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Author: Subject: Nickel Hexamine Perchlorate success
symboom
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biggrin.gif posted on 29-3-2017 at 03:35
Nickel Hexamine Perchlorate success


I think I may have a new compound not sure after if someone could double check so ammonia is added to nickel sulfate until precipitate dissolves then hexamine is added precipitate forms again more ammonia is added to dissolve precipitate then ammonium perchlorate is added and a purple percipitate forms just like tetramine nickel perchlorate without hexamine yet this time it burns faster like flash powder blinding red flash instead of the black powder like burn which for nickel thats odd to have a red flash of flame





Update on copper hexamine perchlorate

So this procedure is tricky laboratory of liptakov has synthesized he used to have a video on it :-(

His procedure is first to make tetramine copper perchlorate
Ammonium perchlorate and tetramine copper hydroxide is used to form this

Needs lots of ethanol to precipitate maybe a different solvent could precipitate it better

Next ammonium hydroxide and hexamine powder is added with tetramine copper perchlorate

I have been thinking of ways around this over the need of ethanol although the precipitation of the first reagent does lessen the need of even more ethanol.

Possible
Perhaps hexamine could already be in the ammonium hydroxide with the tetramine copper hydroxide and ammonium perchlorate and boil off the residual ammonia to form copper hexamine perchlorate

Another procedure to form copper perchlorate is copper carbonate boiling with ammonium perchlorate to form copper perchlorate not sure if that is possible but it works for sodium carbonate and ammonium nitrate.



[Edited on 29-3-2017 by symboom]

[Edited on 29-3-2017 by symboom]
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Laboratory of Liptakov
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[*] posted on 29-3-2017 at 09:45


OK...good attempts... Nickel Hexamine Perchlorate I am yet not try it. Good described. But ethanol you not needed. For precipitate.
(because my video of prepare CHP from TACP was delete from admin, describe here again)
Second part of preparation from point HANP or TACP is dry crystals:
We insert 10g HANP into 60g 20% NH3 water.
Adding 10g hexamine. Close glass jar. (or Erlen) Heated on 50C to dissolving all crystals. This may take 5-10 minutes after reaching 40 - 50 ° C. After dissolving, we put on the table and slowly cooling on 20 C. After insert jar to freezer and cooling on - 10 or - 18C
Prepare ammonia (wet or dry) gas generator. After 2- 3 hrs Insert hosepipe to solution and bubble. Solution absorbed very easy a huge amount of NH3 gas at temperature - 10 C. Insert again to freezer on 1 hrs. After this operations we will have almost 95% weight of HANP-hex clathrate precipitated in jar. Separation on fine sieve or Buchner at temp. cca 0 - 10 C. Drying by 80 C on the inert surface. CHP (TACP-hexamine clathrate) was tested even drying process by 110 C. The mother liquour is possible use, because content about 9g hexamine and 0,5g CHP in solution. Empty solution can be storage in freezer.
....huh....:cool:...LL




Safety explosive Alfred Nobel 1867. Safely ecologic detonator Dr. Liptakov 2015.
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symboom
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[*] posted on 29-3-2017 at 12:58


So copper hexamine perchlorate does not need ethanol I think the problem is the freezer does not go low enough
I added ammonium perchlorate last because of precipitation of tetramine nickel perchlorate I wanted to avoid.

Interesting burn tests
Purple solid melted into dark green solid then a pop with a bright flash what could have happened is I drove off the ammonia which could be left over
More tests needed. Im hypothesizing from the observations
There is a big difference between the black powder burn and the flash powder burn of hexamine nickel perchlorate and tetramine nickel perchlorate


Havnt tried yet
This might be another path
If nickel perchlorate is added to hexamine forms hexamine sulfate and precipitate of nickel hydroxide more hexamine is added forming hexamine nickel perchlorate

Nickel perchlorate synthesis nickel tartrate and ammonium perchlorate heat to drive of ammonium tartrate?

[Edited on 29-3-2017 by symboom]
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[*] posted on 29-3-2017 at 14:38


Is impossible compare BP and metal ligands of perchlorate. Small heap on air is not relevant properties. It is as compare dinitrate of cellulose and HMTD. In solid cavity is maximal speed BP 380 m/s. But perchlorate ligands, especially with hexamine have transfer to detonation on speed over 6000. For copper hexamine perchlorate (shortly CHP) was measurement 7400 - 7600 m/s at density 1,91g/cm3. Respectively detonation pressure 25 GPa. CHP has incredible power even in diameter 4,3 mm. And crossing from deflagration to detonation /DDT/ in long 5 mm ( in cavity.)



Safety explosive Alfred Nobel 1867. Safely ecologic detonator Dr. Liptakov 2015.
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[*] posted on 29-3-2017 at 15:54


Be careful with the names you use...it brings confusion.

Hexamethylenetetramine is C6H12N4 and is sometimes shortened as Hexamine (HEX) or is refered to as tetraazaadamantane.

But Copper tetramine perchlorate or chlorate are Cu(NH3)4(ClO3)2 and Cu(NH3)4(ClO4)2.
and
Nickel hexamine perchlorate or chlorate are Ni(NH3)6(ClO3)2 and Ni(NH3)6(ClO4)2 (not tetramine!!!)

When playing with hexamethylenetetramine (hex) ligand better not call it hexamine into this context.
LL had once posted the documentation about those hexamethylenetetramine complexes...but when making them from Cu(NH3)4(ClO4)2 or Ni(NH3)6(ClO4)2 and HEX...the HEX expell a NH3 to take its place...so in fine you may get hybrid complexes or a mix of complexes...
--> Cu(NH3)3(HEX)(ClO4)2; Cu(NH3)2(HEX)2(ClO4)2
--> Ni(NH3)5(HEX)(ClO4)2; Ni(NH3)4(HEX)2(ClO4)2
The number of HEX ligand is limited owing to their bulkyness.

Main problem with HEX is that it has 4 possible complexing nitrogens so the number of HEX is not wel defined and actually two adjacent metalic core may share the same hexamine ligand (tetraazaadamantane).
Also when starting from pure Cu(ClO4)2 and Ni(ClO4)2 and mixing with HEX one gets (IIRC from LL provided paper) Cu(HEX)(ClO4)2 and Ni(HEX)2(ClO4)2...thus without NH3...adding NH3 will in principle generate hybrid complexes "Amino"-"HEX"

On futher attempts/investigations one should investigate the mixing of HEX.HClO4 and HEX.2 HClO4 instead of HEX alone in a way to improve oxygen balance and explosive power.

Also to investigate the possibility of Ni(3+) perchlorates --> Ni(ClO4)3 --> Ni(NH3)6(ClO4)2 and HEX; HEX.HClO4 and HEX.2 HClO4 cocomplexes...

Finally worth to try also Co(ClO4)2, Co(ClO4)3, Fe(ClO4)3, Zn(ClO4)2, Cd(ClO4)2, Mn(ClO4)2, Mn(ClO4)3, AgClO4 and Ba(ClO4)2, Ca(ClO4)2 and Sr(ClO4)2 (Ca, Sr and Ba are able to hold NH3 gas in a kind of complexation state...for example CaCl2 is able to catch/store NH3 gas and to release it upon heating)

[Edited on 30-3-2017 by PHILOU Zrealone]




PH Z (PHILOU Zrealone)

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