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underground
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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 ? 
[Edited on 10-8-2019 by underground]
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twelti
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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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underground
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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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twelti
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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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underground
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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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twelti
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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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underground
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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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twelti
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| 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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Tsjerk
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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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twelti
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| 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
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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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twelti
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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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underground
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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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twelti
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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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underground
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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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twelti
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| 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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twelti
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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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underground
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Hmmm maybe a mixture of DUN and ETN or even HMTD/TATP would surely sensitize it.
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twelti
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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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underground
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I have not yet do anything but i will
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MineMan
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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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twelti
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| 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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twelti
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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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MineMan
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Excellent.
Do you think it is worth the trouble?
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twelti
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Not really any trouble once you know how. Gotta try detonating the cast version now.
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underground
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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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