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dettoo456
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Melamine itself has solubility issues in water, so a salt would be needed, and I don’t know how prone such a salt would be to hydrolysis. I don’t
have any melamine, but I do have some acetoguanamine, so I might try to mess with that and see if anything promising is yielded.
[Edited on 26-5-2024 by dettoo456]
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Etanol
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Thanks for the idea. Ligand replacement is a real breakthrough in the synthesis of metal complexes. It works!
I successfully prepared copper-bis(4-amino-1,2,4-triazole) perchlorate from [Cu(NH3)4](ClO4)2 by reaction:
[Cu(NH3)4](ClO4)2+2ATrz=>[Cu(ATrz)2](ClO4)2+4NH3
[Cu(NH3)4](ClO4)2 was dissolved in hot water, ATrz was added, then the water is depressed with a hair dryer. Dirty blue powder has formed.
I cannot call the [Cu(NH3)4](ClO4)2 a primary explosive. But despite the poor oxygen balance ATrz complex without a shell in an amount of 50-100 mg
burns a very sharp bright flash. I think, placed in the shell is quite suitable.
The substance is not sensitive to friction. 10-20 mg placed in foil burns sharply when heated, but detonates when hit with a hammer on a steel plate.
upd 50mg dried subs detonated without shall!
[Edited on 4-6-2024 by Etanol]
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Etanol
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[Ni(4-aminotriazole)3](ClO4)2 was obtained in the same way. As you said, it does not detonate without a shell, but 30-50 mg in foil detonate when
heated.
How about [Cu(Diaminourea)2](ClO4)2 and [Ni(Diaminourea)3](ClO4)2? Is it stable with long storage? Is it oxidized by oxygen of air? Hydrolysis?
[Cu(aminourea)2](ClO4)2 and [Ni(aminourea)3](ClO4)2?
Is there a way to make [Cu(aminourea)2](ClO4)2 and [Ni(aminourea)3](ClO4)2 from Semicarbazide Hydrochloride?
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dettoo456
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Carbohydrazide (1,3-diaminourea) can be prepared by amination of Semicarbazide with Hydrazine or just by amination of urea with a large excess of
hydrazine. These amination reactions though, can be complex and will result in aqueous mixtures of Urea, Semicarbazide, Carbohydrazide, and
Hydrazodicarbonamide. If you want a source for Carbohydrazide, pyrohobby.ru might still have some for sale, but they have a horrible payment system
that isn’t secure at all.
trisCarbohydrazide Nickel diPerchlorate (NiCP) apparently works as a decent primary (and is likely stable enough in storage) to function in detonators
as mentioned in some Chinese patents, but at least the trisCHLORATE (NiCC) analogue is also a strong performer; see thread: http://www.sciencemadness.org/talk/viewthread.php?tid=159732
The Cu complex may work as well, though I have no idea and don’t plan to test it. Carbohydrazide is a pain to try to make, at least for me.
[Edited on 7-6-2024 by dettoo456]
Attachment: Tris carbohydrazide nickel perchlorate (NCP).pdf (32kB)
This file has been downloaded 179 times
Attachment: Hydrazodicarbonamide.pdf (300kB)
This file has been downloaded 171 times
[Edited on 7-6-2024 by dettoo456]
[Edited on 7-6-2024 by dettoo456]
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Etanol
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Thanks. I understand correctly that carbohydrazide (diaminourea) is more stable than semicarbazide (aminourea)?
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dettoo456
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Chemically, Semicarbazide is more stable. The hydrazine bond is less stable than the simple amide. But, Carbohydrazide will of course be better as a
fuel, due to the higher energy of the 2 N-N bonds.
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Etanol
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Quote: Originally posted by dettoo456  | Chemically, Semicarbazide is more stable. The hydrazine bond is less stable than the simple amide. But, Carbohydrazide will of course be better as a
fuel, due to the higher energy of the 2 N-N bonds.
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It seems strange to me that carbohydrazide is sold in free form, but semicarbazid is sold only in the form of hydrochloride.
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dettoo456
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Both exist as solids at STP, but Semicarbazide is likely just too hygroscopic and basic, so it’d form hydrated solutions and/or carbonates. Same as
Aminoguanidine and guanidine.
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Etanol
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What is the solubility of copper glycinate-perchlorate?
How fast is its DDT? Is it detonate unconfined or only in a strong metal shell?
I tried to prepare copper glycinate-perchlorate with electrolysis of the equimolar mixture of glycine and NH4ClO4 until hydrogen stopped released.
Then I filled the solution from copper powder, flawed it and dried. Blue non-crystall powder formed, which is not detonate without confined. However,
it burns better than copper tetraammine perchlorate.
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Null
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| Quote: Originally posted by snooby | Okay guys,
ICM 103 is something nobody of us would like to try out. The pyrazole stuff seems inpossible to get hands on. However, I can buy IT and ship it around
the world. Price is around 1000 dollars for 500 grams (WTF). And if I lower the price would increase (50 grams are 380 dollars). So, are there 3 or 2
other guys/girls who would like to share the costs? Price would be around 200 dollars for 100 grams. That's a LIFE supply. I AM willing to receiver
the order and ship IT around our globe. Sent me an PM if you would like to join. Only first 3 guys can get involved.
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Hope this is still relavent to the thread, but it appears there is a decent place to get a precursor for this at chem impex for less than $100 for 100g.
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dettoo456
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I hate to rain on your parade but there are far cheaper, easier to mfg, less toxic, and better performing EMs out there compared to this esoteric
primary; AgNTz, BNCP, DBX-1, or even micronized PETN/C. Most of the ‘next-gen’ EMs are just thought up and pushed by military contractors to win
outrageously expensive contracts for the way too expensive compounds they plan to make.
I.E., LLM-105 is nothing special in terms of performance, sensitivity or environmental safety, and yet is somehow being made in bulk because a company
convinced a general somewhere that it’s God’s gift to man - even though they’ll require $1000s in taxpayer dollars to produce something like 90g
for a hand grenade. Same issue with Cl-20.
If this precursor was some obscure phenethylamine or indole that’d produce a highly active serotonin moderator  , then maybe that ‘investment’ would be worth it.
Also, Chemimpex along with companies like Chemdirect only ship to commercial addresses - and that’s almost universal for all chem suppliers
nowadays.
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Null
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Yep, you're right. I only focused on the pricing and not the delivery requirement. I have had a few companies allow me to use "Individual" for the
company, but you're probably right in this not being one of them.
I will try with something innocuous, but yeah, I was too money focused on that.
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dettoo456
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I was able to get some personal chemical orders shipped to my work’s building from chemimpex, chemdirect, and thermo, and you might have luck with
that too depending on your job, but you’d need to sort it all out beforehand of course (billing and end-use auth).
Good luck with whatever EM research or precursor procurement you’re looking into though
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Etanol
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| Quote: Originally posted by Microtek |
The cobalt complex seems to be very insoluble, and gave a high yield of very fine cream precipitate. I did a second run with slow addition of the
cobalt ions to a hot, stirred solution of ATrz and NaClO4, and cooled slowly with continued stirring, and this gave a slightly more coarse powder that
could more easily be filtered. I ran it through the plate dent test after discovering that I could not set it off by mechanical stimulus, either by
manual hammer blows on my anvil, or by the oblique abrasive pendulum impact test at 5.5 J (the highest setting of my apparatus). In the plate dent
test, it performed disappointingly - somewhere in the vicinity of TNT, possibly due to a surprisingly low density of 1.58 g/cc.
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Hmm, Co(II) or Co(III) ?
Co(II)- 4-ATRz-ClO4 complex may be very powerful.
CoCO3+2HClO4=>Co(ClO4)2+CO2
Co(ClO4)2+NH4ClO4+NH3(excess)+H2O2=>[Co(NH3)6](ClO4)3 red solution
[Co(NH3)6](ClO4)3+3 (4-ATrz)=(boiling?)=>[Co(4-ATRz)3](ClO4)3
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Etanol
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| Quote: Originally posted by Etanol | | Quote: Originally posted by Microtek |
The cobalt complex seems to be very insoluble, and gave a high yield of very fine cream precipitate. I did a second run with slow addition of the
cobalt ions to a hot, stirred solution of ATrz and NaClO4, and cooled slowly with continued stirring, and this gave a slightly more coarse powder that
could more easily be filtered. I ran it through the plate dent test after discovering that I could not set it off by mechanical stimulus, either by
manual hammer blows on my anvil, or by the oblique abrasive pendulum impact test at 5.5 J (the highest setting of my apparatus). In the plate dent
test, it performed disappointingly - somewhere in the vicinity of TNT, possibly due to a surprisingly low density of 1.58 g/cc.
|
Hmm, Co(II) or Co(III) ?
Co(II)- 4-ATRz-ClO4 complex may be very powerful.
CoCO3+2HClO4=>Co(ClO4)2+CO2
Co(ClO4)2+NH4ClO4+NH3(excess)+H2O2=>[Co(NH3)6](ClO4)3 red solution
[Co(NH3)6](ClO4)3+3 (4-ATrz)=(boiling?)=>[Co(4-ATRz)3](ClO4)3
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The subs is a dark-red resin or red-brown grains that easily melt into red resin. When cooling, the resin turns into a red vitreous mass. The
substance is poorly soluble in cold water and insoluble in isopropyl alcohol.
It is difficult to ignite. Unconfined, it melts first, then burns with flashes and burns out. The melting temperature is lower than the decomposition
temperature.
Unconfined, being heated on a metal foil, it melts, then burns with a flash.
Approximately 20-30 mg, confined into aluminum foil, strong detonate when heated.
In my opinion, this is powerful, but unsuitable subs.
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MineMan
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| Quote: Originally posted by Etanol | | Quote: Originally posted by Etanol | | Quote: Originally posted by Microtek |
The cobalt complex seems to be very insoluble, and gave a high yield of very fine cream precipitate. I did a second run with slow addition of the
cobalt ions to a hot, stirred solution of ATrz and NaClO4, and cooled slowly with continued stirring, and this gave a slightly more coarse powder that
could more easily be filtered. I ran it through the plate dent test after discovering that I could not set it off by mechanical stimulus, either by
manual hammer blows on my anvil, or by the oblique abrasive pendulum impact test at 5.5 J (the highest setting of my apparatus). In the plate dent
test, it performed disappointingly - somewhere in the vicinity of TNT, possibly due to a surprisingly low density of 1.58 g/cc.
|
Hmm, Co(II) or Co(III) ?
Co(II)- 4-ATRz-ClO4 complex may be very powerful.
CoCO3+2HClO4=>Co(ClO4)2+CO2
Co(ClO4)2+NH4ClO4+NH3(excess)+H2O2=>[Co(NH3)6](ClO4)3 red solution
[Co(NH3)6](ClO4)3+3 (4-ATrz)=(boiling?)=>[Co(4-ATRz)3](ClO4)3
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The subs is a dark-red resin or red-brown grains that easily melt into red resin. When cooling, the resin turns into a red vitreous mass. The
substance is poorly soluble in cold water and insoluble in isopropyl alcohol.
It is difficult to ignite. Unconfined, it melts first, then burns with flashes and burns out. The melting temperature is lower than the decomposition
temperature.
Unconfined, being heated on a metal foil, it melts, then burns with a flash.
Approximately 20-30 mg, confined into aluminum foil, strong detonate when heated.
In my opinion, this is powerful, but unsuitable subs. |
Compared to what? If it is safe and powerful enough to initiate why are you disappointed?
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dettoo456
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Probably because it seems to just have too low of a DDT. The most promising primaries deflagrate on open flame contact or directly detonate. This
stuff seems too poorly characterized (as of now) and the fact that it melts before fully decomposing is unfavorable in general.
It could have promise though, as you suspect. Cation or anion swapping for EM complexes is always a possible pathway to find good candidates for use.
Perhaps the Ag, Ni, Fe salts of BrO3, IO4, NO3, etc.
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pdb
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Long life, short list
Energetic materials have been a hobby of mine for several decades. Especially primary explosives, due to their diversity and their ability to achieve
DDT, which I find fascinating. As far as I know, the phenomenon that produces a shock wave in a few milligrams of primary explosive from a flame is
not yet fully understood.
What I find ironic is that this passion doesn’t involve thousands of products but only a small number, even though, in chemistry, the substances
capable of exploding number in the tens of thousands. Personally, I believe I have prepared fewer than twenty primary explosives in total, which I
list here:
Pb(N3)2
Hg(N3)2
AgN3
Cd(N3)2
Hg(CNO)2
AgCNO
Ag nitrotetrazole
Ag azotetrazone
Ag2C2
Ag2C2·AgNO3
TATP
HMTD
DBX-1
DDNP
Tetracene
C3H12 cyanuric triazide
3-nitrobenzenediazonium perchlorate (CAS 22751-24-2)
2,4-Dinitro-benzenediazonium perchlorate (CAS 197637-25-5)
It’s not a lot, but it has been enough to keep me captivated for thousands of hours in my life. What should one make of this? Is it absurd and sad,
or just original, like other more popular passions, such as music, painting, sports, etc.?
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greenlight
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There's a lot of hobbies out there that are much stranger than synthesising and testing energetics. It is quite unique due to the danger involved and
illegality in most countries which is enough to deter the majority of people. Embrace it I say, as long as your doing it safely, it's definitely
something different, I have been interested for nearly two decades and on and off experimenting when I can.
You've got quite an extensive list of primaries there. I have only made a few of them as I have always used them mainly for initiation of
secondaries.
We do have some theories on the DDT transition.
When dealing with primaries like TATP or HMTD you may have noticed that the same unconfined pile that poofed underwent DDT when confined in even an
open ended paper tube. In small amounts in the open, the gases are able to expand freely whereas in any spatial confinement they reflect and form
turbulences which increase flame velocity. This exponential rise in flame temperature and resulting gas pressure is thought to be responsible for
the transfer to detonation. Most likely when a certain temperature is reached or a certain speed of flame front (speed of sound).
When you have a large enough unconfined pile, just the weight of the explosive would be enough to cause this effect as well.
As for the primarys like azides which detonate in absolutely tiny quantities the cause is theorised to be the N3 ion. Two of the nitrogen can form
stable N2 gas but the third nitrogen atom is expelled along with a considerable quantity of energy. This lone nitrogen can react with another N3 ion
in the vicinity. If you can imagine this all happening in one small spot with millions of N3 ions decomposing simultaneously and all forming nitrogen
gas plus a lone reactive nitrogen the rapid ly violent DDT transition for say lead azide makes sense. There's more to it as its broken down into two
seperate reactions, this is just what I can recall at the moment.
Be good, otherwise be good at it 
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Etanol
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Wow! Can you say anything about the properties of this? Hygroscopicity, solubility, stability, DDT?
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pdb
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Dinitro-benzenediazonium perchlorate
I hesitated to include it in my list of primaries because I’ve never managed to achieve DDT in open air. The substance deflagrates, leaving a
combustion residue, but doesn’t detonate.
I even tried initiating it with another primary. The photo shows a trail of 2,4-Dinitro-benzenediazonium perchlorate ("DNBDP") interrupted in the
middle by 50 mg of nitrobenzenediazonium perchlorate, which constitutes a pretty powerful initiation. The fire was set at one end, and you can see
that the detonation at the center failed to propagate to the rest of the DNBDP.
Microtek, who also prepared it, said that DBBDP could achieve DDT, but neither Axt nor I have been able to make it detonate.
 
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pdb
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Yes, of course, when the configuration of the charge creates confinement—either because it is contained in an enclosure or under its own
weight—the accumulation of combustion gases and the heat released can lead to the formation of a shock wave. Even a low explosive can be made to
detonate under certain conditions.
But the question is different when a few milligrams deposited without any compression on a metal plate manage to dent or puncture it. What you say
about the N3 radical, where the ejection of one nitrogen atom impacts another N3, merely describes a chain reaction. However, the majority of chain
chemical reactions occur without detonation, so IMO this explanation is not sufficient to account for the behavior of primaries.
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Etanol
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| Quote: Originally posted by pdb | I hesitated to include it in my list of primaries because I’ve never managed to achieve DDT in open air. The substance deflagrates, leaving a
combustion residue, but doesn’t detonate.
I even tried initiating it with another primary. The photo shows a trail of 2,4-Dinitro-benzenediazonium perchlorate ("DNBDP") interrupted in the
middle by 50 mg of nitrobenzenediazonium perchlorate, which constitutes a pretty powerful initiation. The fire was set at one end, and you can see
that the detonation at the center failed to propagate to the rest of the DNBDP.
|
This is strange. Such properties can only occur if the product does not correspond to the formula of 2,4-Dinitro-benzenediazonium perchlorate.
| Quote: Originally posted by pdb |
But the question is different when a few milligrams deposited without any compression on a metal plate manage to dent or puncture
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It appears that rapid DDT requires the presence of chemical bonds with positive enthalpy and low activation energy that can be converted into
detonation products in 1-3 molecular collisions.
This contributes to a small critical detonation diameter and low detonation excitation pressure.
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Axt
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Good god pdb, it's been just shy of 20 years it's good to see you made it to 75 posts haha. This is off topic though, it's not a complex salt and the
original thread is here http://www.sciencemadness.org/talk/viewthread.php?tid=3681 . Yes, I made the dinitrobenzenediazonium perchlorate and yes its ability to DDT is
lower than that of the less nitrated homologues. Its counter intuitive for numerous reasons but is clearly shown in practice. It's likely due to
balance between the electron deficient diazonium group and the electron withdrawing nitro groups creating a stronger bond overall. Most sensitive to
least is benzene>nitrobenzene>dinitrobenzene, a clear pattern with the worst of all being the benzenebis(diazonium) diperchlorate derived from
phenylenediamine which likes to detonate in solution. On the other side, one would expect electron donating groups such as methyl (aminotoluene) to
create a more sensitive diazonium salt than even that of benzene.
I'm not sure what your photo is showing btw, it looks like an orange blob taped to the middle of some angle iron. I've never confined
dinitrobenzenediazonium perchlorate but assumed it would DDT given any excuse with confinement.
[Edited on 18-11-2024 by Axt]
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greenlight
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| Quote: Originally posted by pdb |
Yes, of course, when the configuration of the charge creates confinement—either because it is contained in an enclosure or under its own
weight—the accumulation of combustion gases and the heat released can lead to the formation of a shock wave. Even a low explosive can be made to
detonate under certain conditions.
But the question is different when a few milligrams deposited without any compression on a metal plate manage to dent or puncture it. What you say
about the N3 radical, where the ejection of one nitrogen atom impacts another N3, merely describes a chain reaction. However, the majority of chain
chemical reactions occur without detonation, so IMO this explanation is not sufficient to account for the behavior of primaries.
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I was under the assumption that this chain reaction with a lone reactive nitrogen for each molecule that decomposes multiplied by the billions of
individual molecules present even in a small amount would trigger a chain reaction in rapid time.
But, I must agree that it wouldn't explain it fully, especially when dealing with salts that are not azides.
Maybe the ability of a primary explosive to DDT in extremely small unconfined quantities is due to not one but a combination of factors that exist in
varying degrees in different types.
Theoretically it could be:
1. Enthalpy values and energy release.
2. Temperature of combustion/deflagration reaching a certain threshold.
3. Accelerating combustion/deflagration rate until velocity of speed of sound is reached.
4. Catalytic action of metal ion bonded in complex salts.
5. Knock on effect of a reactive species/ion such as with azides.
6. Adiabatic heating from instantaneous production of hot gases.
Those are just ideas at this point, I did not realise it is such an unsolved part of energetics. Very interesting.
Be good, otherwise be good at it
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