Sciencemadness Discussion Board - Nickel Hexamine Perchlorate success

Nickel Hexamine Perchlorate success

symboom - 29-3-2017 at 03:35

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]

Laboratory of Liptakov - 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

symboom - 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]

Laboratory of Liptakov - 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.)

PHILOU Zrealone - 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)3 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]

symboom - 22-6-2017 at 18:35

Here is the picture the green is Hexamethylenetetramine (fuel tablet hexamine) complex and the purple is hexamine the ammonia complex of nickel they both kept comming out of solution maticulously had to separate tested chunks that were all green

Finally, no I was having problems uploading kept stalling I added select picture and when I clicked edit It did nothing always had problems like that uploading pictures
I know two types ended up mixed but the green is also just as energetic about the same inspiration comes from LLs video on
Copper Hexamethylenetetramine Perchlorate

[Edited on 24-6-2017 by symboom]

[Edited on 24-6-2017 by symboom]

[Edited on 24-6-2017 by symboom]

Laboratory of Liptakov - 23-6-2017 at 08:53

HUh...Very interesting, that can arises much types of hexamine - copper - perchlorate variants. According reaction conditions, especially how diluter is used. Neutral, or ammonia water and concentration and next reaction conditions, teperature, speed of crystallisation and maybe 10 next conditions. Any way....hit on the anvil....

...LL

PHILOU Zrealone - 23-6-2017 at 12:59

Quote: Originally posted by symboom

Here is the picture the green is hexamine and the purple is tetramine

[Edited on 23-6-2017 by symboom]

[Edited on 23-6-2017 by symboom]

I suppose that when editing your post you erased by mistake the pictures...nothing to be seen now...could you repost the pictures?

PHILOU Zrealone - 26-6-2017 at 00:26

Nice thank you for the edit with the pictures now.

Strange phenomenon that two color display...could also be due to:
-hybrid complexes amino-hexamino Ni(NH3)x(HEX)y(H2O)z(ClO4)2
-critsallo-solvato-chromism...a single complex is loosing or H2O or NH3 and thus leads to different complexes and colors...or to a wel defined specific complex.
This is observed with some Co(2+) complexes that are thermochrome and moisturo-chrome and passes from blue to pink...this is used into kitten pee absorbing sand/silica gel to visually see when the sand is saturated and will no more catch moisture...same into lab drying silicagel beads....then oven...switch to the other color ensure visual control of dryness for reuse as dessicant.

LoL had put somewhere onto this forum a paper or a link to a pdf article about transition metals Hexamine complexes and energetic behaviour...the Nickel one was into it...I don't have my full document datas at hand...thus hard to provide you more precise info. But Ni was less energetic than Cu...eather Cu is a better catalyst or its lower amount of ligands makes it display a better OB and thus more power. Bert was quite enthousiatic about it but unhappy/disapointed for sensitivity data missing into the article IIRC.

[Edited on 26-6-2017 by PHILOU Zrealone]

symboom - 26-6-2017 at 02:37

Precisely LLs Copper Hexamino perchlorate is more powerful I was expecting the green nickel complex to be just as powerful as it is about the same both complexes are insouble In ammonia and water I would like to see articles on Energetic
Amine and oHexamine
Complexes with
Zn (I)
Cr(III),
Co(III),
Ni(II),
Cu(II)

[Edited on 26-6-2017 by symboom]

Laboratory of Liptakov - 26-6-2017 at 14:18

Really should be tested this: Aminoguanidine Nickel Perchlorate and Aminoguanidine Copper Perchlorate. Nickel is usually weaker than copper. Of course, that problem is availability of aminoguanidine against hexamine. But properties from patent are incredible.

https://encrypted.google.com/patents/EP2450330A2?cl=un

Next thing, what showed during testing of CHP is it, that cavity must by really solid.
Minimum is copper tube wall is 1mm. Aluminium 1mm is weak. Works steel 1mm or for rich developers, stainless steel tube. Cavity diameter usually 6 mm or 1/4" = 6,35 mm. LL.

PHILOU Zrealone - 27-6-2017 at 02:44

Quote: Originally posted by Laboratory of Liptakov

Really should be tested this: Aminoguanidine Nickel Perchlorate and Aminoguanidine Copper Perchlorate. Nickel is usually weaker than copper. Of course, that problem is availability of aminoguanidine against hexamine. But properties from patent are incredible.

https://encrypted.google.com/patents/EP2450330A2?cl=un

Next thing, what showed during testing of CHP is it, that cavity must by really solid.
Minimum is copper tube wall is 1mm. Aluminium 1mm is weak. Works steel 1mm or for rich developers, stainless steel tube. Cavity diameter usually 6 mm or 1/4" = 6,35 mm. LL.

True...
The more the container is solid/resistant, the more the confinement and thus the easier the D2D...but also the higher the powder and potentially lethal schrapnels...

Last week I was thinking that guanidine (what is more OTC-ish and quite basic...thus should complexate readily) could be interesting to test with various salts (Cu(II), Zn(II), Co(II), Fe(II), Cd(II), Ni(II), Mn(II), Co(III), Cr(III), Fe(III), Ni(III), Mn(III).../ NO3(-), ClO3(-), ClO4(-), BrO3(-), IO4(-), C(NO2)3(-), C2(NO2)4(2-), ...)

So yes aminoguanidine because related to energetic hydrazine...
But also all other related structures...that may display complexating ability...thus they must hold a NH2 or NH sufficiently basic...acidity increases with surrounding groups...double link, N atoms, NO2 groups...
-Amino guanidine --> H2N-NH=C(NH2)2
-Guanidine --> HN=C(NH2)2
-Diaminoguanidine --> HN=C(NH-NH2)2
-Triaminoguanidine --> H2N-N=C(NH-NH2)2
-Biguanidine --> (H2N)(HN=)C-N=C(NH2)2
-Nitroguanidine O2N-N=C(NH2)2
-Nitroaminoguanidine O2N-N=C(NH2)(NHNH2)
-Nitrodiaminoguanidine O2N-N=C(NHNH2)2
-Dinitroaminoguanidine H2N-N=C(NHNO2)2

One may even think about trinitromethyl based complexation agents....like:
* H2N-NH-C(NO2)3 (positive OB ligand) thus anion could be a fuel like C#N (cyanide), S(sulfide), SC#N (thiocyanate), picrate...or even an oxydiser --> super oxydiser and fuel for OB could be a plasticizer.
* H2N-CH2-C(NO2)3 (perfect OB ligand)
* H2N-NH-CH2-C(NO2)3 (slighly negative OB ligand)
* H2N-N(-CH2-C(NO2)3)2 (slighly positive OB ligand)

It may even be interesting to test for melamine based complexation agents...
*Melamine/triamino-s-triazine (-C(-NH2)=N-)3 (related to guanidine and biguanidine because cyclic triguanidine)
*Triamino-melamine/trihydrazino-s-triazine (-C(-NH-NH2)=N-)3

As explained elsewhere into this forum...the number of possibilities is as infinite as imagination and many discoveries can be done into the field of energetic transition metallic salt based amino complexes.

[Edited on 27-6-2017 by PHILOU Zrealone]

Chisholm - 27-6-2017 at 15:10

Quote: Originally posted by PHILOU Zrealone

Quote: Originally posted by Laboratory of Liptakov

What about 1,4-diaminotetrazine complexes?

PHILOU Zrealone - 28-6-2017 at 02:30

Quote: Originally posted by Chisholm

Quote: Originally posted by PHILOU Zrealone

Quote: Originally posted by Laboratory of Liptakov

What about 1,4-diaminotetrazine complexes?

Yes DATAZ :-)

Or 1,4-dihydrazino-tetrazine...
Or amino-/hydrazino-/diamino-/dihydrazino-tetrazoles...
Or amino-/hydrazino-triazoles

Or hydroxylamines like HONH2-CH2-CH2-NH2OH or H2N-O-CH2-CH2-O-NH2 or hydrazines like CH3-NH-NH-CH3 or H2N-NH-CH2-CH2-NH-NH2...

Variations onto the subject are limiteless...so much to test and relatively simple chemistry as soon as you have the metallic salts, water, alcohol, ether and the desired complexing amine...

Beware that some may prove to be unstable....and self ignite...
I have experienced strong unstability of Cu(N2H4)2(NO3)2 and Ag(N2H4)NO3...probably because the Cu(2+) and Ag(+) are too oxydant for N2H4...same should occur with IO3 and IO4 anions vs N2H4...

Some are explosive even into solution like Ni(N2H4)3(ClO4)2 and highly sensitive to shock or friction even from a spoon swirling into the solution...