Sciencemadness Discussion Board - DIAMINOURONIUM (DI)NITRATE

DUN is quite insensitive, you wont have any problem for casting it. Your product thow looks a bit transparent while mine is complitely white solid, strange. Is it hygroscopic ? Is it solid at room temperature?

[Edited on 2-8-2019 by underground]

My crystals are also transparent-ish, even before casting. Was yours white even after casting? I'm still wondering if using stronger NA like you are is an issue. I'm not sure if it is hygroscopic. It looks just like hardened plastic. i did notice a mall area that was still gooey after cooling, though it seemed to eventually harden.

What do you guys think it will take to detonate this stuff. SADS for example. 60 mg, 100, more...?

underground - 2-8-2019 at 13:52

Put some ETN as a booster for detonate. If it goes try then w/ο ETN. After casting it, is it still transparent-ish or not ?

Is there any possibility that there is still some water in there ?

[Edited on 2-8-2019 by underground]

MineMan - 2-8-2019 at 22:35

Whoever detonates this makes history on this board!!

twelti - 2-8-2019 at 22:59

Whoever detonates this makes history on this board!!

I did a cast, around 1.5 g of DAUN, poured into a plastic tube, I put 200 mg of ETN lightly pressed on top. Then around 100 mg of SADS. Will test tomorrow.

Tested: no detonation. I guess it needs more. Will try with 700 mg.

[Edited on 3-8-2019 by twelti]

twelti - 3-8-2019 at 19:49

I now remembered one reason I am wondering about using concentrate nitric acid in the synth. What about leftover acid in the DAUN?? For other EMs we can easily recrystallize and nuetralize them. How do we do that here? I tested and of course it is acidic. Will it be stable as is? It may be a pain to reX this stuff to get all the acid out of the crystals. Maybe THAT is why they used dilute NA?

underground - 4-8-2019 at 03:34

Your solution should not be acidic. I did not check mine but i really doubt that it was acidic. Did you correctly use your molar ratio ? You may have added a lot of NA and what you may have now is the Dinitrate salt.

twelti - 4-8-2019 at 10:06

Your solution should not be acidic. I did not check mine but i really doubt that it was acidic. Did you correctly use your molar ratio ? You may have added a lot of NA and what you may have now is the Dinitrate salt.

I checked twice, with litmus paper. Amount of NA and DAU used was same as in Fischer, though in the last one I used less NA dilution. Could be off very slightly due to measurement error.

In the last batch, I went to drive off the extra water, and overshot a little. Came to find a white gooey mass. Before, when I melted crystalline DAUN to cast it, it was clear. This stuff was opaque white. When it cooled off it was still a very slightly gooey in parts. I'm thinking there was still water in it. I added some water to the gooey white mass and it readily dissolved. Then I added Methanol and it came out of solution. Looked like curdled milk. So I guess this is how it could be recrystalized if that were necessary.

EDIT: looks like the DAUN does not really dissolve in water, since upon standing the water separates. It's a little confusing.

[Edited on 4-8-2019 by twelti]

underground - 4-8-2019 at 13:07

From pdf they claim that the salt got high density due to hydrogen bonds between the molecules. I believe the same is happening with water, and maybe that is why it is hard to crystalise out, even thow the solubility is not that great.

[Edited on 4-8-2019 by underground]

MineMan - 5-8-2019 at 22:54

Surly Rosco has some input on this thread...?

twelti - 7-8-2019 at 16:08

Surly Rosco has some input on this thread...?

Wherefor art Thou, Sir Roscoe?

twelti - 7-8-2019 at 16:14

I have tried a couple of times, to detonate some of this. Twice w cast and once with pressed powder. Seems to want a healthy kick to get it going...?

underground - 7-8-2019 at 22:51

I have tried a couple of times, to detonate some of this. Twice w cast and once with pressed powder. Seems to want a healthy kick to get it going...?

So did you actually detonate it ?

MineMan - 8-8-2019 at 15:47

The world is waiting....

twelti - 8-8-2019 at 19:58

I'm not 100% sure. I have been using the steel conduit box cover plates that you buy at the HW store. compared to what 700 mg of PETN does to it, the damage from around 2.5 g of DAUN didn't look to be enough. I think I need a larger diameter charge.

Here is my latest batch. 6.5 ml 70% NA, diluted to 40 ml with H2O, and added 9 g of DAU. I gently boiled it down to 20 ml, then vacuum down to 15 ml. Then I added EtOH, up to 80 ml. It seems that at least once when I quickly poured in EToH, I got a lot of crystals fairly quick. This time I added it gently and din't stir. Nice layer of oily DAUN at the bottom. Even after I eventually it did stir it, it settled back down.
What does the alcohol DO? Shuld we be using EtOH or MeOH or even something else?

I'm still wondering about the concentration of the NA. Does the actual concentration matter? Or is it purely the amount of NA, irregardless of how much water there is? Could one go the other way and use WFNA then, and have NO water to remove? Probably a bad idea but....

Tsjerk - 8-8-2019 at 20:43

I think diaminouronium nitrate really needs a water molecule to crystallize, ethanol and methanol either pull of water molecules or dilute the water available (while the crystals not being soluble in the alcohol), making the crystallization possible.

I'm interested in a reaction, theory all over, where methanol/ethanol is used as a solvent and the needed nitric acid is added with just a 1:1 molar amount of water. Keep this reaction below zero during the first try!

Edit: dissolve the base in ethanol/methanol --> cool in a freezer --> put on ice --> add 50:50 molar water/HNO3.... see what happens. My guess: instant crystallization of the mono-hydrate.

Quote:

I'm not 100% sure. I have been using the steel conduit box cover plates that you buy at the HW store. compared to what 700 mg of PETN does to it, the damage from around 2.5 g of DAUN didn't look to be enough. I think I need a larger diameter charge.

How do you detonate? What primary do you use?

What does the alcohol DO? Shuld we be using EtOH or MeOH or even something else?

I think it dissolves one (or more) of the products and forms an "organic layer". I see the same when reacting benzaldehyde/acetone/NaOH/water. I get a separation that is not linear with one of the reactants.

[Edited on 9-8-2019 by Tsjerk]

twelti - 9-8-2019 at 12:32

Quote: Originally posted by Tsjerk

I think diaminouronium nitrate really needs a water molecule to crystallize, ethanol and methanol either pull of water molecules or dilute the water available (while the crystals not being soluble in the alcohol), making the crystallization possible.

I'm interested in a reaction, theory all over, where methanol/ethanol is used as a solvent and the needed nitric acid is added with just a 1:1 molar amount of water. Keep this reaction below zero during the first try!

Edit: dissolve the base in ethanol/methanol --> cool in a freezer --> put on ice --> add 50:50 molar water/HNO3.... see what happens. My guess: instant crystallization of the mono-hydrate.

Quote:

How do you detonate? What primary do you use?

What does the alcohol DO? Shuld we be using EtOH or MeOH or even something else?

Thanks for your comments. I will try your suggested approach and report back. As for primary, i was using SADS+KCLO3, then 600 mg of PETN. I think maybe it just needs a bigger kick and/or larger diameter tube.

Actually, when you are you talking about the monohydrate, are you talking about the dintrate monohydrate, i.e. [3] from Fischer? that is the less interesting version as I understand it. The nitrate is the one we want.

[Edited on 9-8-2019 by twelti]

Tsjerk - 9-8-2019 at 14:45

No, I'm talking about they mono-nitrate monohydrate, I didn't dubblecheck but from what I remember both the nitrates crystallize as the mono-hydrate.

twelti - 9-8-2019 at 17:34

BTW I found this patent which is related
US2970899A

This sort of describes what happened to my when I boiled the product solution down too far:

in attempting to dehydrate the carbohydrazide mononitrate by lheating C.), it was found that water was driven off. At the cessation of this water evolution, heating was discontinued. The distillate was opaque milky white and very viscous. Upon standing, it scparated into two phases into a clear, colorless, viscous liquid and the white solid. It was found that the solid constituted about 18% of the total weight of the distillate. Repeated attempts at analyzing and classifying this substance were unsuccessful. It was assumed that the solid material was either a decomposition product or a product of molecular rearrangement or both.

[Edited on 10-8-2019 by twelti]

MineMan - 9-8-2019 at 20:27

Does this mean one does need 40 percent or less HNO3 for the mononitrate?

I see. So we can’t boil it? Guess that’s why you’re did not det

underground - 10-8-2019 at 02:52

Hmm interesting. That is why my product was a solid white. It possibly must be a molecular rearrangement or the unhydrate form since i did not heated it that much to decompose the whole product and the whole product was that white solid. In addition the decomposition temp of mononitrate is 242 C and i really doubt that i reached that temp.

[Edited on 10-8-2019 by underground]

twelti - 10-8-2019 at 08:10

I'm not sure, but I think now that white stuff might be an EM too. I put around a g in a small tube w 700 mg of PETN and I think it did detonate. I'm not 100% sure. I need to try a larger amount.

The whole thing is driving me nuts since I have done this maybe 7 times and on one attempt I got a pretty good and quick yield of crystals, but not positive what I did different. I WILL find out though. If anyone wants to try, and doesn't have the carbohydrazide, I can send some. I have plenty!

underground - 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 ?

[Edited on 10-8-2019 by underground]

twelti - 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?

underground - 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.

twelti - 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??

underground - 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]

twelti - 10-8-2019 at 16:31

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?

underground - 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]

twelti - 10-8-2019 at 19:09

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?

Tsjerk - 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

twelti - 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.

twelti - 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?

underground - 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]

twelti - 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.

underground - 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.

twelti - 16-8-2019 at 12:08

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.

twelti - 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?

underground - 25-8-2019 at 13:27

Hmmm maybe a mixture of DUN and ETN or even HMTD/TATP would surely sensitize it.

twelti - 25-8-2019 at 14:21

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?

underground - 25-8-2019 at 14:45

I have not yet do anything but i will

MineMan - 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.

twelti - 26-8-2019 at 07:34

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.

Success!

twelti - 1-9-2019 at 17:42

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:

MineMan - 1-9-2019 at 20:39

Excellent.

Do you think it is worth the trouble?

twelti - 1-9-2019 at 22:31

Excellent.

Do you think it is worth the trouble?

Not really any trouble once you know how. Gotta try detonating the cast version now.

underground - 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]

twelti - 2-9-2019 at 18:37

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]

I think it IS the white stuff like you got. It is just powdered. I found that if you evaporate it down to a syrup, and add a small amount of methanol, maybe 2 or 3 times the volume of the syrup, you can get it to a (suspended) crystalline powder, and filter or whatever. Much easier to handle that way. It is weird though, sometimes it doesn't work and i have to try again. It is somewhat unpredictable, or I just haven't figured it out yet. I did previously do one that was solid white like yours, and I think it worked too. Just needs a healthy kick.

I will try 2.5 g of ETN, same setup.

underground - 3-9-2019 at 01:00

Very good information twelti, well done! I will let you know when i test my own. It looks promising.

Rosco Bodine - 3-9-2019 at 11:06

Surly Rosco has some input on this thread...?

The carbohydrazide perchlorate would be the interesting candidate for testing from what I get as an impression.

It could make an interesting double salt with guanidine perchlorate, or triaminoguandine perchlorate, or other perchlorates like betaine perchlorate or glycine perchlorate or hydrazine perchlorate or methylamine perchlorate, or trimethylamine perchlorate, or tetramethylamine perchlorate, or possibly even hexamethylene tetramine diperchlorate.

Some of these might also form complex salts with nickel or copper or possibly even silver.

Another possibility is that the nickel carbohydrazide perchlorate might form a double or mixed salt with nickel hydrazine perchlorate or nickel semicarbazide perchlorate. The complex nickel hydrazine perchlorate is reportedly exceedingly sensitive and dangerous but the semicarbazide nickel complex analogue is a material on which I have been unable to find any references.

[Edited on 9/3/2019 by Rosco Bodine]

MineMan - 3-9-2019 at 11:54

Quote: Originally posted by Rosco Bodine

Surly Rosco has some input on this thread...?

Why would these double salts be interesting...?the molecules you listed already contain a nitrogen containing fuel and an oxidizer...

The nitrate is easy and cheap to make... any thoughts on raising its heat of formation (explosion) or on how to crystallize effectively?

twelti - 3-9-2019 at 14:21

Quote: Originally posted by Rosco Bodine

Surly Rosco has some input on this thread...?

Not sure bout the heat, but crystallizing is easy. I'm using about a quarter of the water they used in Fischer, to minimize water content but prevent too much heating when you add the carbohydrazide. I evaporate it down (a little heat and a lot of stirring and air), then put some methanol on top, so it layers, then drop a couple of seed crystals in. Around 3 days and it is done - no refrigeration needed. I think the methanol is sucking the remaining water from the nitrated mixture, not sure.

wessonsmith - 3-9-2019 at 15:04

Are you going to make a nice, easy to follow step by step how-to video

[Edited on 3-9-2019 by wessonsmith]

Rosco Bodine - 3-9-2019 at 16:11

Quote: Originally posted by Rosco Bodine

Surly Rosco has some input on this thread...?

Sheesh...Put on your thinking cap to become a curious cat. But try not to let curiosity kill the cat. Be a very wary and careful smart cat. Paranoid watchful nervous cats are rarely and less likely to become road kill or get their twitching little low mileage tails pinched by any ancients' rocking chairs.

What are unknowns there about such double salts or complexes or mixtures are interesting because properties can be synergistic and desirable.

It is only very rarely that single compounds are used neat in pure form as an ideal component but are more often "compounded" in "medicinal" designer formulations where the various components contribute their benefit to the formulation that is a sum and maybe more than just a simple sum of the components.

Carbohydrazide Perchlorate is itself interesting and so is its complex with Nickel.

Another possible reaction and double salt would be the possible reaction of Carbohydrazide with Ammonium Perchlorate.

Would simply dissolving Carbohydrazide in a warm water solution of Ammonium Perchlorate result in displacement of Ammonia byproduct and formation of Carbohydrazide Perchlorate and/or a double salt?

If the solubility driven reaction would occur, that would be worth knowing. Or such a reaction might require a different approach to exploit solubility for driving a metathesis "ion exchange" reaction.

Calcium Hydroxide can be reacted with Ammonium Perchlorate to displace Ammonia and result in a Calcium Perchlorate solution.
A low solubility Calcium Sulfate or even lower solubility Calcium Sulfate - Sodium Sulfate double salt could possibly be precipitated
to leave a dilute Perchloric Acid having been substantially stripped of its Calcium value....ready for neutralization by Carbohydrazide, with evaporation and crystallization and filtering to obtain the Carbohydrazide Perchlorate. If a cocrystallization with Ammonium Perchlorate does occur then that could be done to facilitate isolation of a double salt.

Thinking Cap / curious cat / example / exhibit A

[Edited on 9/4/2019 by Rosco Bodine]

twelti - 4-9-2019 at 09:22

Quote: Originally posted by wessonsmith

Are you going to make a nice, easy to follow step by step how-to video

[Edited on 3-9-2019 by wessonsmith]

Could do, maybe this weekend!

wessonsmith - 4-9-2019 at 10:19

Could do, maybe this weekend!

Awesome!

twelti - 7-9-2019 at 19:56

OK, I did a comparison to the 2.5 g of DAUN (see previous post). This was 2.5 g ETN straight up. Same conditions, both in 3/8" ID CF tubes, next to conduit cover plate. Looks like the DAUN is more brissant, though this is not a super scientific test.

underground - 7-9-2019 at 23:53

WoW twelti this is amazing!!! I didn't expect that!! Sometimes i was thinking if i did well by buying DU but now i am really glad i bought it lol.

[Edited on 8-9-2019 by underground]

twelti - 8-9-2019 at 08:50

WoW twelti this is amazing!!! I didn't expect that!! Sometimes i was thinking if i did well by buying DU but now i am really glad i bought it lol.

[Edited on 8-9-2019 by underground]

Me too, I was beginning to doubt, but now I know I didn't waste my money! Have you managed to get the crystalline powder form yet? I'm now wondering if there is some way to control crystal size etc. Right now it is either medium sized crystals or solid. Also want to try adding the aluminum, and maybe investigating the perchlorate salt as Rosco mentioned.

underground - 8-9-2019 at 11:34

I will definitely try what you did in order to get the crystals. I will let you know when i got any news.

MineMan - 8-9-2019 at 11:57

OK, I did a comparison to the 2.5 g of DAUN (see previous post). This was 2.5 g ETN straight up. Same conditions, both in 3/8" ID CF tubes, next to conduit cover plate. Looks like the DAUN is more brissant, though this is not a super scientific test.

Excellent work! This makes sense as the VOD is almost 9000 and the volume of gas is very high.

Can you try casting it now?

I hate starting this thread and not contributing, but, I am not able to at this time.

Some thoughts

franklyn - 14-9-2019 at 02:29

1,3-Diaminourea
N,N'-diamino-Urea
Carbohydrazide
Carbonicdihydrazide
Carbonyldihydrazine
https://en.wikipedia.org/wiki/Carbohydrazide
Hazardous Chemicals Desk Reference
https://books.google.com/books?id=WZeBDwAAQBAJ&lpg=PA161...

Any of the above names appended with dinitrate identify the same molecule.
Essentially this compound is comprised of 2 Hydrazino Nitrate moieties joined to a carbonyl. It's properties must be much like the known data on Hydrazinium Nitrate.
www.sciencemadness.org/talk/viewthread.php?tid=874#pid187600
www.sciencemadness.org/talk/viewthread.php?tid=10058#pid1194...
www.researchgate.net/publication/330474244_Detonation_proper...

It's annoying the cited paper only evaluates the hydrate which can scarcely be regarded a discreet compound. The mol of water is a spectator and absorbs much heat on detonation. Using Engager's Detonation utility and the heat of formation value Δ f in the paper to evaluate the hydrate gives a detonation velocity a little short of the one printed , ~ 7200 m/s .

Given the affinity for water similar polar solvents such as Methanol and Glycol should blend. Adding a small amount of Methanol less than 4.7 % , stoichiometrically balances detonation products and may serve to sensitize. Ethylene Glycol thinned with Methanol blended with the anhydrous Dinitrate and vacuum drying off the lighter Methanol so only the Glycol remains to prevent formation of the crystal latice can yield a plastic composition. Refrain from kneading with fingers until properties are determined. 5.4 % composition of Glycol is oxygen balanced.
3 CO(NH.NH2)2•2HNO3 + CH3OH => 4 CO2 + 14 H2O + 9 N2
5 CO(NH.NH2)2•2HNO3 + C2H4(OH)2 => 7 CO2 + 23 H2O + 15 N2

Peroxidates of ionic Nitrates disussed here => www.sciencemadness.org/talk/viewthread.php?tid=1778&page...
suggest Hydrogen Peroxide can substitute the water of the hydrate to form an adduct. Vacuum drying from a solution with 40 vol hair bleach which is 12 % peroxide should yield the adduct. To acertain the product put a smal puddle of Hypochlorite solution ( laundry bleach ) a few centimeters from a sample and tilt the setup so the liquid runs to contact it to react effervescently. I don't think this can cause detonation but assume it could.

Acidity of the Dinitrate as yet undisclosed or referenced can perhaps join with a base molecule in a co-crystal lattice. I discussed this liklihood with Dinitrourea + Nitroguanidine to form an Adduct. 5 CO(NH.NH2)2•2HNO3 + 2 (NH2)2CHNNO2 => 7 CO2 + 25 H2 + 19 N2
www.sciencemadness.org/talk/viewthread.php?tid=9443#pid17013...

Actual test detonation velocity data can be had with this setup.
www.sciencemadness.org/talk/viewthread.php?tid=63051#pid4130...

.

MineMan - 14-9-2019 at 13:05

Really interesting franklyn... glad to see your back and thank you for the thoughts!!

I have to admit, the mono nitrate seems much simpler... but I am assuming the techniques you provided will greatly increase the dinitrate.

More thoughts

franklyn - 16-9-2019 at 14:47

Would be nice if this program were in the public domain , providing one would not also need a supercomputer to use it.

Theoretical Prediction of the Heats of Formation , Densities , (etc.) by computation
www.arl.army.mil/arlreports/2015/ARL-TN-0693.pdf

CO(HNNH2)2• HNO3 => 3 H2O + CO + 3 N2 + H2
2 CO(HNNH2)2• 2HNO3 => 8 H2O + 2 CO2 + 6 N2 + O2

Co-crystallization of two dinitrate mols with one mononitrate mol is oxygen balanced.

2 CO(HNNH2)2• 2HNO3 + CO(HNNH2)2• HNO3 => 12 H2O + 3 CO2 + 9 N2

The mononitrate must have some slight basic quality favoring formation of a peroxidate.

CO(HNNH2)2• HNO3 •H2O2 => 5 H2O + CO + 3 N2
CO(HNNH2)2• 2HNO3 => 4 H2O + CO2 + N2 + 1/2 O2

Co-crystallization of one mol mononitrate peroxidate with one mol dinitrate is oxygen balanced.

CO(HNNH2)2• 2HNO3 + CO(HNNH2)2• HNO3 •H2O2 => 9 H2O + 2 CO2 + 4 N2

From the known behavior of Nitromethane in composition with Ammonium Nitrate , alias Kinepak , similar sensitization occurs with Urea Nitrate , it follows some addition to Diaminouronium mononitrate can make it readily detonable.

Digressing from the subject of this thread , chlorinating DAU should substitute at least the amine hydrogens producing a di-acid 1,3-Dichloramine urea.
CO(HN.NCl2)2 => 2 HCl + COCl2 + 2 N2 ( Hydrogen Chloride & Phosgene as a product , hmm )
Complete chlorination takes it to CO(NCl.NCl2)2 , not a known compound from what I can see , although Tetrachlorohdrazine exists N2Cl4
Dichlorourea CO(HNCl)2 preparation
https://books.google.com/books?id=vyPOAAAAMAAJ&lpg=RA1-P...

A diverse varied chemistry evolves from this seemingly bland precursor DAU presenting many further avenues for investigation.

www.sciencemadness.org/talk/viewthread.php?tid=20296#pid2604...

www.sciencemadness.org/talk/viewthread.php?tid=2945&page...

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twelti - 21-9-2019 at 14:40

Yer makin my head spin again. If there is a simple and most interesting thing to try, what would it be?

BTW, tried again with the cast DAUN. Still no go, though it may be my fault. I think I may have had a small physical gap in the firing train, between the ETN (0.7 g hand pressed) and the 2 g of cast DAUN. Maybe .5 mm gap. Not sure if that would cause it to not kick off.

underground - 21-9-2019 at 16:51

Try a core of ETN or a mini shape charge for better initiation

[Edited on 22-9-2019 by underground]

MineMan - 12-10-2019 at 11:23

Any update for the cast stuff? This looks like the perfect insensitive explosive. Also. Would love to see a cast mixed with 20 percent fine aluminum.

underground - 12-10-2019 at 13:02

Unfortunately i am quite busy those days. I have already cast some DUN into some small containers but i have not tested them yet. I wraped them with some plastic wrap and all are dry except one where the wrap was almost removed. The top of that container was like cream due to its hygroscopicity, after removing that cream, it was solid like all the others. I will post here when i got any news from future tests.

[Edited on 12-10-2019 by underground]

Mr.Greeenix - 22-12-2019 at 04:15

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?

I just wondered can you maybe describe exactly how you got those crystalls? I cant seem to get any crystalls from an water/ethanol mixture, even after weeks of standing...

underground - 26-12-2019 at 09:33

I just tried to ddt some DUN with just hmtd and with hmtd+petn for a booster, thet both failed to ddt. I will do some more tests but the stuff looks quite insensitive.

MineMan - 27-12-2019 at 08:49