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Author: Subject: Exotic Primaries - Complex Salts
pdb
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[*] posted on 18-11-2024 at 12:50


Quote: Originally posted by Axt  
Good god pdb, it's been just shy of 20 years it's good to see you made it to 75 posts haha.


It's nice to see you're still alive and still tuned in to our favorite topic !

Quote: Originally posted by Axt  
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.


I'll try to be more explicit. It's a pyrotechnic train consisting of a segment of 2,4-dinitrobenzenediazonium perchlorate, followed by a segment of 3-nitrobenzenediazonium, and then another segment of 2,4-dinitrobenzenediazonium perchlorate. The result shows that the detonation of the 3-nitrobenzenediazonium (which bent and pierced the angle iron) did not cause the 2,4-dinitrobenzenediazonium perchlorate to achieve DDT. I had conducted other tests at the time and failed to achieve DDT.
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Etanol
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[*] posted on 20-11-2024 at 11:46


How about Copper(II) Perchlorate Complex with Aminoguanidine?
According to the "Synthesis, Structural and Energetic properties of Copper(II) Perchlorate Complex with Aminoguanidine", its thermal behavior is not much lower than that of NAP: 215°C vs 230°C.
However, I am afraid that the combination of copper and hydrazin bond will make the product unstable and dangerous.
Also, I found a youtube video with this substance. However, the author prepared not a pure substance that does not work.
I want to make a pure product without impurities of sulfate or acetate.
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[*] posted on 20-11-2024 at 13:17


Isn't example 2.4 of patent EP2450330A2 ?
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[*] posted on 20-11-2024 at 13:46


Yes, although no reference gives its extraction, whether it readily precipitates or not.

Generally if the complex is very water soluble you can use the metal sulphate and sodium salt oxidiser then run an ethanol extraction. Dissolve everything in a small amount of water, add ethanol as sodium sulphate is poorly soluble in ethanol/water it precipitates, heat to 40 degrees or so and filter while hot, cool solution down to -5 in freezer and filter the complex.

copper agn perchlorate.png - 870kB
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[*] posted on 20-11-2024 at 14:32


Quote: Originally posted by Axt  

Thank you. But apparently this is Fake. Copper aminoguanidine perchlorate cannot exist.
When trying to synthesize, aminoguanin perchlorate slowly oxidizes copper perchlorate in a Cu2O in an hot acidic environment and instantly does this in a slightly alkaline environment.
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[*] posted on 22-11-2024 at 07:03


Copper perchloride ? Such errors do not writte anyone from this forum. Text looks a like bullshit from AI.....:cool:



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[*] posted on 22-11-2024 at 10:25


Quote: Originally posted by Etanol  

Thank you. But apparently this is Fake. Copper aminoguanidine perchlorate cannot exist.


You literally just linked to another prep of it, are you saying they are both lying and are both "fake".

The other is a google image translate of the patent.

Screenshot 2024-11-23 051022.png - 261kB
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[*] posted on 23-11-2024 at 09:02


The time has come when you can't believe everything you see with your own eyes. Another error....hemesulfate ....Yes, aminoguanidine hemisulfate exist: https://pubchem.ncbi.nlm.nih.gov/compound/Aminoguanidine-hem...:cool:



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[*] posted on 14-12-2024 at 02:15


Quote: Originally posted by dettoo456  
Anyone had experience with Silver 5-ATz complexes such as [(2Ag)5-ATz] NO3 or ClO4?
My product crashed out of the sol immediately on addition of AgNO3 to the 5-ATz/HNO3 mix as an off-white precipitate that started to yellow to a pastel yellow on air drying on a filter.


In referernce to http://www.sciencemadness.org/talk/files.php?pid=689047&...

Dettoo, did you change anything from the literature procedure to make this work? I gave it a go and achieved as much as you did in this post, it just dumps the silver aminotetrazolate out as soon as the silver nitrate solution is added. Nothing like as described in the article.

The article sems to be wrong, it uses equal molar quantities of silver nitrate and aminotetrazole thus impossible to achieve their stated 80% yield of Ag2(CH2N5)NO3.

I just went and checked the original 1972 patent (US3663553) for the perchlorate and they are using the same nonsensical molar ratio as well. Make it make sense.

[Edited on 14-12-2024 by Axt]
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[*] posted on 14-12-2024 at 06:34


I have not revisited this complex any time recently, as the product was pretty lackluster IMO (performs on the level of MTX-1). Klapotke has a stellar reputation regarding EM synthesis methods as well, so I don’t know why this particular preparatory method from him seems so finicky. I’m assuming the amphoteric nature of the 5-substituted tetrazoles is what is causing these inconsistencies. pH control is likely more important in this case than I guessed.

On page 3 of the article you linked, the authors notice that the complexes are “ are extremely insoluble in every common solvent, and only dissolve in concentrated acid solutions (e.g., hydrochloric, nitric, or perchloric acid) to form the corresponding 5- amino-1H-tetrazolium salt (chloride, nitrate, or perchlo- rate) in which the silver cations are no longer coordinating to the tetrazole ring”.

If I get time I can try again, though I’d currently like to mess with DPPE-1 & its Ag analogues. I’ll need to make some more HNO3 before I prep the Ag 5-ATz complex again :|

[Edited on 14-12-2024 by dettoo456]
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[*] posted on 14-12-2024 at 10:52


As I posted that it was stirring so I just threw an extra molar equivalent of silver nitrate into it. It actually did get near 100% yield, 3.6g by using 0.02mol AgNO3 and 0.01mol 5-ATZ but it's no more energetic, just sputters with an energetic puff now and then. I can't say this was comparative to MTX-1 which will at least POP. I'll just throw this one in the bin of failures.

I really wanted a nitrate to work, I tried "DAN-2" the nitrate perovskite but I wouldn't even class it as an energetic, barely burns. DAP-2, DAP-4 and DPPE all follow their prep details well though, instantly dropping out of solution as small cubes. I cannot quantify their sensitivity but it's much more than the articles state.

I'm looking at copper aminotriazole chlorate with mild interest. Only if its soluble in ethanol enough to extract it from the sulfate as I'm not using barium chlorate.

[Edited on 14-12-2024 by Axt]

Attachment: copper aminotriazole chlorate.pdf (725kB)
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[*] posted on 14-12-2024 at 14:01


The DPPE-1 I trust to at least perform, as another member here shared some of his experience in preparing it along with showing properties. I made what I thought to be the K-DABCO-ClO4 too, though that burned about as well as black powder (like you mention with the DAN-2). I have around 500g of DABCO though, so those perovskites are more enticing at the moment than tetrazole complexes.

I may try a CuAG-IO4 complex now that I think about it, may be an interesting alternative to NAP if it hasn’t already been tried and found to be shit.

[Edited on 14-12-2024 by dettoo456]
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[*] posted on 16-12-2024 at 12:36


Quote: Originally posted by dettoo456  
The DPPE-1 I trust to at least perform, as another member here shared some of his experience in preparing it along with showing properties. I made what I thought to be the K-DABCO-ClO4 too, though that burned about as well as black powder (like you mention with the DAN-2). I have around 500g of DABCO though, so those perovskites are more enticing at the moment than tetrazole complexes.

I may try a CuAG-IO4 complex now that I think about it, may be an interesting alternative to NAP if it hasn’t already been tried and found to be shit.

[Edited on 14-12-2024 by dettoo456]


I'd be happy to be proven wrong, but I don't think copper will form complexes with periodate. I have tried it with ethylenediamine and ammonia and only received what I took for copper periodate (I'm sure that can be easily tested, but I haven't). Light green powder that when ignited It would smoulder through the mass releasing a bit of iodine smoke.

The potassium DABCO perchlorate and its ammonia analogue burn more like some type of rocket fuel. Potassium DABCO nitrate I would have loved to be a blackpowder like propellant, but as best I can determine just turns black and splutters a bit.
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[*] posted on 18-12-2024 at 14:52


Quote: Originally posted by Axt  
Quote: Originally posted by Etanol  

Thank you. But apparently this is Fake. Copper aminoguanidine perchlorate cannot exist.


You literally just linked to another prep of it, are you saying they are both lying and are both "fake".

The other is a google image translate of the patent.


There is a thread on this, where the user compares it to NAP.
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[*] posted on 18-12-2024 at 14:53


Quote: Originally posted by Axt  
Quote: Originally posted by Etanol  

Thank you. But apparently this is Fake. Copper aminoguanidine perchlorate cannot exist.


You literally just linked to another prep of it, are you saying they are both lying and are both "fake".

The other is a google image translate of the patent.


There is a thread on this, where the user compares it to NAP.
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[*] posted on 3-1-2025 at 01:19


I have been evaluating ZnCP as a primary for indoor testing due to concerns over the potential production of nickel carbonyl gas when using nickel based primaries such as NAP, NHN or NiCP (NAP is IMO still the state of the art primary where good ventilation is possible, or outdoors).

I have prepared ZnCP in a number of different ways, but while the substance seems to be ZnCP, I'm not impressed with its power. For this reason I wanted to ask here, if anyone has prepared ZnCP and has some experience with it.
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[*] posted on 3-1-2025 at 22:24


I've no answer Microtek but are you making the carbohydrazide yourself? The only accessible literature route I see is cyanuric acid + hydrazine hydrate (40% to 100% concentration), the prep seems quite trivial. US3258485.

The only zinc salt I can remember making was Bis(ethylenediamine)zinc(II) Bromate (possibly tris) which would flash on ignition, with notably less vehemence than the copper analogue which would go off with a bang. The zinc complex that did catch my attention was the tetrakis(DMSO)zinc(II) perchlorate complex, anhydrous and melts at about 70 degrees. No explosive properties mentioned although the silver analogue is said to be the most violent and dangerously explosive.
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[*] posted on 4-1-2025 at 02:39


I'm using commercial carbohydrazide, and it has worked as expected in other syntheses such as NiCP (which is almost as good as NAP) or CoCP. The reason I was going for ZnCP apart from the low toxicity is that reportedly, the chinese have begun using this material in their caps. One explanation could be that they use a large amount of primary, maybe 200-300 mg in a cap. Another could be that they use it in conjunction with something else, much like the common LA/LS mix.
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[*] posted on 4-1-2025 at 05:20


This report seems to affirm your experience. Co and Ni Fired, Zn did not. Although it doesn't clearly state by which manner it failed, it reads as if it didn't ignite.

Attachment: Ni Co Zn carbohydrazide complexes.pdf (410kB)
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[*] posted on 5-1-2025 at 23:29


It might be worth converting the carbohydrazide to urazine and complexing that, if only for experimentation. Urazine is highly dense and purported to be the highest VOD, urazine perchlorate salt at 9799m/s @ 2.12g/cm3. Urazines prep is online in https://sites.lsa.umich.edu/jbuss/wp-content/uploads/sites/8... , page 29 (it's just heating carbohydrazide with HCl). It's perchlorate salt and copper complex is given here https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002... .

I threw some a small amount of hydrazine and cyanuric acid together, held at 110 degrees the past 36hrs and received what I believe to be a poorly soluble portion of hopefully urazine and a larger portion of hopefully carbohydrazide. Definitely buy it if you can, surely the better option to distilling hydrazine but the patent seems to work.

carbohydrazide 1.png - 2MBcarbohydrazide 2.png - 2.1MB
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[*] posted on 6-1-2025 at 01:01


I was experimenting with the urazine derivatives some time ago, but found that the perchlorate, while very powerful indeed (and also very sensitive), was too hygroscopic for most uses. I did do a little work on urazine complexes, but nothing systematic as that wasn't my focus at the time. I didn't find anything worthwhile to report.

On a side note, the major byproduct of the carbohydrazide to urazine reaction is hydrazine hydrochloride. I tried adding 50% sulfuric acid to the filtrate, and did receive large amounts of white precipitate that is probably hydrazine sulfate (though I haven't analysed it properly). If so, the reaction is efficient enough that it could be a valid alternative to the usual amateur pathway to HS (if you can buy carbohydrazide).
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[*] posted on 6-1-2025 at 03:29


Yeh I should have searched the forum for urazine, you've mentioned it a couple times before. Can you comment on the isolation of the salt? there's no details in the article and presumably it's pretty soluble.

What about the solubility of the ZCP? does it precipitate from water or other?
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[*] posted on 6-1-2025 at 11:32


UzP is very soluble. I isolated it by reacting with a stoichiometric amount of perchloric acid and then evaporating the water at elevated temperature.

ZnCP is not very soluble in cold water, but fairly soluble in boiling water. In the method I followed, the reactants are combined (dropwise addition of CHZ soln to Zn2+ / ClO4- soln) which precipitates the product. Then temp is raised to reflux which redissolves the ZnCP. The temp is then allowed to come to 10C (or just room temp) with stirring to crystallize the product in a slightly less fine morphology.
As far as I can tell, there is no reason to go to the trouble of preparing ZnClO4, any soluble Zn(II) salt along with a soluble perchlorate will give the same product.
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[*] posted on 7-1-2025 at 06:45


Quote: Originally posted by Microtek  
As far as I can tell, there is no reason to go to the trouble of preparing ZnClO4, any soluble Zn(II) salt along with a soluble perchlorate will give the same product.


Have you tried many other salts? Mixing my putative carbohydrazide with zinc sulphate results in immediate precipitation, I don't know if you can confirm the insolubility of the sulphate with the commercial grade or not.

Mixing it with silver nitrate also produces an immediate white precipitate, this is unstable and seems to reduce to silver when drying. Adding the wet white product to hot water immediately turns it black/brown.
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[*] posted on 7-1-2025 at 09:12


No, I just tested it by dissolving ZnO in sulfuric acid and adding a carbohydrazide soln. No precipitate was formed. Your carbohydrazide might contain some hydrazine (as the bicarbonate maybe), which could give slightly soluble hydrazine sulfate and would also explain the reaction with silver.
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