think I can see what's going wrong here. You're dissolving the erythritol in pure sulfuric acid. You need to add it to the nitrating mixture, not pure sulfuric acid. That will destroy your erythritol for sure.


taking a part of sulfuric acid that would be put into a nitration mix and dissolving erythrytol into it below 30*C gives a colourless goo, which poured into a nitration mix works just fine, it's actually better because the temperature rises only barely, as the E doesnt have to be dehydrated anymore by the H2SO4.(gives off additional heat that would combine with the heat of the nitration reaction thus giving sharp temp spikes)

Also, after adding the E, you make sure it heats up to 18-20*C, as the reaction doesnt really progress if cold.

Energetics-testin - 30-3-2023 at 13:22

Quote: Originally posted by karolus28  


Also, after adding the E, you make sure it heats up to 18-20*C, as the reaction doesnt really progress if cold.


Yes absolutely,the temperature when letting it "chill" is almost as important as keeping it cool during the addition of erythriol to the nitration mixture .

Also thank you very much karolus28,For P-DDNP via DNAc we basically do that and there is pretty much no temperature spikes..

I wasnt really sure if the Erythriol would have been able to handle the 98% H2SO4

[Edited on 30-3-2023 by Energetics-testin]

karolus28 - 31-3-2023 at 05:44

https://www.sciencemadness.org/whisper/viewthread.php?tid=15...

i just quoted some info from wesson smith