C6H3N3O9Pb

[Tony Montana]

Also called: lead styphnate, lead trinitroresorcinate
Explosive type: high-primary
Det. rate: 5200 m/s
Lead block test: 130cc
Form: orange to brown crystals
Deflagration temp: 275c (527f)
Impact sensitivity: moderately high - 5 Nm
Water sensitivity: moderate
Initiate with: spark

Pour 17.5 u.b.w.(units by weight) of water into a container, add 6 u.b.w of C6H3N3O8 to the water. Slowly stir in 1 u.b.w. MgO to the H2O/C6H3N3O8 solution, this will give of a bit of heat. Gently warm the solution to 60 degrees celcius, then allow to cool to room temperature. Filter the liquid to remove any solids, dilute the solution with water until it has a density of 1.043g per ml. Allow solution to stand for 12 hours, you now have a diluted magnesium styphnate solution.
Place 3.1 u.b.w. of diluted magnesium styphnate solution into a new container, slowly heat solution to 55 degrees celcius, then remove from heat source. Very SLOWLY(one drop at a time) stir 1 u.b.w. of 34%
Pb(NO3)2 solution into the magnesium styphnate solution, if the temperature approaches 60 degrees celcius then stop adding Pb(NO3)2, but keep stirring until the temperature drops to at least 55 degrees celcius. Once all of Pb(NO3)2 is added, cool the solution to 25 degrees celcius, stop stirring and allow solution to stand for 20 minutes at 25 degrees celcius. LS crystals will start to settle to the bottom, gently filter and wash the crystals with 5 u.b.w. of water to wash away impurities. Dry the crystals and BINGO!
Hope some of you find this interesting, even helpful.

[Mr Cool]

Yes, very helpful thanks.
C6H3N3O8... obviously that's styphnic acid, but I'm not sure about the structure. Could one also call it 1,3-dihydroxy-2,4,6-trinitrobenzene? Like picric acid with another hydroxyl group instead of one of the hydrogens? Or am I completely wrong?

[a_bab]

I think that a styphnic acid synthesis from resorcine will be much more welcome...

________________________
http://move.to/pyromania

[Tony Montana]

TRINITRORESORCINOL
Also called: styphnic acid
Form: yellow powder
Chem. formula: C6H3N3O8
Specific gravity: 1.82
Toxic effects: Information unavailable. Treat as a toxic material.

[This message has been edited by Tony Montana (edited June 25, 2001).]

[Mr Cool]

I'd say just use the method for making TNP from phenol, but use an equivalent number of moles of resorcinol instead of phenol.

[Tony Montana]

I dont actuallly have that synthesis on hand, but would pretty much say that Mr.Cool is right. A three stage nitration, the first nitration yeilding; mono-nitroresorcinol. The second yeilding; di-nitroresorcinol.
The third yielding; tri-nitroresorcinol.
Exactly like Tri-nitrotoluene, nitrating toluene results in MNT(mononitrotoluene) after that DNT(dinitrotoluene) and the last one produces TNT(trinitrotoluene).
Is there anyone who knows how to find patents? A search for styphnic acid would be handy!

[PHILOU Zrealone]

On a reactivity scale:
if the speed of nitration for benzene is 1 (it is quite slow)
nitrobenzene is 0.05
toluene is 25
phenol is 2000

If you really want to make a three stage process then you have to start from low concentrate nitric otherwise you go directly to the dinitro and even to the trinitrophenol.

------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[Tony Montana]

Yeah, that the same as TNT synthesis, I had a good link to put up but have not got the right adress yet.
Here it is get this while it lasts, trust me
http://chppm-www.apgea.army.mil/documents/tg/techguid/tg140.pdf
An excellent read!


[This message has been edited by Tony Montana (edited June 26, 2001).]

[Ezikiel]

Hello gang ...
I had prepared a batch of Styphanic acid 3 years ago when I was in grade 10 (I was friends with the lab assistant).
Anyways I simply replaced the Phenol in the preperation of Picric acid with Resorchinol.
I had made 3 batches using 1,2 di hydroxy benzene, 1,3 dhb and 1,4 dhb.
out of these three the styphanic acids had almost the same sensitivity but the Pb styphanates had quite different sensitivties.
1,2Pb Sty < 1,3Pb sty < 1,4Pb sty.
There was something I was wondering about but wasn't able to try .... R the -OH's estrifiable.

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"Go out in a BLAZE OF GLORY"

[PHILOU Zrealone]

HO of phenol or not esterifiable! Hopefully, otherwise in TNP synthesis you would have troubles :-°.

------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[Tony Montana]

The reason I put that link above was hopefully some people would actually download and read it. If you did read it you would have noticed it not only shows you how a TNR (trinitroresorcinol) manufacturing plant works, it tells you how to make TNR from resorcinol!!

[Mr Cool]

Making TNR from resorcinol is easy. But what do you make resorcinol from???

[Hex]

You could make it from 1,3-dichlorbenzene and NaOH, but I think this would need pretty high temp/pressure. Might be better to approach it from another angle, and nitrate 1,3-DCB to 1,3-DC-5-nitrobenzene or 1,3-DC-4,6-dinitrobenzene (probably difficult to do the latter), then do the reaction with NaOH - it should go a lot easier once the nitro groups are on the ring.
The dichlorobenzene can be made from benzene, elemental chlorine and a FC catalyst, but frankly it seems like a lot of trouble to go to make this stuff. As far as I'm aware Lead Styphnate is only used for getting azide started as it has good ignition sensitivity. For any other purpose a picrate would probably be just as good.

[This message has been edited by Hex (edited August 13, 2001).]

[Tony Montana]

Thanx Hex,
Resorcinol can made from less carcinogenic precursors, also. Check this out, Resorcinol from Glucose:
http://es.epa.gov/ncerqa_abstracts/grants/97/sust/frost.html

[Mr Cool]

Shit!!! That link reminded me - I've seen resorcinol glue! One half paraformaldehyde, one have resorcinol that you mix together!!! I can't remember anything else about it, I didn't look closely as I didn't have a need for resorcinol and I had a cheaper source of formaldehyde.
I have to find it again! I think it was in a B&Q Warehouse - all Brits, go to your local one and see if you can find it!

[deezs]

You (I) can buy resorcin in the pharmacy. If you can find a pharmacy, where they make medicines, they surely have it, and a lot of other stuff. If you need a list of useful chemicals, write me.

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"Don't belive anything, just because there is a good proverb for it."

"To avoid injury in a battle, watch them from the nearer hill."

[Mr Cool]

A pharmacy where they MAKE medicines? Surely that all happens in big factories? Also I'm surprised they sell it to members of the public.

[Tony Montana]

Mr.Cool, just out of curiosity where do you you acquire your formaldhyde from? Not an exact address, just what type of store and what is it used for (what do you tell them its used for?)
Thanx

[cutefix]

I think resorcinol is suitable also as an antiseptic so it can possibly be found in the pharmacy….

Formaldehyde is available as formalin solution.Funeral establishment where they do a lot of embalming of corpses, usually have large inventories for it….maybe you can ask some…..In some pharmacies it is available also.maybe you can try asking them also.
For a valid reason tell them ,you are having zoology lessons and would like to preserve animal cadavers for further future experiments….

[Mr Cool]

Camping shops as portable toilet disinfectant (both paraformaldehyde and a formaldehyde solution can be found), dairy farm suppliers again as some sort of disinfectant, garden centres as moss killer, fungicide or mildewcide.

[deezs]

I don't know, how it goes in other parts of the world, but in Eastern Europe, there are a lot of medicines, which are made in the pharmacy. They are mostly solutions and suspensions to drink, or to rubbing in (no tablets). There's a useful book which contains the recipes for these, It must be in every older pharmacy. It is bilingual, latin and the national. It's latin title is Formulae Normales. You can find in this almost all the chemicals, you can buy in the pharmacy.
An example:
Ask, if they have Solutio Castellani (if the salesgirl doesn't know, call the pharmacist!). This is used against mycosis, and 50g contains: .25g fuchsin, .5g boric acid, 1g phenoli liquefacti (I can't translate this from latin), 2g resorcin, 2.5g aceton, 5g ethanol, water.

In my country, laws becoming more and more strict. I can get chemicals so easily, because the pharmacist knows me as a young "genius" for 5 years now. I buy there ccHNO3, ccHCl, formaldehyde, KNO3, S, phenol.............................
In an other pharmacy, I wanted to make more connections, so I asked KMnO4 and formaldehyde solution. They gave only 10 g KMnO4, and asked for receipt to give the formaldehyde. I never went back.
I just want to advise, to find a friendly pharmacist, and build a good connection with him. If you keep telling him your interesting, but innocent experiments, later, he will give you chemicals illegally too...


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"Don't belive anything, just because there is a good proverb for it."

"To avoid injury in a battle, watch them from the nearer hill."

[Mr Cool]

I think many pharmacists know what I do anyway. I once asked for three bottles of 9% H2O2, and he asked me what I was going to blow up! But I lied and said it was for sterilising jam jars, and he sold it me. I bet as I walked out the shop he was wondering what sort of jam I could be making in December!!!

[Tony Montana]

In regard to the glue, there turned out to be a few noteworthy types:
Resorcinol /Phenolic
http://www.avsyntec.com.au/docs/a022.pdf
Urea /Formaldehyde
http://www.avsyntec.com.au/docs/a006to9.pdf
Marine grade Resorcinol /Phenol
http://www.avsyntec.com.au/docs/a018to19.pdf
Has anyone ever experimented with any of the above??

[PHILOU Zrealone]

As I explained earlier, Phenol is way more reactive than Toluen. Here the resorcinol is even more reactive than the phenol.
As mentioned Hex, dichlorobenzene can lead to resorcinol. But to make dichlorobenzene is not trivial since it uses:
Benzen (what is no more available due to carcinogenicity), AlCl3 (very sensitive to moisture and corrosive --> HCl + Al(OH)3) and Cl2 (toxic gas).
The AlCl3 is a lewis acid and catalyses the generation in situ of the Cl+ that can reach the electron rich benzenring what can't do the Cl- due to electrostatic repulsion.
AlCl3 + Cl2 --> AlCl4- + Cl+
Cl+ + C6H6 --> [C6H6Cl+]--> C6H5Cl + H+
H+ + AlCl4- --> HCl(g) + AlCl3

Now there are a lot of troubles here!
Since the reaction is a specific generating every possibility between monochloro to hexachlorobenzene all isomers and we only need the 1,3 dichlorobenzene.
So here is one of the procedure you can think off:
C6H6 + HNO3 dil -heat-> C6H5-NO2 + H2O
C6H5-NO2 + Fe + HCl dil -Boil-> C6H5-NH2
C6H5-NH2 + HNO3 dil -heat-> metanitraniline
mO2N-C6H4-NH2 + Fe + HCl dil --> metadiaminobenzene (mNH2-C6H4-NH2)
Or Conc HNO3 + H2SO4 + C6H6 --> m-dinitrobenzene
mNO2-C6H4-NO2 + Fe + HCl dil --> mNH2-C6H4-NH2
NH2-C6H4-NH2 + NaNO2(aq) + HCl(dil) + 2CuCl --> via a didiazoniumchlorine salt --> Cl-C6H4-Cl
Even better
NH2-C6H4-NH2 + NaNO2(aq)+ H2SO4 dil -boil-> resorcinol (also via a diazonium salt)

If you have m-dichlorobenzene you simply trinitrate it with H2SO4/SO3 and HNO3conc and get trinitrodichlorobenzene. You boil this in alkaline water (H2O or H2O/Na2CO3 or NaOH) and you get the TNR.

There is a lot of possibilities when you know more about organic chemistry...



------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[PHILOU Zrealone]

Read aspecific instead of a specific

------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[Hex]

Philou,

Interesting, but aniline nitration isn't that easy, I think. I reckon you'd have to deactivate that amine by acetylation before you could nitrate it without ending up with an oxidised mess. Like I said before - probably best to stick to good old lead picrate!!

[CodeMason]

I'm sure I've seen "dichlorobenzene" written on the packet of modern mothballs.

[Alchemist]

It's Para-DichloroBenzene!

[CodeMason]

Is that para as in a polymer like paraformaldehyde, or para as in the placement of the chloro radicals on the benzene ring? If the latter, does it -REALLY- make that much of a difference? I think not, except in terms of relative reactivity. http://theforum.virtualave.net/ubb/smilies/tongue.gif

[Hex]

I'm sure it will refer to chloro-orientation on the ring. I don't really know how much difference it would make. Probably not much in the nitration steps, but positioning of the -O 's in the final product may be important in formation of the salt with lead, depending on how "salt like" lead TNR is...some organo-lead compounds show typical covalent properties.

[Alchemist]

Hello all,

It is the chloro-orientation and it does make a differance! How much??? Try it and let us know. I have been wondering what to use MOTH Balls For anyway! Good luck!

[THe_rEaL_dEaL]

para-dcb is found in levels >90% in urinal deodouriser cakes.

[Zeitgeist]

http://www.powerlabs.org/chemlabs/styphnic.htm

A synth of Styphnic acid from Resourcinol