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Author: Subject: Exotic Primaries - Complex Salts
Bear_with_vodka
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[*] posted on 16-1-2010 at 08:25
[Cu(en)2]3[Co(NO2)6]2


Hi everyone. First, please forgive my rusty english :(
I can’t find anything about this odd complex in literature, any advice?
It was made by the reaction of somewhat concentrated warm solutions of Na3[Co(NO2)6] and [Cu(en)2](NO3)2, using stechiometric amounts. The mixture was brown and… nothing happened. But after 5-10min glistening small needles started to separate. After 2 hours the solution was light-brown with heavy crystals on the bottom. It was filtered, the crystals washed with cold water and dried at room temperature.
Dark-brown small needles, very sparingly soluble in water, non-hygroscopic, decomposes fiercely at ~150C, does not decompose with applied friction or strike, looks stable in air.
Small 300mg pile was ignited. It burned fast, but smooth and quiet with ~15cm high yellow-orange flame with a little light-green at the end without smoke and smell. There was a lot of black residue.
I know nothing about corresponding NH3 complex as it does not precipitate.

[Cu(en)2](NO3)2 was made by adding ethylenediamine into warm conc. solution of Cu(NO3)2 – from copper wire and 70% nitric acid (neutralized with a little NaHCO3 in the end). Beautiful big dark-violet plates. They melt in a spoon on the torch, then burn with a light-blue flash with loud fizzing.
The hydrazine complex of Cu(NO3)2 is very unstable. It’s an amorphous light green powder, which turns black after a few minutes, so it’s impossible to isolate it…


it's better to take cold, not warm solutions - that increases yield

one more edition:)
just finished another reaction... total failure:(
Both solutions were room temp. The mixture turned dark-green and a little of colourless gas evolved... 10min after - it started to smell intensively, very strange unpleasant smell
It was filtered in a gasmask (as I'm afraid of nitrosoamines, who knows what's in there...) The yield this time was 10% AND the compound burned much slower:(
Why so? But more interesting - what's the smell??

[Edited on 16-1-2010 by Bear_with_vodka]
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[*] posted on 17-1-2010 at 03:42


I'll just keep talking to myself then:)
This time two solutions were cold, below zero. They were mixed and left outside for the night (-12 or so). The yield was 50% of nice quite big heavy crystals, cubic this time.
Now then, I'm not so sure about the right formula of complex as it is essencial to use excess of cobaltinitrite otherwise the stinky green solution is formed.




влажный комплекс2.jpg - 252kB

slightly wet

[Edited on 17-1-2010 by Bear_with_vodka]
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Evilblaze
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[*] posted on 17-1-2010 at 05:33


Quote: Originally posted by Bear_with_vodka  

[Cu(en)2](NO3)2 was made by adding ethylenediamine into warm conc. solution of Cu(NO3)2 – from copper wire and 70% nitric acid (neutralized with a little NaHCO3 in the end). Beautiful big dark-violet plates. They melt in a spoon on the torch, then burn with a light-blue flash with loud fizzing.
The hydrazine complex of Cu(NO3)2 is very unstable. It’s an amorphous light green powder, which turns black after a few minutes, so it’s impossible to isolate it…


[Edited on 16-1-2010 by Bear_with_vodka]


Wow, I'm happy to read this. I tried similar things in last month. At me Cu(ClO4)2 was used instead of the Cu(NO3)2, but I had similar results. The Cu-perchlorate solution with ethylenediamine gave a purple/pink solution. I just didn't had time to wait until it crystallizes so I thrown it out (but I will make it again soon).

But with the hydrazine it gave a really good complex. It is unstable until it is not dry. I made the complex quick, I waited for 10 minutes to participate (I added some alcohol, it made this quicker). I just filtered it fast, I washed it twice with water and twice with IPA. It was dried at 40 Celsius and it was used. I just have a small sample from this. The sample is 1 month old and there is no problem with it. If I ignite a small piece it just work's correctly. I think it is a really good complex salt :D

I will also try with the Cu(NO3)2. I think your solution was a bit acidic because of the nitric acid and maybe this caused the "color change from green to black".

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Bear_with_vodka
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[*] posted on 17-1-2010 at 05:52


hydrazine-hydrate-copper-perchlorate
Great thing! It does not burn but detonate.
I always wanted to make it, but I don't have HCLO4 :(
And there is no way of making that complex without HCLO4, am I right?
And yes, you have to wait after adding ethylendiamine. Just put it in the refregirator for a night. Thats about [Cu(en)2](NO3)2, maybe CLO4 complex is more soluble, I don't know

The only CLO4 complex I had made is [Ni(NH3)6](ClO4)2. It is insoluble, so the preparation is very easy. NiSO4 solution + NH3aq = deep-blue solution + NaClO4 solution = immediate light-blue-violet amorphous precipitate. It burnes violently with flashes.
[Ni(N2H4)2(3??)](NO3)2 is also insoluble (light green), but I think it's not interesting at all. Hard to burn it.

[Edited on 17-1-2010 by Bear_with_vodka]
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Evilblaze
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[*] posted on 17-1-2010 at 06:03


Quote: Originally posted by Bear_with_vodka  

I always wanted to make it, but I don't have HCLO4 :(
And there is no way of making that complex without HCLO4, am I right?


No! I made it from NaClO4 and CuSO4. NaClO4 or KClO4 can be obtained easier than HClO4. KClO4 = pyrotechnic supply shop;)
The only thing that you have to do is to wash it with water twice to get out the NaCl/KCl, because if the salt is in the mix, it won't detonate, it will just burn really quick, but no bang:D

Long ago I made a complex of hydrazine perchlorate (hyrdrazine hydrate and HClO4) and CuCl2. It was also a really good explosive, but it was not so stable as the hydrazyne hydrate -copper perchlorate complex (what is actually the BEST!).

I got some methylamine solution on the shelf.... Maybe I will try a complex with that too.....:D

[Edited on 17-1-2010 by Evilblaze]
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[*] posted on 17-1-2010 at 06:23


Evilblaze I had a virus warning when I DL'ed your video (Conficker worm).

AFAIK Copper(II)nitrate dissolves quite well in EtOH, so you could try to make the complex in almost water-free enviroment (Cu(NO3)2 comes in hydrated form however).

Copper(II)perchlorate is insoluble in EtOH tough.

Interesting to see that the hydrazine complex is reasonably stable. I tought they would be way too dangerous to make. From looking at your video I'd say its similar to the nitroaminoguanidine complex I described previously. It deflagrates *very* quickly, sort of on the verge to making DDT even in smallest amounts. It gives a dull report but not the high pitched bang you get when it is smacked with a hammer. Try wrapping in a few layers of aluminium foil, it should DDT even in minute amounts.

en-copper(II)-perchlorate crystallizes in *beautiful* dark purple needles. I made these by adding ethylenediamine to a cold solution of copper perchlorate, then boiled down to half its volume, added an equal volume of EtOH and put in the freezer. Even when quickly cooled down the solution deposits crystals of impressive size. It can be made anhydrous by carefully heating with warm air; the dark purple crystals then desintegrate into a pale light pink powder which is quite sensitive to impact.

[Edited on 17-1-2010 by Taoiseach]
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[*] posted on 17-1-2010 at 06:31


@Bear_with_vodka

>[Ni(N2H4)2(3??)](NO3)2 is also insoluble (light green), but I think it's not interesting at all. Hard to burn it.

Something must be wrong with your hydrazine. An ethanolic solution of nickel(II)nitrate upon addition of hydrazine *immediately* precipates light pink microcrystalline powder of [Ni(N2H4)3](NO3)2. This compound deflagrates violently upon ignition, also giving a dull report. It makes DDT *very* easily. Just the confinement from a few layers of aluminium foil is sufficient to make it detonate. I dont know what the green stuff is you described, possibly just hydrated nickel nitrate.
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[*] posted on 17-1-2010 at 06:34


Quote: Originally posted by Taoiseach  
Evilblaze I had a virus warning when I DL'ed your video (Conficker worm).


Virus? What the....? The video was recorded half month ago, I just made 1 video from 4 with windows movie maker and that's all. Who packed a virus in it?

Quote: Originally posted by Taoiseach  
Try wrapping in a few layers of aluminium foil, it should DDT even in minute amounts.


In aluminum foil with a hammer it ignites from a 8cm drop. The hammer weighted 140g.

It is not really stable to use it in larger amounts, but it was interesting to make it and test it.
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[*] posted on 17-1-2010 at 06:47


[Ni(N2H4)3](NO3)2
*looking at notes*
aarrr... yes it's light-pink, sorry
I had only about 200mg, it burned with very small flashes-strikes and I didn't like it))


[Edited on 17-1-2010 by Bear_with_vodka]
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[*] posted on 17-1-2010 at 07:14


@chemolo

>Very nice!
>I don't like the method of drying the sample with NaOH (to remove HClO4), at least use KOH!
>Why do you need 80 deg C for reaction (complexation) of NAG with copper perchlorate?

The complex seems to be quite soluble in water. Thats why I wanted to minimized amount of water and used hot saturated solutions.

>Impressive that the Cu-NAG-ClO4 crystals are stable at air! That is very unusual!

The reasoning was that if hydrazine complexes of perchlorate are unstable, maybe the condensation product of hydrazine with nitroguanidine would be more stable. Also I figure that the bromate complex would DDT even easier - comparing en-copper-perchlorate (deflagrates) with en-copper-bromate (detonates in smallest amounts). Unfortunately it is quite temperature sensitive and cannot be made from hot saturated solutions.

>Pb(C6H2N3O7)2 - please clarify for the uninformed what it is.

Well think about it: C6 suggests a benzene ring, the N3O6 amount for 3 nitro groups. Its lead picrate :D
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[*] posted on 17-1-2010 at 07:22
[Cu(en)2]3[Co(NO2)6]2 or something...


when completly dry, it decomposes without flame:(
just somewhat stupid decomposition, although there a lot of gas
200mg


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[*] posted on 17-1-2010 at 07:52
[Cu(en)2](NO3)2


forgive the dirty bowl:)
100mg overall

Attachment: copper en no3.avi (1.2MB)
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Burning of _finely_powdered_ [Cu(en)2]3[Co(NO2)6]2 is much more fun:D
250mg



Attachment: Cu-Co.avi (666kB)
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666kB:D


[Cu(en)2](ClO4)2
if I'm bothering with those small videos, feel free to tell me that:)
200mg, finely powdered



[Edited on 18-1-2010 by Bear_with_vodka]

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[*] posted on 30-1-2010 at 12:45


Concerning the lead chlorate complexes, I have to report that a mixture of lead(II)acetate, sodium chlorate and glycerine doesn't precipate shit upon addition of ethanol :( The patent maybe isn't complete bullshit but likely you have to start with lead(II)chlorate to form these complexes :(
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[*] posted on 31-1-2010 at 06:46


I tried making Ni(NH3)6(ClO4)2 as mentioned further above in this thread. I found that making this compound is more succesful if the solutions are not too strong.

I did two experiments.

In the first experiment I added excess 5% ammonia to a solution of nickel sulfate. This gives a blue/purple solution. To this I added a fairly dilute solution of ammonium perchlorate, but not enough to precipitate all of the nickel complex. When this is done, then at first nothing seems to happen, but after a few seconds the solution turns opaque and then quickly a glittering crystalline precipitate settles at the bottom. The crystalline precipitate is compact and can easily be separated from the liquid, simply by decanting the liquid from the precipitate. The liquid above the precipitate still is pale blue/purple. I also could easily rinse with some cold distilled water and I obtained a light blue/purple solid. The rinse-water also was pale blue.

In the second experiment I added a slight excess of 5% ammonia to a solution of nickel sulfate. This gives a blue/purple solution. To this I added a fairly large excess amount of a moderately concentrated solution of ammonium perchlorate. This results in quick formation of a slimy precipitate which only settles very slowly. The liquid above the precipitate is completely colorless. Even after a hour the precipitate still did not settle (still appr. 60% of liquid contained the precipitate). I did not attempt to isolate this slimy precipitate, it simply is too much of a hassle.

The other crystalline batch was dried and tested in a flame. The dry material easily can be ignited and it burns very fast with only moderately strong light output and a hissing sound. Only a little amount of smoke is produced.

Personally I find this nickel-complex moderately interesting. It is energetic but it is not really impressive.




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[*] posted on 22-6-2010 at 21:25


Unsymetric dimethylhydrazine perchlorate mixed with Au(ClO4)4- anion dissolved in an inert ionic liquid, might form a coordination complex. Au(ClO4)3 would precipitate, the extra ClO4- makes it soluble. The protonation of the amine group and the two methyl groups on the other side should protect the hydrazine from oxidation by the gold compound. Although Au(ClO4)3 is a sensitive explosive, the complex with the DMhydrazine should sterically hinder any interaction of the Au+3 with the perchlorates, greatly stabilizing the perchlorates. This would be an extremely powerful salt.
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[*] posted on 24-7-2010 at 17:08


How do you make TACPC (Tetraminecopper(II) Perchlorate

I have CuO, CuSO4, NH3, and NH4ClO4

Thanks
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[*] posted on 26-7-2010 at 01:05


TACP is badly soluble in EtOH so you could try

CuSO4 + 2NH4ClO4 + 4NH3 ---(ethanol)---> [Cu(NH3)4](ClO4)2 + (NH4)2SO4

Any other route would involve making copper(II)perchlorate first. Unfortunately I dont see how you can make this compound starting with NH4ClO4. Ammonium carbonate decomposes at 60-70°C thus

2NH4ClO4 + CuCO3 ---> (NH4)2CO3 + Cu(ClO4)2 ---> NH3 + CO2 + H2O + Cu(ClO4)2

seems possible at first glance. However I'm afraid that boiling copper carbonate with ammonium perchlorate will simply ecompose the copper carbonate into black copper(II)oxide.
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[*] posted on 26-7-2010 at 01:40


What about tetraminecopper(II) persulfate

Saw a video once bout it wasn't in english.

I have ammonium persulfate but can make sodium persulfate if needed
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[*] posted on 26-7-2010 at 03:11


Doesnt matter if u use sodium or ammonium persulphate. You could easily make this compound from the chemicals u have but I'd advise against it. The complex is very unstable and decomposes within a few weeks. Storing in a glass bottle is potentially hazardous. The compound dehydrates easily in warm air, and then it is becomes a very sensitive and unstable low-powered explosive. To sum it all up: its useless dangerous crap.

Try precipating TACP with ethanol, I guess it'd work. This complex is stable, stores indefinetly. It comes in hydrated form and is absolutely safe to handle. When dehydrated it is quite powerful and sensitive tough; according to literature it has initiating power.
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[*] posted on 26-7-2010 at 14:11


TACP is tetraminecopper(II) perchlorate not persulfate right?

I'll try making it when I come home.
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[*] posted on 27-7-2010 at 15:52


Quote: Originally posted by mewrox99  
How do you make TACPC (Tetraminecopper(II) Perchlorate

I have CuO, CuSO4, NH3, and NH4ClO4

Thanks


This compound is pretty simple to make. First react copper sulfate with excess of ammonia to get solution of [Cu(NH3)4]SO4, product can be separated by adding several volumes of ethanol.

CuSO4(aq.) + 4NH3(aq.) => [Cu(NH3)4]SO4(aq.)

Sulfate can be easily replaced by perchlorate by action of Ca/Sr/Ba perchlorates, witch can be easily produced by dissolving corresponding oxide/hydroxide/carbonate in commercially available perchloric acid and evaporating solution to dryness. Dissolve some pure tetramminocopper sulphate in water and add solution of Ca/Sr/Ba perchlorate, corresponding sulphate will be precipitated leaving pure solution of tetraaminocopper perchlorate:

[Cu(NH3)4]SO4(aq.) + Ba(ClO4)2 => [Cu(NH3)4](ClO4)2(aq.) + BaSO4 (precipitate)

Evaporation of this solution will give you pure tetraaminocopper perchlorate.




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[*] posted on 1-8-2010 at 10:28
DACP


DACP supposedly stands for "double azido cobalt perchlorate", the correct formula is trans-tetraamminediazido-cobalt(III) perchlorate [(NH3)4(N3-)2Co(3+)](ClO4-). Whats interesting about this complex is the fact that it contains azide ligands, fuel and an oxidizer in a single compound.

It is briefly investigated in a freely available paper "Lead Azide Replacement Program NDIA Fuze Conference" by Bichay and Hirlinger. It is also discussed in more depth in several Chinese publications. I cannot download nor understand these papers but the google translation of the abstracts gives some valuable hints. The compound is a powerful initiating explosive with properties comparable to BNCP (bis-nitrotetrazolate-cobalt-perchlorate) and has been proposed as replacement for both BNCP and lead azide.

A German paper "light absorption of azido-cobalt-ammines" is available in reference section and sheds more light on this family of complexes.

Experimental:

2,6ml 70% perchloric acid was neutralized with basic cobalt carbonate and filtered. Another 1ml of perchloric acid was neutralized with ammonia and the solutions combined. The resultung solution was a light magenta color .

In another beaker, 4g sodium azide was dissolved in 50ml water and 9ml 25% ammonia was added with stirring. The solutions where then combined. Complexation occured, as evidenced by deep blue coloration of the liquid.

A stream of air was then drawn through the solution for 3 hours. During this time the color changed from a deep blue to a lavender color. After standing for several hours, a microcrystalline powder had settled which was filtered and air dried.




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[*] posted on 1-8-2010 at 11:35


Did you make the compound yourself? Is this picture from a sample you made yourself? It sounds quite interesting. I however am missing a test on its sensitivity and explosive properties (such as igniting the compound or trying to hit with a hammer).

I'll consider doing the experiments at a small scale (I have all required chemicals and could do the experiment at a 10 times smaller size for safety), but if you have done the experiment yourself then some extra tips from you are welcomed.

[Edited on 1-8-10 by woelen]




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[*] posted on 1-8-2010 at 12:04


Yes I made this very small sample myself. The compound is almost insoluble in water so preparation was a breeze. It is annoying to filter tough; probably it is a good idea to heat the solution and cool down slowly to grow larger crystals.

The first time I tried the reaction I tried to use H2O2 to oxidize the Co(II). This works nicely to make other cobalt(III) complexes. In this case however it turned the solution dark-brown and the resulting precipate was not explosive (tough it did burn). I figure H2O2 destroys the complex and air must be used for its preparation.

As for explosive properties: It can be handled safely IMHO. I tested friction sensitivity and it is very low. It crackled a bit when rubbed with the head of a hammer on concrete ground but even picric acid does that. Flares off upon flame contact. The wee bit of confinement given by a few layers of aluminium foil make it DDT in smallest amounts.

I believe this is a very interesting class of energetic coordination compounds. DACP is very badly soluble and thus there is a good chance it can be prepared from a soluble cobalt(II) salt, any soluble perchlorate and sodium azide. I believe the bad solubility is partly due to the perchlorate ion. For example, hexamminecobalt(III)perchlorate, hexamminecobalt(II)perchlorate, hexamminenickel(II)perchlorate, pyridinecopper(II)perchlorate are all insoluble in water, and tetramminecopper(II)perchlorate is badly soluble in cold water.

It might be possible to form similar azido-cobalt(III)-perchlorate complexes with more energetic fuel kind of ligands. Hydrazine, hydroxylamine, aminoguanidine, nitroguanidine, nitraminoguanidine pop to mind...
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[*] posted on 1-8-2010 at 23:55


Quote: Originally posted by Taoiseach  
Unfortunately I dont see how you can make this compound starting with NH4ClO4. Ammonium carbonate decomposes at 60-70°C thus

2NH4ClO4 + CuCO3 ---> (NH4)2CO3 + Cu(ClO4)2 ---> NH3 + CO2 + H2O + Cu(ClO4)2

seems possible at first glance. However I'm afraid that boiling copper carbonate with ammonium perchlorate will simply <d>ecompose the copper carbonate into black copper(II)oxide.


A solution of Copper Perchlorate can easily be boiled without any decomposition, it will not even be oxidizing. Ammonium Carbonate begins to decompose when mixed with water, let alone being heated in water, so it is fairly safe to say that the solution need not even be boiled, just heated. Your reaction seems very reasonable. I have made Cu(NO3)2 this way.

"Ammonium bicarbonate decomposes at 36 to 60 °C into ammonia, carbon dioxide and water vapor in an endothermic process (as it is with many ammonium salts) and so causes a drop in the temperature of the water." (wiki)

[Edited on 2-8-2010 by Hoveland]
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