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Author: Subject: Styphnic acid and lead styphnate
Tdep
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[*] posted on 15-10-2015 at 06:50


Quote: Originally posted by Keith Fletcher  

Any suggestions for future videos.


The DDNP thread looks interesting recently, and theres some nice writeups on making the two slightly different versions, what is it DDNP and iso-DDNP. Would be interesting to compare them and see a nice video of their formation.
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Keith Fletcher
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[*] posted on 15-10-2015 at 07:12


I will do so work with DDNP



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nitro-genes
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[*] posted on 15-10-2015 at 07:54


Or DDNR...:) Stannous chloride can be made from dissolving tin in concentrated hydrochloric, I think Rosco posted a patent for the reduction of TNR to dinitro amino rescorcinol this way in the DDNP thread. The potassium salt is very energetic reportedly, though very sensitive as well...
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Keith Fletcher
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[*] posted on 15-10-2015 at 08:26
TNR salts


Im thinking about making the Mercury, Nickle, Cobalt, Cadmium and Chromium salts of TNR. Has anyone had any expirance with these compounds?



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Herr Haber
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[*] posted on 24-7-2016 at 11:30


Hey all,

I just got a new (and better!) magnetic stirrer / heater and was wondering what to do with it when it struck me: Magnesium Styphnate then Lead Styphate !

So I weighted 2 grams of TNR, added them to an Erlenmeyer flask with 500 ml water (then added 300 more during the course of the experiment) and cranked the heat up to 70°c with stirring on.
So far, so good. The TNR had dissolved and I started adding Magnesium Carbonate.
And then I added more. And more. And turned the heat up to 80°c but still no color change. The solution with now a good amount of Magnesium Carbonate was still yellow. A magnesium styphnate solution should be clear right?

Seing that a good number of Sodium salts can be used (hydroxide, bicarbonate etc). I was pretty certain using MgCO3 instead of MgO would be ok.

Then I noticed the label on this food grade Magnesium Carbonate : 4MgCO3*Mg(OH)2*5H20

Was I wrong in assuming the carbonate could replace MgO or is it my food grade Magnesium Carbonate who's to blame?

Thanks for your input.
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PHILOU Zrealone
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[*] posted on 25-7-2016 at 03:34


Maybe that Magnesia (4MgCO3*Mg(OH)2*5H20) is more basic than MgCO3 and as such is responsible of the yellower tinge of your trinitroresorcinate salt.

This is observed with trinitrophenates too basic a media and the colorfull nitronic form of the salt is present.
-C(-NO2)=C(-OH)- <--base==> -C(=N(O)-OH)-C(=O)-
So the proton switches from the phenol to the nitrogroup.

In principle the nitronic colored form is slightly more sensitive to shock and heat than the normal phenic form...

[Edited on 25-7-2016 by PHILOU Zrealone]




PH Z (PHILOU Zrealone)

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[*] posted on 17-8-2016 at 13:43


Well... As I kept the TNR with the magnesia settled in the bottom I thought "Why not play with it a bit and test Philou's theory?"
I didnt have what I wanted and I have a bit of lead nitrate so this is what I did:

- Filter out the excess magnesia that had settled in the bottom.
- Heat the filtrate to 70°c as if I was going to proceed with the normal synthesis
- Dissolve and heat 1g of lead nitrate
- Add the lead nitrate to the assumed magnesium styphnate solution.

Lo and behold! A precipitate appeared !

Since I was curious, I pipetted a few ml of 69% HNO3 and started adding it drop by drop to my not so scientific experiment.
- First some fizzing was observed therefore confirming Philou's theory that the solution was basic
- Then, while adding drop by drop all of a sudden all the precipitate vanished further confirming that theory.
It would have been interesting to know what was the PH when this happened.
At this point, I wanted confirmation and grabbed some NAOH. I added some tiny pearls and got back a precipitate.

I filtered out everything, let it dry and unsurprisingly the precipitate doesnt react to the flame.

In a few days I might try lead styphnate "the right way" through sodium styphnate.
I've been wondering though what would happen if instead of MgO I couldnt use straight powdered Mg.
And in that case, what would be the dynamics of the reaction?
Would it be straight to Magnesium Styphnate or would it go through Magnesium hydroxide first?
Or am I totally wrong? :)
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PHILOU Zrealone
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[*] posted on 18-8-2016 at 06:11


Magnesia is MgCO3 mixed with Mg(OH)2.
It is "unsoluble" but stil a little --> the MgCO3 is a little more soluble than the Mg(OH)2...
Solubility is defined by the solubility product even for "unsoluble" products.
MgCO3(s) <==H2O--> Mg(2+) + CO3(2-) (cations and anions are solvated /aqueous)
Mg(OH)2(s) <==H2O--> Mg(2+) + 2 OH(-) (cations and anions are solvated /aqueous)

Trinitroresorcinol (2,4,6-trinitro-1,3-dihydroxybenzene) is a diacid
(O2N)3C6H(-OH)2 <--H2O-->(O2N)3C6H(-O(-))2 + 2 H(+)
As such it should have fizzed a bit with the MgCO3 unless the Mg(OH)2 has reacted faster with it.
H(+) + OH(-) <--==> H2O (neutralization)
2 H(+) + CO3(2-) <--==> H2CO3 <--> H2O + CO2(g) (another kind of neutralization)
So
(O2N)3C6H(-OH)2 + Mg(OH)2 --> (O2N)3C6H(-O-)2Mg + 2 H2O (in fact (O2N)3C6H(-O(-))2 + Mg(2+))
(O2N)3C6H(-OH)2 + MgCO3 --> (O2N)3C6H(-O-)2Mg + H2O + CO2(g) (in fact (O2N)3C6H(-O(-))2 + Mg(2+))

If there was exces MgCO3/Mg(OH)2 as proven by the remaining precipitate then you have into the media after filtration:
Mg(2+), CO3(2-), OH(-) and (O2N)3C6H(-O(-))2

Adding Pb(NO3)2 will precipitate traces PbCO3, Pb(OH)2 aswel as (O2N)3C6H(-O-)2Pb all less soluble (= more unsoluble).

Adding HNO3 will fizz from CO3(2-) and PbCO3 by setting CO2(g) free and neutralize OH(-) and Pb(OH)2...but it will also solubilise them by forming the soluble Pb(NO3)2
PbCO3 + 2 HNO3 --> Pb(2+) + 2 NO3(-) + H2O + CO2(g)
Pb(OH)2 + 2 HNO3 --> Pb(2+) + 2 NO3(-) + 2 H2O
Then the HNO3 will act further and solubilise the lead styphnate/trinitroresorcinate because HNO3 is a stonger acid than TNR and as such it will displace the weaker acid from their salts.
(O2N)3C6H(-O-)2Pb + 2 H(+) --> (O2N)3C6H(-OH)2 + Pb(2+)
If too much acid is added then TNR will be dropped out of solution because the later equation is an equilibrium
(O2N)3C6H(-OH)2 <--H2O-->(O2N)3C6H(-O(-))2 + 2 H(+).

The neutralization pH must close to 7 and more than certainly between 6 and 8.

Adding NaOH will precipitate only Pb(2+) and Mg(2+) as unsoluble white Pb(OH)2 and Mg(OH)2...the nitrate and TNR will remain solubilized as Na(+) salts...thus normal that the precipitate doesn't react to flame!

Mg metal will be probably too reductive to allow for direct reaction with TNR so some reduction of the nitro into amino (or intermediary nitroso, hydroxylamino groups, diazo oxyde)




PH Z (PHILOU Zrealone)

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