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Author: Subject: DIAMINOURONIUM (DI)NITRATE
Tsjerk
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[*] posted on 9-7-2019 at 14:34


It could be the one molecule of water is actually needed to crystallize the mono-nitrate monohydrate. Or is only the the di-nitrate crystallizing as the mono-hydrate?
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twelti
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[*] posted on 9-7-2019 at 15:31


Quote: Originally posted by underground  
I also did evaporate carefully as much water as i could (atmospheric pressure). It was like honey at room temp. I transfer it into deep freeze and i got few crystals. I checked it again after a while and more crystals came out. I will leave it all day there and check it after. Evaporating the water as much as possible and transfer it into deep freeze looks to be the way to go.


[Edited on 9-7-2019 by underground]

Did you add the methanol? It would be interesting to try some other (anti?) solvents.
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underground
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[*] posted on 9-7-2019 at 16:25


Only the dinitrate salt form a monohydrate.

I did not add any solvent. Most of ethanol was evaporated. After that i did not add any another.

[Edited on 10-7-2019 by underground]
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underground
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[*] posted on 10-7-2019 at 04:02


Today i checked it out and everything was solid like a rock. I had to broke my beaker to take it out. Next time i will use a blastic bottle. It is quite hygroscopic, the surface became wet in about 2 minutes.





[Edited on 10-7-2019 by underground]
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[*] posted on 10-7-2019 at 09:12


Quote: Originally posted by underground  
Today i checked it out and everything was solid like a rock. I had to broke my beaker to take it out. Next time i will use a blastic bottle. It is quite hygroscopic, the surface became wet in about 2 minutes.





[Edited on 10-7-2019 by underground]

WOW! That looks about as much different from mine as it could possibly be. For mine, it has now mostly dried out, and there doesn't seem to be much material there, considering i started with a gram. What I do have is crystalline. I'm going to make a bigger batch and split it up into smaller containers and try different things. In the paper it mentions as the first option Crystallizing with ethanol/water, sitting for a long time at RT I think.
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[*] posted on 11-7-2019 at 05:11


I just melt it again and filter with a screen to remove any glass and transfer it into a greaseproof paper. I seal it airtide and put it into -20 C.


https://i.ibb.co/fH878ZC/20190711-155346.jpg

The good things is that it can easily casted. Aslo during casting, most of water evaporates. The bad thing is that it is very hygroscopic. There is no way to keep it as a dry powder. It can be casted though into some small airtide containers, like 5g, and use it accordingly. The next step is actually to see how easily it goes ddt, but it will take a bit to test it myself.

[Edited on 11-7-2019 by underground]
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MineMan
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[*] posted on 16-7-2019 at 20:49


Anyone have any updates? I know magnesium sulfate readily crashes the DAUN.
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[*] posted on 18-7-2019 at 05:49


Quote: Originally posted by MineMan  
Anyone have any updates? I know magnesium sulfate readily crashes the DAUN.

Where did you see that? i am out of town so no further work yet.
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[*] posted on 23-7-2019 at 15:50


Can someone help us understand what this means:

"The water is removed in vacuo and the product is isolated as a colorless solid after addition of methanol to the evaporated residue. The compound crystallizes as a monohydrate although showing an oxygen balance of 10.3 %. However, the water can be removed at 75 °C using vacuo. DAU_2NO3 is completely insensitive towards impact and friction but, unfortunately, decomposing already at 115 °C. Latter property retards probably all possible applications. "

What does adding the methanol accomplish? If we remove the water first, how can it crystalize as a monohydrate? Or is it just confusingly written? Or am I just an idiot? Don't answer that!
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[*] posted on 23-7-2019 at 19:09


That’s the dinitrate. We have been after the monk nitrate.
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[*] posted on 23-7-2019 at 23:14


Quote: Originally posted by MineMan  
That’s the dinitrate. We have been after the monk nitrate.

It sounds very similar to what they say about the mononitrate though.
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[*] posted on 24-7-2019 at 05:00


Quote: Originally posted by twelti  
Quote: Originally posted by MineMan  
That’s the dinitrate. We have been after the monk nitrate.

It sounds very similar to what they say about the mononitrate though.


Oh. For crystallizing. Yes.
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[*] posted on 28-7-2019 at 09:14
Is it Christmas?


Back from business trip, doing some experiments on DAUN. I have noticed some things.
1. DAUN seems to not not dissolve in water once crystalized. I have my first small batch is floating in water for days now, still crystalized.
2. Crashing newly prepared DAUN ( no water removed) into saturated magnesium sulfate water solution had no effect.
3. I noticed before that DAUN did not dissolve in EtOH, so I tried adding that to the freshly prepared DAUN (no water removed). I got immediate milky crash, which then dissipated and went clear again. Overnight however, I got this. Now I put it in the freezer to see if any more crystals come out.

Seems promising.




20190728_083333.jpg - 3.7MB

[Edited on 28-7-2019 by twelti]
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[*] posted on 28-7-2019 at 09:41


I also got a milky thing after adding ethanol. Indeed it does not dissolve easily in water once it ppt out. I removed as much water as i could and then deep freeze. It solidified immediately. As i said above, it is quite hygroscopic, it become wet if you left it outside in for few minutes. When i got some time i will try to detonate few grams.

Edit: I used 1:1 molar ratio so i got mostly DU nitrate

[Edited on 28-7-2019 by underground]
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[*] posted on 28-7-2019 at 21:50


Quote: Originally posted by underground  
I also got a milky thing after adding ethanol. Indeed it does not dissolve easily in water once it ppt out. I removed as much water as i could and then deep freeze. It solidified immediately. As i said above, it is quite hygroscopic, it become wet if you left it outside in for few minutes. When i got some time i will try to detonate few grams.

Edit: I used 1:1 molar ratio so i got mostly DU nitrate

[Edited on 28-7-2019 by underground]

Strange behavior too: It went from clear to milky when I did the initial crash, then eventually back to clear. THEN when I simply poured from one container to a larger one, it went milky again. Weird.
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[*] posted on 29-7-2019 at 14:43


This is just some speculation on my part, but in the one attempt of synthesizing nitroxylitol I made, I learned that the reason it is probably so obnoxiously liquid is that the different stages of nitration are soluble in each other. Could there be a similar behavior here? Perhaps when poured, the physical agitation separates it a bit? The only other thing I can think of is that there is some kind of shift in the "crystal" structure when agitated, and I don't know which would be more likely. I would think that the required temperature change in the presence of methanol lends itself more to the second one, but both seem plausible and maybe not even mutually exclusive....



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[*] posted on 29-7-2019 at 18:06


Quote: Originally posted by James Ikanov  
This is just some speculation on my part, but in the one attempt of synthesizing nitroxylitol I made, I learned that the reason it is probably so obnoxiously liquid is that the different stages of nitration are soluble in each other. Could there be a similar behavior here? Perhaps when poured, the physical agitation separates it a bit? The only other thing I can think of is that there is some kind of shift in the "crystal" structure when agitated, and I don't know which would be more likely. I would think that the required temperature change in the presence of methanol lends itself more to the second one, but both seem plausible and maybe not even mutually exclusive....

It is an equilibrium reaction, so entirely plausible I guess. Makes me also wonder about the method used by Underground. He did the same reaction (1 equivalent of precursor and of acid) but with undiluted acid (65%) so less water. I wonder if that affects the equilibrium process, since his results were somewhat different than mine. I stuck to the exact reaction in the Fischer paper.

For me, I feel like if I added enough EtOH, it would all crystalize out, but it would take a large volume. Not sure though.
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[*] posted on 30-7-2019 at 23:04
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I made a larger batch, using the 2M nitric acid as per Fischer. Using 9 g of the DAU. Diluting the product with a lot of Ethanol, I got around maybe 3 gram to crystalize fairly quickly. I have tried a few experiments with the remaining liquid, which must have a lot of DAUN still in it. I tried various diluants to see if any caused crystallization. The last thing I just tried was I took around 25 ml of the remaining liquid and added 2 drops of sulfuric acid (conc.). I though maybe it would suck up the water and force crystalization. Well, a whole lot of white solid did crystalize out. I've no idea what it might be. DAUN? or something else.
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[*] posted on 31-7-2019 at 07:37


You may have dehydrated your DUN, maybe aminonitrourea is produced. I just use 65% NA cause i really dont want to boil all tha water out. Try to carefully boil out all the water to the point you may decompose few of the salt. Put it into a deep freeze and i am sure you will get what i got. What is happening is that you mostly got molten DUN and by freezing it, it become solid. The is no need for crystalization as long as you use pure nitric acid, just evaporate all the water out.

[Edited on 31-7-2019 by underground]
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[*] posted on 31-7-2019 at 10:01


Quote: Originally posted by underground  
You may have dehydrated your DUN, maybe aminonitrourea is produced. I just use 65% NA cause i really dont want to boil all tha water out. Try to carefully boil out all the water to the point you may decompose few of the salt. Put it into a deep freeze and i am sure you will get what i got. What is happening is that you mostly got molten DUN and by freezing it, it become solid. The is no need for crystalization as long as you use pure nitric acid, just evaporate all the water out.

[Edited on 31-7-2019 by underground]

But then why did they use dilute NA in the Fischer paper? You said it generated a lot of heat.
Have you done any testing on your product? you also got a single solid chunk, did you not? Are you sure it is working correctly?
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[*] posted on 31-7-2019 at 11:44


It looks good το me, i have not tried yet to detonate. The melting point is correct. I also got some crystals at the walls of the beaker like umbrella, the rest at the bottom was like the photos above. By melting and rapid cooling it, crystals become really small, that is why you cant actually see any crystals at all.

[Edited on 31-7-2019 by underground]
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[*] posted on 31-7-2019 at 19:25


BTW, I weighed the product I already got, using the standard procedure and crashing with EtOH (with some dying first but still some water in it). I was surprised that I actually had around 9 g of DAUN. Starting form 9 g of DAU, that's not as bad as I thought. I want to try your method with 70% NA, but now that I think of it, that is physically not a lot of liquid for the given amount of solid precursor. to try to mix.
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[*] posted on 31-7-2019 at 23:15


This is exciting!

Sorry for my recent silence on this thread and DMs. I feel at this time I am unable to contribute.
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[*] posted on 31-7-2019 at 23:22


Cool the NA and then add it to the DAU. You can even add some ice. This is what i did. I dont see any reason why 65% NA will not work and 2% will work. 65% still got plenty of water to do any nitration.
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[*] posted on 1-8-2019 at 08:50


Quote: Originally posted by underground  
Cool the NA and then add it to the DAU. You can even add some ice. This is what i did. I dont see any reason why 65% NA will not work and 2% will work. 65% still got plenty of water to do any nitration.

Sounds good. Have you tried to cast it yet?
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