| Pages:
1
2
3
4
5
..
8 |
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
You can use either 5 ml 10 mmole 2M NA and 10mmole DU or 2 M, 11.1 mL, 22.2 mmol and 22.2mmol DU for the mononitrate salt. It is the same. Molar ratio
is what it matters.
[Edited on 5-7-2019 by underground]
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
I just got some carbozydrazide and react it with some 65% Nitric acid . 97 grams of 65% NA (1 mole) was reacted with 90,1g of DU (1 mole). The
reaction produces quite a bit of heat so i put the NA into an ice bath and add DU. Everything was dissolved really quick leaving an oil like
substance. Trying to boil off the water does not work as it looks like it decomposes before even it crystallize out. The more water is removed the
more like syrup became. It is a bit tricky to crystallize it out. I will try to put some into -20C and bring it back to room temp few times. Also i
will put some into a desiccator bag to see if it will dry out.
[Edited on 7-7-2019 by underground]
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
I mixed some up using the 2M acid. Not much, if any, heat. Put it in a dessicator for a couple of days, then vacuum for half an hour. I added
approx equal volume of Methanol to it. Then into the freezer overnight. So far no luck getting it to crystalize though. Tried dropping a couple of
crystals of PETN in to seed it. Nothing yet...
[Edited on 7-7-2019 by twelti]
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
I removed as much water as i could with just gentle boiling. It become very thick. I added some ethanol, it actually was not dissolving a lot,
remaining mostly on top. After adding methanol from clear solution become white. Put it into the deep freeze and became like honey consistency, like a
white honey. From pdf that i have read it claims to remain at that low temp for couple of days. I will keep it freeze for about 4-5 days and i will
bring it back to room temp and scrach the flask to see if i got anything.
[Edited on 7-7-2019 by underground]
|
|
|
MineMan
International Hazard
Posts: 1004
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
It’s like being a little kid and waiting for your parents to get up in the morning on Christmas Day.
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
What did YOU get for Christmas? Some very insensitive, cheap an powerful secondary explosive? Ok, go play with the other kids!
Seriously:
I'm wondering if using a larger amount would help it start to crystalize. Are there any other nifty chemistry tricks? Ultrasound? Microwave?
I read in one place to scratch with glass rod at the liquid/air interface (i.e. not at the bottom of the container like I was). Also another trick,
dip in the glass rod and remove, allowing liquid on it to evaporate or at least crystalized, then put it back in the liquid. Finally, what about
colder temps. Salt/ice bath or even dry ice/alcohol?
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
Quote: Originally posted by underground  | I removed as much water as i could with just gentle boiling. It become very thick. I added some ethanol, it actually was not dissolving a lot,
remaining mostly on top. After adding methanol from clear solution become white. Put it into the deep freeze and became like honey consistency, like a
white honey. From pdf that i have read it claims to remain at that low temp for couple of days. I will keep it freeze for about 4-5 days and i will
bring it back to room temp and scrach the flask to see if i got anything.
[Edited on 7-7-2019 by underground] |
Did you get an emulsion then?
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
Yea it is still an emulsion. The stuff will not crytalize if you made the trick with the glass rod. I have made 2 bunches of 1 mole each. I got almost
2 moles of DUN, it is a bit big scale. For now i will just try to do whatever pdf say. In general they claim to keep it at -20C for several days as i
said above. It is just few hours till now.
[Edited on 7-7-2019 by underground]
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
| Quote: Originally posted by underground | Yea it is still an emulsion. The stuff will not crytalize if you made the trick with the glass rod. I have made 2 bunches of 1 mole each. I got almost
2 moles of DUN, it is a bit big scale. For now i will just try to do whatever pdf say. In general they claim to keep it at -20C for several days as i
said above. It is just few hours till now.
[Edited on 7-7-2019 by underground] |
Yeah it is strange that they say to let it go up to RT, then scratch. I would have thought it would crystallize at lower temp first.
I just put in a larger amount of PETN crystals in there as seed. Still only a fraction of a mg though.
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
Is there any way the uncrystalized oil could be used, as a straight liquid explosive?
|
|
|
Tsjerk
International Hazard
Posts: 3032
Registered: 20-4-2005
Location: Netherlands
Member Is Offline
Mood: Mood
|
|
Maybe it is an idea to take a known weight small sample, say a couple of grams, smear that out in order to form a big surface area and put that in a
desiccator to see if there is still water in your sample. Maybe a last little bit of water is making things hard for you guys.
As long as your container and your detonator are watertight you can probably set it of while it being a liquid, why not?
[Edited on 8-7-2019 by Tsjerk]
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
| Quote: Originally posted by Tsjerk |
As long as your container and your detonator are watertight you can probably set it of while it being a liquid, why not?
[Edited on 8-7-2019 by Tsjerk] |
I was thinking the same in worst case scenario, but it may be quite hard to ddt and the extra water may drop the performance. We have to try a
desiccator bag too and maybe with some strong drying agents like concentrated H2SO4.
[Edited on 8-7-2019 by underground]
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
| Quote: Originally posted by underground | | Quote: Originally posted by Tsjerk |
As long as your container and your detonator are watertight you can probably set it of while it being a liquid, why not?
[Edited on 8-7-2019 by Tsjerk] |
I was thinking the same in worst case scenario, but it may be quite hard to ddt and the extra water may drop the performance. We have to try a
desiccator bag too and maybe with some strong drying agents like concentrated H2SO4.
[Edited on 8-7-2019 by underground] |
I tried with silica gel. So H2SO4 is better? What about P2O5?
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
I dunno about P2O5. Try cacl/NaOH/H2SO4. You can put them all together separately into the same bag. Although h2so4 is the strongest.
Edit: After searching a bit i found that P2O5 is very strong desiccant agent, possibly even more than concentrated H2SO4. You can give it a try.
[Edited on 8-7-2019 by underground]
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
So, I attempted to dry it some more, using gentle heat and then vacuum. I got it down to a fairly small amount of liquid. I think it was nearly
water free. I added more methanol and put it back in the freezer for a day. Today there was something there. I thought maybe ice, and in fact some
did melt, although reluctantly. Still 2 hours after I took it out, it has been at RT for a while now and Ive still got about half of the mass
unmelted. May be a mix of DAUDN and water? Strange also since the first time I had it in the freezer for a day and a half and got NO crystals or
ice. If anything there should be less water in it now, yet I'm getting this:
 
most of that has melted but there is still some that is definitely a solid, at RT for 3 hours now.
[Edited on 9-7-2019 by twelti]
|
|
|
Microtek
National Hazard
Posts: 869
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
Do you know what the solubility of DAUDN is in this solvent system? The "melting" that you see may actually be the product dissolving as the
temperature rises and the solubility therefore increases.
About the dessicants: P2O5 is certainly a stronger dessicant than concentrated sulfuric acid. In fact also stronger than SO3, since P2O5 can dehydrate
sulfuric acid to form SO3 and phosphoric acids of diferent kinds.
|
|
|
MineMan
International Hazard
Posts: 1004
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
Good job twelti! You made history! Now do a witness plate test
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
Good job twelti. Step by step we getting closer to our goal.
|
|
|
wessonsmith
Hazard to Others
Posts: 203
Registered: 15-2-2018
Location: elsewhere
Member Is Offline
|
|
| Quote: Originally posted by twelti | So, I attempted to dry it some more, using gentle heat and then vacuum. I got it down to a fairly small amount of liquid. I think it was nearly
water free. I added more methanol and put it back in the freezer for a day. Today there was something there. I thought maybe ice, and in fact some
did melt, although reluctantly. Still 2 hours after I took it out, it has been at RT for a while now and Ive still got about half of the mass
unmelted. May be a mix of DAUDN and water? Strange also since the first time I had it in the freezer for a day and a half and got NO crystals or
ice. If anything there should be less water in it now, yet I'm getting this:
most of that has melted but there is still some that is definitely a solid, at RT for 3 hours now.
[Edited on 9-7-2019 by twelti] |
Not sure if this helps:
16.DIAMINOURONIUM DINITRATE
We recently investigated diaminouronium nitrate, which is a new secondary explosive. With
regard to development of new high-oxidizers the double-protonated compound
diaminouronium dinitrate (DAU_2NO3) was synthesized starting from cheap available
diaminourea, which is protonated with two equivalents of dilute nitric acid according to
Synthesis of diaminouronium dinitrate monohydrate.
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.
p44 https://www.serdp-estcp.org/content/download/10799/136954/fi...
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
| Quote: Originally posted by wessonsmith | | Quote: Originally posted by twelti | So, I attempted to dry it some more, using gentle heat and then vacuum. I got it down to a fairly small amount of liquid. I think it was nearly
water free. I added more methanol and put it back in the freezer for a day. Today there was something there. I thought maybe ice, and in fact some
did melt, although reluctantly. Still 2 hours after I took it out, it has been at RT for a while now and Ive still got about half of the mass
unmelted. May be a mix of DAUDN and water? Strange also since the first time I had it in the freezer for a day and a half and got NO crystals or
ice. If anything there should be less water in it now, yet I'm getting this:
most of that has melted but there is still some that is definitely a solid, at RT for 3 hours now.
[Edited on 9-7-2019 by twelti] |
Not sure if this helps:
16.DIAMINOURONIUM DINITRATE
We recently investigated diaminouronium nitrate, which is a new secondary explosive. With
regard to development of new high-oxidizers the double-protonated compound
diaminouronium dinitrate (DAU_2NO3) was synthesized starting from cheap available
diaminourea, which is protonated with two equivalents of dilute nitric acid according to
Synthesis of diaminouronium dinitrate monohydrate.
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.
p44 https://www.serdp-estcp.org/content/download/10799/136954/fi... |
Yes, that and the Fischer paper seems to be the only source on this synthesis that we are all using, as far as I know (and I have looked). There is
one older, similar ref by the same author(s).
[Edited on 9-7-2019 by twelti]
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
Right now I'd need to use aluminum foil as my witness plate, as I don't have a lot of material here. But I'm gonna make a much bigger batch.
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
| Quote: Originally posted by Microtek | Do you know what the solubility of DAUDN is in this solvent system? The "melting" that you see may actually be the product dissolving as the
temperature rises and the solubility therefore increases.
About the dessicants: P2O5 is certainly a stronger dessicant than concentrated sulfuric acid. In fact also stronger than SO3, since P2O5 can dehydrate
sulfuric acid to form SO3 and phosphoric acids of diferent kinds. |
That is what confuses me. What IS the solvent system. There should only be maybe some water, and if one removes that, DAUDN only. Maybe there was a
small amount of water still in my mixture.
|
|
|
Microtek
National Hazard
Posts: 869
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
Didn't you add methanol? This may function as a solvent or maybe an anti-solvent in conjunction with water, I can't really tell.
|
|
|
underground
National Hazard
Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
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]
|
|
|
twelti
Hazard to Others
Posts: 217
Registered: 20-2-2019
Member Is Offline
|
|
| Quote: Originally posted by Microtek | | Didn't you add methanol? This may function as a solvent or maybe an anti-solvent in conjunction with water, I can't really tell.
|
Right, of course, I forgot about that. It just seems weird to be adding a solvent to an oil.
|
|
|
| Pages:
1
2
3
4
5
..
8 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
