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Tsjerk
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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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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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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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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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twelti
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| 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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underground
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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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Anyone have any updates? I know magnesium sulfate readily crashes the DAUN.
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twelti
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Where did you see that? i am out of town so no further work yet.
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twelti
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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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MineMan
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That’s the dinitrate. We have been after the monk nitrate.
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twelti
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It sounds very similar to what they say about the mononitrate though.
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MineMan
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Oh. For crystallizing. Yes.
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twelti
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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.
[Edited on 28-7-2019 by twelti]
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underground
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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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twelti
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| 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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James Ikanov
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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....
“To do good work one must eat well, be well housed, have one's fling from time to time, smoke one's pipe, and drink one's coffee in peace” -
Vincent Van Gogh
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twelti
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| 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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twelti
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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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underground
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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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twelti
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| 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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underground
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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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twelti
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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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MineMan
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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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underground
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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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twelti
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| 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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