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Laboratory of Liptakov
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Follow procedure when preparing Lithex. Stainless steel flat pan (absolutely clean), stainless steel planchet, temperature 150 - 155 Celsius. Never
use teflon...
Development of primarily - secondary substances: CHP (2015) neutral CHP and Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024) Diper
60 (2025)
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ManyInterests
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And I finally did it a second time. This time I do believe my ammonium perchlorate was pure enough to have a noticeable reaction difference. I also
barely (and I mean BARELY) had any nickel carbonate left over to the point where I wasn't sure even if decanting was necessary since I only saw a
singular speck of green.
I ultrasonicated it for 10.5 minutes. The temp rose from 20C to 32C during that time, but it looks like amazing. I love it! I really, REALLY hope I
got a working product this time around.
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ManyInterests
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It failed. I tried to light some up on aluminum foil and it didn't detonate or even burn. I used a jet lighter to generate more heat and it failed the
same way my first batch did.
I honestly am at a loss as to what is going wrong. The ammonium perchlorate IS pure this time. Why it is failing is beyond me. I will need some
help...
Edit: I looked up the ultra sonicator frequency. It might be in 40kHz and not 42kHz. I am not sure if the difference is what is causing the problem...
but at any rate I think I might want to try the iNAP method instead of ultrasonication. The energy output is not the same, but with 50 or 100mg
loadings that should still be effective.
At any rate, I have nothing to lose by trying iNAP.
[Edited on 7-1-2025 by ManyInterests]
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Microtek
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Have you used other methods to succesfully make NAP?
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ManyInterests
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I wasted no time in trying again with iNAP. I used a the same proprotions (0.86g of ammonium perchlorate, 1g of aminoguadine bicarbonate, and 0.43g of
nickel carbonate) and around 40ml of isopropyl alcohol (91%) that I brought to a boil first then added everything and I boiled with strong stirring in
a mostly sealed borosilicate jar for 5 minutes and 15 seconds.
As you can see, there were some chunks of unreacted nickel carbonate that I removed (I had powdered the carbonate earlier by hand). Maybe one issue is
that the mixture as I added it were mostly apart in chunks and not 100% powdered. But they all dissolved over time (the aminoguanadine was in hard
chunks that I broke up with a dowel afterward in the same cup.
But there is a lot more unreacted nickel carbonate than I thought. Maybe 0.43g is far too much of an excess?
 
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ManyInterests
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I had waited for several hours to try a little... and it does not appear to have any result.
Maybe it is not my ammonium perchlorate. I am realy, really curious as to why it is failing consisently in such abysmal ways. I am at a loss. I did
everything exactly as specified but still not even a slight burn?
Edit: I am really baffled as to what is wrong.
[Edited on 7-1-2025 by ManyInterests]
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Etanol
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Quote: Originally posted by ManyInterests  |
I ultrasonicated it for 10.5 minutes. The temp rose from 20C to 32C during that time...
Edit: I looked up the ultra sonicator frequency. It might be in 40kHz and not 42kHz. I am not sure if the difference is what is causing the problem...
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It doesn't matter.
Ultrasonic is not a magic wand. This will not force a reaction to proceed that cannot proceed due to low temperature and/or low solubility of the
reactants.
Try replacing isopropyl alcohol with ethyl alcohol or increasing the water content in the mixture of isopropanol and water. The temperature should not
be below 90-100 degrees! If the mixture contains carbonate, this is an indispensable condition. Until the carbonate of aminoguanidine and nickel has
decomposed into carbon dioxide, NAP will not form.
[Edited on 7-1-2025 by Etanol]
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ManyInterests
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| Quote: Originally posted by Etanol | | Quote: Originally posted by ManyInterests |
I ultrasonicated it for 10.5 minutes. The temp rose from 20C to 32C during that time...
Edit: I looked up the ultra sonicator frequency. It might be in 40kHz and not 42kHz. I am not sure if the difference is what is causing the problem...
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It doesn't matter.
Ultrasonic is not a magic wand. This will not force a reaction to proceed that cannot proceed due to low temperature and/or low solubility of the
reactants.
Try replacing isopropyl alcohol with ethyl alcohol or increasing the water content in the mixture of isopropanol and water. The temperature should not
be below 90-100 degrees! If the mixture contains carbonate, this is an indispensable condition. Until the carbonate of aminoguanidine and nickel has
decomposed into carbon dioxide, NAP will not form.
[Edited on 7-1-2025 by Etanol] |
So let me write the steps according to your instructions to make sure I understood you.
1: mix the components and make sure they're as finely powdered as possible
2: Get a 70% isopropyl alcohol solution and not 91%. It must be at a rolling boil before anything else is done and heat is at maximum at all times.
If water is used instead, it also must be at a rolling boil at all times.
3: after boiling, keep it covered and let it boil until all the reaction is done. Well over 5 minutes, and the cover cannot completely tight, it must
allow some air to get out to let the CO2 leave.
after that, it is decant and ultrasonicate (if making uNAP) or just pour on a coffee filter to dry out (if iNAP).
How much time do you believe it would need to be boiling? 10 minutes? 30 minutes?
[Edited on 7-1-2025 by ManyInterests]
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Etanol
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| Quote: Originally posted by ManyInterests |
So let me write the steps according to your instructions to make sure I understood you.
1: mix the components and make sure they're as finely powdered as possible
2: Get a 70% isopropyl alcohol solution and not 91%. It must be at a rolling boil before anything else is done and heat is at maximum at all times.
If water is used instead, it also must be at a rolling boil at all times.
3: after boiling, keep it covered and let it boil until all the reaction is done. Well over 5 minutes, and the cover cannot completely tight, it must
allow some air to get out to let the CO2 leave.
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1.ok
2.ok
3.ok +If possible, turn on the ultrasonic in the 3rd step. This will accelerate the dissolution of nickel carbonate.
15 ... 90 minutes. It depends on many factors. Keep the solution in a boil until most of nickel carbonate is dissolved and the solution becomes
red-black.
4.Filter a hot solution to remove the rest of the nickel carbonate.
5.Evaporation the hot solution to a concentration of about 10%.
6.Turn on the ultrasonic again and cool the solution to 0C.
7.Filter NAP.
[Edited on 8-1-2025 by Etanol]
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ManyInterests
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So it will be for a uNAP since iNAP does not call for ultra sonication. So I will update my steps (I am autistic and I prefer to have everything in a
step-by-step format as it is easier to follow), and I will do it with a water solvent... unless you also want to ultrasonic the iNAP...
1: Measure the components, mix, and grind as finely as possible. Set aside
2: Measure out around 25ml-30ml of distilled water (for the 1:0.86:0.43 proportions).
3: Bring the water to a boil, once it is at a boil, start the stirring and dump all the ingredients in at once
4: Cover the jar, but let it be a little loose as to allow some steam to leave.
5: Keep the boil and stirring for a minimum of 15 minutes, the main thing to look for is the color and the dissolution of the nickel carbonate.
6: Decant and heat again uncovered to evaporate the solution further
7: ultrasonic it. Around 10 or 15 minutes?
8: cool down to 0C
9: filter out the final product and let it dry.
Am I on the right track?
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Microtek
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I think the best change will be to replace the NiCO3 with a soluble nickel salt. If the carbonate sometimes works for producing NAP it is DESPITE
being a really bad choice. I simply cannot believe that you don't have access to any acid (HCl or H2SO4 or HNO3) that will dissolve the carbonate.
Also dissolve the aminoguanidine bicarbonate in acid (don't use more acid than the stoichiometric amount for either of the dissolutions).
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Etanol
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Step 7 and step 8 are simultaneous.
Ultrasonic modifies the size and shape of the grains as it fall out.
| Quote: Originally posted by Microtek | | I think the best change will be to replace the NiCO3 with a soluble nickel salt. If the carbonate sometimes works for producing NAP it is DESPITE
being a really bad choice. I simply cannot believe that you don't have access to any acid (HCl or H2SO4 or HNO3) that will dissolve the carbonate.
Also dissolve the aminoguanidine bicarbonate in acid (don't use more acid than the stoichiometric amount for either of the dissolutions).
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Nickel nitrate forms a complex [Ni(AGu)2](NO3)2, but not NAP. I did it.
I think HCl and H2SO4 salts are not allowed in this synthesis.
The only use of the nickel sulfate is a two-step synthesis of the [Ni(NH3)6](ClO4)2, then its reaction with aminoguanidine perchlorate. It is
important! the aminoguanidine perchlorate be prepared before adding the [Ni(NH3)6](ClO4)2, rather than attempting to prepare it from ammonia
perchlorate and aminoguanidine carbonate in the presence of the [Ni(NH3)6](ClO4)2.
[Edited on 8-1-2025 by Etanol]
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ManyInterests
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| Quote: | | I think the best change will be to replace the NiCO3 with a soluble nickel salt. If the carbonate sometimes works for producing NAP it is DESPITE
being a really bad choice. I simply cannot believe that you don't have access to any acid (HCl or H2SO4 or HNO3) that will dissolve the carbonate.
Also dissolve the aminoguanidine bicarbonate in acid (don't use more acid than the stoichiometric amount for either of the dissolutions).
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I do have nickel nitrate. I also have an ample supply of HCl and H2SO4. I can distill some HNO3 whenever I need.
But as Etanol said, it is not a viable route.
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Step 7 and step 8 are simultaneous.
Ultrasonic modifies the size and shape of the grains as it fall out. |
How would I do them at the same time? I can add ice cold water to the ultrasonic cleaner and (I think, I need to confirm) that the ultrasonic cleaner
is also temperature controlled that can also cool down the water. I need to confirm that. But the solution will be hot once I start the ultrasonic.
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Etanol
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You can prepare Ni(ClO4)2 from NiSO4 and NaClO4 in hot ethyl alcohol:
NiSO4+2NaClO4=Ni(ClO4)2+Na2SO4
Separately, prepare aminoguanidine perchlorate by boiling ammonium perchlorate and aminoguanidine carbonate in water until carbon dioxide and ammonia
no longer evolve.
Then, merge the two solutions together and adjust the acidity by adding aqueous ammonia or NAOH. NAP is formed.
Gradually change the hot water in the ultrasonic cleaner to cold water, then add ice.
[Edited on 9-1-2025 by Etanol]
[Edited on 9-1-2025 by Etanol]
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Axt
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It's true that the chloride complex has as limited a solubility as the perchlorate, been there tried that. Mixing a 100mL solution of the chloride
derived from 1.5g NiO results in immediate precipitation of the chloride. Precipitation from a mix of chloride and perchlorate NiCl2 ⇌ 2NaClO4
results in a precipitate with notably less explosive vehemence then the perchlorate alone.
On the other hand a complex that is precipitated from a mixed solution of nitrate and bromate Ni(NO3)2 ⇌ 2NaBrO3 is extremely vehemic, as or more so
than the perchlorate. Although I say nothing of the stability/sensitivity/compatibility. Bromate is more innocuous and readily available here.
I have never tried to actually precipitate the nitrate complex alone, has anyone had experience with that?
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Axt
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I've run a few mixed salt reactions now, this is the results.
Ni(CH6N4)2(ClO4)2 ⇌ 4NaCl
When held into flame only weak intermittent pops, pretty much inert.
Ni(CH6N4)2(ClO4)2 ⇌ 4NaNO3
Deflagrates mildly on ignition, much like the pure nitrate.
Ni(CH6N4)2(NO3)2 ⇌ 2NaNO3 ⇌ 2NaBrO3
Detonates violently is tiny amounts, more vehemic than the perchlorate, only slightly less vehemic than Ag nitrotetrazolate.
Ni(CH6N4)2(NO3)2 ⇌ 2NaCl
Deflagrates mildly, only slightly less energetic than the pure nitrate complex.
Conclusion: The solubilities seem to be Bromate < Nitrate < Chloride < Perchlorate
ps. Yes I invented the word "vehemic" as there is no word in the english language to describe what I need, but I'm sure it makes sense in the context
for which it is written.
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pdb
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| Quote: Originally posted by Axt |
ps. Yes I invented the word "vehemic" as there is no word in the english language to describe what I need, but I'm sure it makes sense in the context
for which it is written. |
Funny, where did you get inspiration from ? Because 'véhément' exists in French as an adjective, and means (talking of a person) 'Someone who
demonstrates passion and great expressive and impetuous strength'.
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Axt
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Oh it is a word here too, well without the dots or dashes or whatever the fuck they are  Vehement and vehemently, but surprisingly not vehemic (see it has a red squiggly line if you type it) so it's now assigned in my mind to a
compounds ability to self-accelerate to detonation unconfined.
Fulminic is the archaic term but its draws too many connotations now, being coopted by a certain acid.
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ManyInterests
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OK, so in the next few days I will be trying again. I already listed out my steps, but since you say that cooling to 0C is necessary, I found a way.
Not only will I be using ice cold water (cooled to the point of just starting to solidify into ice) while ultrasonicating, what I also do is have my
ultrasonicator done outside. It is a very cold outside where I live, so the ambient temperature will be helping.
As for heating it, I will NOT just the jar with a lid, I will use a beaker with a watch glass atop it, mostly covered, but it will be given the space
to allow the CO2 to leave. Maybe I will be using slightly more water as I will let it boil for a full 20 to 25 minutes with strong stirring. I need to
make sure it doesn't run completely dry since that can be very dangerous. letting it boil for 5 minutes didn't lose a lot of water I must say, but I
never did it for 25 minutes.
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