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B(a)P
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Quote: Originally posted by Etanol  | | Quote: Originally posted by B(a)P |
What is this based on? I have not done much testing on anything other than azotetrazolates and what I have done has been limited, but it did not seem
to be that azotetrazolates lacked explosive energy.
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I was wrong. The calc explosive heat of copper azotetrazolate is sufficient. Due to the high enthalpy of formation.
I think Ni azotetrazolate is perpective if it does not form hydrates, because it should have similar power but less sensitivity. In addition, Ni does
not oxidize in the air unlike Fe(2+)=>Fe(3+).
[Edited on 19-4-2024 by Etanol] |
I have previously done some experimentation trying to form Ni azotetrazolate perchlorate, I am still in the process of trying to work out what the
product was (eg which hydrate if any and is it a complex or double salt). It has some promising properties, but needs more work before I can report
anything meaningful back.
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Microtek
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I have recently experimented with 4-amino-1,2,4-triazole as a ligand for nickel perchlorate. I think it probably forms with two 4-ATrz ligands based
on yield. The product is not hygroscopic and very insensitive for this kind of compound. I was not able to get any reaction in the oblique impact test
on sand paper (highest setting, 5.5 Joule impact), and I was also not able to set it off with hammer and anvil (though this test is not 100%
reliable).
It Does DDT from fuse ignition at the 25 mg level, lightly confined. I haven't tested initiation ability yet. Based on flame tests of samples in
Al-foil, it seems very thermally stable.
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Etanol
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| Quote: Originally posted by dettoo456 | If you are really concerned with yield, just dry out the solids from a 5-ATz synthesis and reflux in anhydrous EtOH for an hour or two to completely
extract any available 5-ATz. In my experience though, the crystallization of 5-ATz is consistent enough to disregard a different extraction method.
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Thanks. Acetone is better. Using the standard method, I got less than 50% 5-ATZ*H2O from aminoguanidine bicarbonate, H2SO4 and NaNO2. But by adding
extraction I increased the yield to 83% of theory.
I compared Сu 5,5'-azotetrazolate and poorly crystallized AgNT compressed by hand with the same force in plastic tubes on metall plates.
Сu 5,5'-azotetrazolate 0.9g/cc was compacted with alcohol then dried within a day because dry subs is very dangerous.
AgNT 1.25g/cc
Сu 5,5'-azotetrazolate at this density is 2 times weaker than AgNT and much weaker than NAP or PVA-Lead Azide compressed with the same force.
Does anyone know the max density and enthalpy of formation of copper 5,5'-azotetrazolate or some other 5,5'-azotetrazolate to evaluate detonation
parameters?
I prepare Ni and Co(II) 5,5'-azotetrazolates from raw Na 5,5'-azotetrazolate. Being placed in a flame or on hot foil, they only crack. That is,
microdetonation occurs instead of complete detonation. It looks like these are hydrates.
Both substances are poorly soluble in water, but are very difficult to filter. These are rather colloids than crystals.
Is Ag nitroaminotetrazolate sensitivity acceptable for practical use?
[Edited on 23-4-2024 by Etanol]
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Etanol
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More questions about making BNCP
| Quote: Originally posted by snooby |
1. Preparation of [Co(NH3)4CO3]2SO4*3H2O complex. 47g CoSO4*7H2O is dissolved it 125 ml of water and is added to solution of 100g (NH4)2CO3 in 500 ml
H2O + 250 ml 25% ammonia solution. Resulted dark violet solution is oxidised by addition of 14 ml of 30% hydrogen peroxide. Solution is allowed to sit
for 30 minutes, after that period it is placed on boiling water bath and is evaporated to 300 ml volume. During course of the concentration process,
solid ammonium carbonate (25 g) was added in installments. Solution is filtered from unsignificant ammount of precipitated black cobalt oxide and is
further concentrated to 200 ml volume. Solution is slowly cooled to room temperature, product precipitates as small deep-red prisms. They are filtered
out from the solution and allowed to dry at room temperature. Yield is 16 g of pure product, mother liquer can be further concentated with addition of
ammonium carbonate to get more 16 g of complex, but it is less pure.
2. Preparation of [Co(NH3)4CO3](ClO4) complex. 16g of complexed synthesised on first stege is dissolved in 320 ml of water. Solution is filtered and
16g of sodium perchlorate in 40 ml of water is added with stirring. Mixture is cooled on ice (or in freezer) for 3-4 hours. Product precipitates as
small, lustrous, sharp violet prisms. Crystalls are filtered off, washed with small ammount of ice cold water and dried at room temperature. Yield is
about 14 gramms.
3. Preparation of BNCP. 14g [Co(NH3)4CO3](ClO4) is dissolved in 140 ml 10% perchloric acid, and solution of 26.5g of sodium 5-nitrotetrazolate
dihydrate in 450 ml of water is added with stirring. Solution is placed on boiling water bath, and allowed to sit there for 4 hours. Solution is
slowly cooled to room temperature and then cooled in freezer to 10°С, precipitated crystalls of BNCP are filtered of, washed with cold water, and
recrystallised from 1% perchloric acid. Yield is 12.9g.
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How can I check that I have prepared a cobalt-3 compound and not a cobalt-2 or a mixture of both? They are the same color.
How can I be sure that I am getting a [Co(NH3)4CO3](ClO4) precipitate and not a mixture of [Co(NH3)4CO3](ClO4) and [Co(NH3)4CO3]2SO4?
I have CoCO3 for ceramics. Can I use it and NH4ClO4, to immediately prepare [Co(NH3)4CO3](ClO4) without SO4 or NO3 anions ?
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Etanol
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How could you oxidize Cobalt(II) ammine complex into Cobalt(III) with H2O2? I add H2O2 drops and it immediately decomposes with bubbles even 3%
concentration.
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Etanol
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Acid strangeness in hot synthesis of 5-NT
To prepare NaNT, I dissolved 0.2 mol of ATz*H2O (prepared from aminoguanidine bicarbonate) in 0.2 mol of 37% sulfuric acid for accumulator and diluted
with distilled water to a volume of about 200 ml.
Then I dissolved 0.6 mol of NaNO2 in distilled water, filtered it and diluted it to a volume of 200 ml.
I heated both solutions to 60-70 degrees and added a solution of ATz and H2SO4 to a solution of NaNO2 within 60 minutes.
I took into account the acidity of 5-NT, so I thought that the reaction would go like this:
1)2NaNO2+H2SO4=>Na2SO4+2HNO2
2)ATZ+HNO2=>diazoTZ+H2O
3)diazoTZ+HNO2=>NT+H2O+N2
4)NT+NaNO2=>NaNT+HNO2
Thus, only Na2SO4 and NaNT were left in the solution.
I planned to remove the remains of NaNO2 by adding a new portion of H2SO4, but when I measured the acidity of mix, it was already about pH1!
I did not add new H2SO4, but I stir the mixture for 60 minutes at the same temperature.
Then I began to neutralize a hot mixture of baking soda(NaHCO3) to pH7.
I needed 0.2 mol of NaHCO3!
Where could unaccounted 0.2 mole-equivalent of strong acid come from in the reaction mixture?!
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Sir_Gawain
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Did you end up with a yield of NaNTz? It’s possible the reaction didn’t work and so none of the original acid was consumed.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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Etanol
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| Quote: Originally posted by Sir_Gawain | | Did you end up with a yield of NaNTz? It’s possible the reaction didn’t work and so none of the original acid was consumed.
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I can say the yield when I evaporate the acetone extract.
The reaction works because a golden NaNT extract in acetone was obtained and earlier I already received NaNT and other nitritetrazolates in this way
with 50-60% yield with unknown degree of purity.
But the reaction does not work as in theory, it goes with a large overspending of NaNO2.
I have already allocated about 0.5 grams of green copper aminotetrazolate from the remaining mixture of mineral salts after an extraction and I am
afraid that even more unreacted 5-ATZ went into acetone extract.
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