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Author: Subject: DIAMINOURONIUM (DI)NITRATE
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[*] posted on 10-8-2019 at 10:15


Well, twelty it does worth the efford. With 1Kg of DU, around 1.5kg of DUN can be produced. Have you ever considered how much money and effort is needed for the same amound of another equivalent energetic ? :D

[Edited on 10-8-2019 by underground]
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[*] posted on 10-8-2019 at 10:58


For me, cost is not a huge issue. I was more attracted by the ease of synthesis and safety. If I can't figure out how to crystallize, I may have to reconsider. I'm sure there is a way though.

I had one thought, that if I added a little sulfuric acid to grab the water, that might help. I tried it and indeed, just one or two drops caused a lot of white precipitate. Not sure if it is DAUN or something else though. Anyone have any thoughts?
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[*] posted on 10-8-2019 at 13:43


Why just don't you try out my way ? Try to remove as much water as possible with gentle boiling, don't bother to crystallize it out. The white solid it is indeed hygroscopic. I just left outside a small solid piece and in few hours became gooey.
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[*] posted on 10-8-2019 at 14:29


I'm now doing a large batch. I figured I'd make a large batch, and take out small portions to try different things on it. I tried adding EtOH and MeOH to a small amount if the natrated mixture, without removing any water first. No reaction.

Now I am gently heating and stirring with lots of air movement to get the water out with minimal heat (just in case it matters). I guess if I could get it to crystallize nicely using alcohol, like I did once before, that would be nice. If not I guess I'll just boil it down as you do. I'm just not sure what exactly that does. What is happening when you "boil it down" after the water is already gone? What is the difference between this white sticky/gooey substance (which does solidify into opaque white mass), and the crystallized stuff form the original paper? I did melt the crystallized stuff down and it remains more clear than the opaque white material, so it is clearly different. Maybe I'll try making one charge of each, equal weight and equal initiating charge and compare that way.

Have you done anything with yours??
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[*] posted on 10-8-2019 at 15:33


Not yet. I still have to try to detonate it. It is a bit strange but that white solid cant be anything else except DUN as long as only NA and DU used. Unfortunately there are not many information and properties about DUN.

[Edited on 10-8-2019 by underground]
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[*] posted on 10-8-2019 at 16:31


Quote: Originally posted by underground  
Not yet. I still have to try to detonate it. It is a bit strange but that white solid cant be anything else except DUN as long as only NA and DU used. Unfortunately there are not many information and properties about DUN.

[Edited on 10-8-2019 by underground]

Can it not be the di-nitrate instead of mono nitrate that we want?
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[*] posted on 10-8-2019 at 18:44


I believe it cant because of the DU ph and the amount on NA is used. It cant be a di-nitrate molecule and a freebase DU molecule together. The dinitrate would be too acidic for the freebase to both exist.

[Edited on 11-8-2019 by underground]
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[*] posted on 10-8-2019 at 19:09


Quote: Originally posted by underground  
I believe it cant because of the DU ph and the amount on NA is used. It cant be a di-nitrate molecule and a freebase DU molecule together. The dinitrate would be too acidic for the freebase to both exist.

[Edited on 11-8-2019 by underground]

I wish I could contribute, but I'm not educated in chemistry. I guess it is just a different form then? Different hydration level? or simply amorphous instead of crystals? That could still have an effect on its EM properties though. Has anyone ever tried to communicate with any of the professional chemists (like Fischer or Klapotke) on any of these questions?
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[*] posted on 11-8-2019 at 03:21


Anyone here with some 79% (w/w) or more concentrated HNO3? I did some calculations and I think the problem of under and/or over-dehydration of the reaction mixture could be solved, or at least confirmed correct or not.

A 79% HNO3 solution has a 1:1 molar ration of HNO3:water. If this is reacted in a 1:1 molar ratio with diaminourea you would expect the product to be the mono-nitrate mono-hydrate salt.

Reacting 79% HNO3 with diaminourea as is will probably give a runaway or decomposition, so a solvent for the base should be used. Ethanol is a good candidate as the product apparently is not soluble in it. Concentrated HNO3 and ethanol are known to react, but solutions of 9% (w/w) can be made when water is present.

This proposed procedure would never reach 9% though as long as all diaminourea is dissolved in ethanol and the HNO3 is added to this solution. The HNO3 will be neutralized during the reaction; just run it cold and slow.

Preperation of HNO3 in ethanol

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[*] posted on 11-8-2019 at 20:03


Quote: Originally posted by Tsjerk  
Anyone here with some 79% (w/w) or more concentrated HNO3? I did some calculations and I think the problem of under and/or over-dehydration of the reaction mixture could be solved, or at least confirmed correct or not.

A 79% HNO3 solution has a 1:1 molar ration of HNO3:water. If this is reacted in a 1:1 molar ratio with diaminourea you would expect the product to be the mono-nitrate mono-hydrate salt.

Reacting 79% HNO3 with diaminourea as is will probably give a runaway or decomposition, so a solvent for the base should be used. Ethanol is a good candidate as the product apparently is not soluble in it. Concentrated HNO3 and ethanol are known to react, but solutions of 9% (w/w) can be made when water is present.

This proposed procedure would never reach 9% though as long as all diaminourea is dissolved in ethanol and the HNO3 is added to this solution. The HNO3 will be neutralized during the reaction; just run it cold and slow.

Preperation of HNO3 in ethanol


Sounds interesting for sure. I don't have anything stronger than 70% and was hoping not to need any. I did try your other idea about dissolving the DAU in alcohol first. I found out it is not soluble, even though some references say it shuld be.

My last batch, made according to Fischer, starting with 9 grams of DAU, and slow-crystallized for several days, gave me this. The yield is the best so far, at around 75% of theoretical.



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[*] posted on 15-8-2019 at 20:50


Hi underground, I tried boiling down the DAUN mixture, like I guess you are doing. I very gently heated it, with a lot of air movement over it to help it evaporate. It reduces to a think oil, but then? I tried adding methanol and it slowly "curdles" (like milk and vinegar) out as white amorphous opaque white material. Is this what you are doing?
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[*] posted on 16-8-2019 at 02:47


Yea that is what i got. I then evaporate it again, like you did and put it into deep freeze. It will solidify like mine. Put it somewhere so you can remove it after easily, like inside a bowl covered with a greaseproof paper. Do not put it into a beaker cause you would have to break it like i did.

[Edited on 16-8-2019 by underground]
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[*] posted on 16-8-2019 at 07:33


I did this once before, by accident. That time I left it to evap long enough that it was a thick white goo when I came back. I added a little water and it seemed to dissolve. Again, addi g a little methanol forced it solid. But that way I ended up with a powder. I did press some into a tube and I believe I detonated it. I need to do a larger charge to be certain though.
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[*] posted on 16-8-2019 at 08:52


A bit strange that you ended up with a powder. You could see what i got after evaporation from photoes.

P.S. I did not redisolve it, evaporate water, deep freeze, add alcohol, evaporate, deep freeze.
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[*] posted on 16-8-2019 at 12:08


Quote: Originally posted by underground  
A bit strange that you ended up with a powder. You could see what i got after evaporation from photoes.

P.S. I did not redisolve it, evaporate water, deep freeze, add alcohol, evaporate, deep freeze.


Try dissolving some in water, and then add methanol. it was a bit strange though, because even if i just "dissolved" the white solid in water, and let it stand for a bit, it seems to settle out even without even adding the methanol. The methanol just seemed to speed up the process. Not sure what is going on.
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[*] posted on 25-8-2019 at 11:19


UPDATE: I have now figured out how to crystalize this stuff out, nice pristine and largish crystals. I have figured out how to get it into a nice crystaline flowable powder form. I have cast it. I have done quite a few things except manage to detonate any (unequivocally). Just tried 5 g of cast DAUN, with 1.2 g hand pressed PETN, in a 10 mm tube. I found the cast part in the bucket, so no det that time. I tried once already, using the powder form, pressed in a tube, didn't seem to work either. I've tried a few different things, but no joy yet. I wonder how I could sensitize it a little. MM, you mentioned adding aluminum for more energy. Would that sensitize it as well? Can anyone calculate the critical diameter?
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[*] posted on 25-8-2019 at 13:27


Hmmm maybe a mixture of DUN and ETN or even HMTD/TATP would surely sensitize it.
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[*] posted on 25-8-2019 at 14:21


Quote: Originally posted by underground  
Hmmm maybe a mixture of DUN and ETN or even HMTD/TATP would surely sensitize it.

ETN maybe. or I could try pressing the powder form. I tried once but maybe with booster. Aluminum? microballons?

What about you, have you had any luck?
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[*] posted on 25-8-2019 at 14:45


I have not yet do anything but i will
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[*] posted on 26-8-2019 at 07:25


Does it burn with a flame?

Could try mixing with 15 percent Al. If it does not burn with a flame something might be wrong.

Another option would be to cast 5g and send a small shape charge jet through the center.
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[*] posted on 26-8-2019 at 07:34


Quote: Originally posted by MineMan  
Does it burn with a flame?

Could try mixing with 15 percent Al. If it does not burn with a flame something might be wrong.

Another option would be to cast 5g and send a small shape charge jet through the center.

Mine burns, though not super fast. I have some Al, will try.
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[*] posted on 1-9-2019 at 17:42
Success!


Finally got a good det. 2.5 g DAUN powder pressed in a CF tube, 0.6 g hand pressed ETN, 80mg dextrinated Ni Aminoguanidine perchlorate. I have been doing quite a few tests using the same steel plates (conduit box covers), so I know what 0.6 g ETN should do. Instead I got:


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[*] posted on 1-9-2019 at 20:39


:D:):D:D

Excellent.

Do you think it is worth the trouble?
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[*] posted on 1-9-2019 at 22:31


Quote: Originally posted by MineMan  
:D:):D:D

Excellent.

Do you think it is worth the trouble?


Not really any trouble once you know how. Gotta try detonating the cast version now.
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[*] posted on 2-9-2019 at 09:41


Wow amazing news. Well done!! Will you try the white thing, like what i got?

Also compared to 2.5g ETN or PETN the damage to the plate is similar ? Do you have another plate with lest say 2.5g ETN or PETN ?

[Edited on 2-9-2019 by underground]
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