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Author: Subject: Trinitrophenol (TNP)
DeusExMachina
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[*] posted on 5-1-2003 at 09:16
Trinitrophenol (TNP)


Has anyone tried making this? As soon as I get the chance, I am going to get a whole bunch of chems and make this and a few other stuff. I was wonering if anyone here has tried making this. Please tell me about your experience with making/detonating TNP. To make it you need KNO3, H2SO4 and ASA.
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[*] posted on 5-1-2003 at 12:57


Check out the thread in this section "Picric Acid and the Mystery of the Red Goo".



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[*] posted on 5-1-2003 at 20:11


This might help you a bit. I don't know what you're looking for though.

http://www.roguesci.org/ubb/ultimatebb.php?ubb=get_topic;f=6...

For some reason, this link was to a picric acid thread, but now leads to something on North Korea. Sorry!.

[Edited on 21-3-2003 by Haggis]
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[*] posted on 5-1-2003 at 21:21


Keep in mind it is highly toxic and to wear the adiquit protection when making it.

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[*] posted on 5-1-2003 at 23:06
I made it


I had made TNP before. I used brainfevers methoh. First I took 10 grams of ASA and added it to 120ml of 93% H2SO4 then I heated it to 80*C. After that it is dissolved. The color of the soloution changes color.Then I add 20 grams of KNO3. Gram by gram and after each addition HNO3 fumes is given off.While you are adding and yuo are done the soloution turns brown. Then wait till the soloution cools to room temperatures and the soloution turns orange. After its cooled I added it to 1000ml of cold water. Heat will be generated. Then I put the soloution in the fridge and let all the TNP percipitate over night. After that I filter the TNP with filterpaper. This is the painful part. Then after that I let it sit outside in the sun to dry. It takes a while to dry. My TNP had been sitting outside for 6 days now and it still moist.



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[*] posted on 24-1-2003 at 15:23


Is it nessary to use ASA or can you just add the unpurified asprin?

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[*] posted on 24-1-2003 at 16:16


Aspirin is acetylsalicylic acid with small amounts of impurity (usually calcium phosphate and starch). When I prepare picric acid, I don't bother to purify the acetylsalylic acid in the aspirin. I grind up the aspirin and use as-is.



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[*] posted on 24-1-2003 at 20:16


Yes the other binders and shit is a very small amount. They will get nitrated and the yield of TNP will be SLIGHTLY smaller but nothing to worry about.
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wink.gif posted on 21-2-2003 at 17:21
Here's my batch


I made a batch recently with about 15 g Salicylic acid. It is way cheaper and easier than using ASA.

DSCF0002.JPG - 125kB




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[*] posted on 23-2-2003 at 20:05
I am sorta confused


On quite a few references I have seen ... Trinitrosalicylic acid and its salts (esp.Pb) to be explosive. So how do I know if I have TNP in that pic or TNSA. Is there some sort of test, that someone can suggest, that I can perform, which will be accurate enough to tell me what it is ?



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[*] posted on 19-3-2003 at 08:55


TNASA should be HO-C6H(NO2)3-CO2H and weight 273g/mol
TNP is HO-C6H2(NO2)3 and weight 229g/mol

The first one is a biacid while the second one is a monoacid!
A simple titration of a known dry amount of the solid should answer!
Ex use a 20ml 0,01 mole solution of the acid and titrate with a 0,01 mole solution of NaOH!
If it is the first acid you will need nearly 40ml, while if it is the second one you will need 20ml!

Anyway since we don't know your process of making, a possible side product is dinitrosalysilic acid!




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[*] posted on 22-3-2003 at 06:57


i ve recently tried to do this i used 10grs salicilic acid 16 gr NaNO3 and 55ml 96%H2SO4 is still drying but i ve never try to detonate a high explosive so im not sure about how will it work
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[*] posted on 22-3-2003 at 11:01


I would recommend not making any high explosives yet, menchaca, because you need a primary to 'detonate a high explosive'. This sounds like your first time with a synthesis so I assume you don't have any primaries laying around. Also, I wouldn't want to store it. If you just really like the chemistry part, make it, enjoy it, and destroy it. If you want to use it as an explosive, I reccommend that you get a stronger base in high explosives first.
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[*] posted on 19-11-2003 at 11:00


;)
http://www.powerlabs.org/chemlabs/picric.htm
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[*] posted on 24-11-2003 at 10:48
carbolic acid


Phenol, C6H5OH, is also commonly known as carbolic acid. Well I found a disinfectant at a supermarket called 'Jeyes Fluid' which on the container states; 'CARBOLIC ACID COEFFICIENT 4 TO 6'
It's a black liquid with a tar-like odour. When mixed with water it goes milky white. I was wandering if anyone has encountered such a product and if it is possible to extract the phenol, if it is phenol??




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[*] posted on 24-11-2003 at 14:37


That means that it is 4 to 6 times better at killing bacteria than phenol. That, in turn means it isn't phenol. IIRC it's a mixture of cresols and soaps.
There may well be some phenol in it but it would be tricky to isolate it.
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smile.gif posted on 24-11-2003 at 15:41
TNP production


well, lately I've been producing alot of piceric acid useing the method posted above, powerlab's method, but I scale it up a bit to suit my applications - 40 grams of ASA are disolved in 80mls of hot 95% H2SO4 and once its disolved, chill it down to 10*C, then add 120mls of 70% HNO3, a big reaction will happen, once the reaction has ended you should mix it to get all the NO2 out then dump in an equal amount of H2O this will precipitate the picric acid which is filterd and washed with a bit of water. this synthasis yields around 46g of TNP after pureification. :cool:

TNP.jpg - 171kB




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[*] posted on 25-12-2003 at 15:44


I would purify the apirin anyway, you just dissolve it hot alcohal, filter it, and evaporate the filtrate. Not too much trouble, but yields are bit better.



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[*] posted on 25-12-2003 at 16:14


JDP getting high TNP yields are always fun like that...getting a nice fluffy layer of stuff on the bottom. Your TNP looks pretty crystaline. Mine has always been soft fluffy powder. Is it because of your purification steps?

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[*] posted on 25-12-2003 at 19:41


Yeah, that TNP batch was quite crystaline, and as you guessed it is because of my pureifaction procedure - recristalisation from a solution of acetone and water. Moastly I was going for the highest pureity, for picerate salts. upon cristalition from the acid mix it was a finer product aswell as larger cristals.:)



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[*] posted on 28-12-2003 at 21:02


This project has been resting for a while only because of the great dissappointment which it was.
10g ASA was dissolved in 33ml conc. H2SO4. In retrospect this was probably too little acid since at ~10 mins under heating fine crystals started to appear at the surface of the solution. To attempt to remedy the situation an addition 7ml acid was added. From here the KNO3 was slowly added, with no real noticible change other than the evolution of HNO3 vapors. The mix was heated to 50C and stirred for about 1hr. 20 min by hand until foaming was no longer noted. The color gradually changed from black to dirty yellow. The mix was precipiated and recrystalized which gave a final yeild of 5g after recrystalization from 1:2 ethanol/H2O.

Now the problem is that the flame test of this material does hardly anything. No flames or drama as shown in the powerlabs videos. It simply glows red for a bit and evolves large quantities of black ash resembling very much those lame "Black snake" fireworks. The appeareance seems to be right, though it seems to be a slightly darker shade than the pics which have been posted.

My guess is that it consists of mononitrophenols and dinitrophenols, anyone care to hazard a guess of what happened?

TNP_Attempt.jpg - 14kB
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[*] posted on 28-12-2003 at 22:06


1. Did you purify your asa in alcohal?
2. You need more sulfuric acid per acetylsalysylic acid. The ratio of sulfuric acid in mL to grams of asa should be at least 4:1 from the start, maybe even more like 5:1 or 6:1 (this is most likely your problem, you did not have enough sulfuric acid to catalyze the reaction thus the incomplete nitration).
3. Before adding the asa to the sufuric acid did you heat it to 60-70 degrees?
4. How much potassium nitrate did you add? Ratio of potassium nitrate to asa should be ~ 2:1 by mass(temperature should rise above 70 during the addition, without additional heating).
5. 1 hour and 20 minutes might be too long, add 1 gram potassium nitrate per minute which would give you about 20 minutes, then don't keep it sitting for one hour, cool it to room temp and dump it in water, no additional heating is needed after all the potassium nitrate dissolves.

[Edited on 29-12-2003 by Mendeleev]
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[*] posted on 28-12-2003 at 22:33


The first time I tried TNP it worked great. And then the tries after that not so great. Now that you mentioned it Mendeleev I was using as little H2SO4 as possible, but why the excess acid?
I notice that the ratios you give for the SA and ASA are not in accordance with what powerlabs states;- 0.5g ASA per 1ml H2SO4. I'm sure both ratios would give different yields. There must be an optimum.
The last batch I made was BRIGHT yellow and it burns but I don't think it's pure TNP.

[Edited on 29-12-2003 by froot]




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[*] posted on 29-12-2003 at 12:51


The ASA was painstakingly purified using hot acetone. The sulfuric was heated for at least 10 minutes when the ASA dissolved, and heating was continued until the acetic acid odor was not noticible. The temp only increased slightly when the KNO3 was added and heating was continued even after, with stirring since the evolution of gas continued, as the color slowly changed to a dirty yellow.

This was a long time ago and am only following notes, I guess it can be chalked up to not enough H2SO4 being used. It seems like an excessive amount to use, would there be any way of recycling it after the rxn? Boiling it back down to reconcentrate it and filtering through glass wool would seem to work, but does this seem like it would be safe because of the residual TNP in the boiling acids?
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[*] posted on 29-12-2003 at 14:13


Froot:
Sulfuric acid due to its hygroscopity serves as a catalyst in nitration reactions, because it takes away the water produced and thus maintains a high concentration of nitric acid in the system so that the system does not reach equilibrium due to low nitric acid concentrations. Nitrations of aromatic hydrocarbons are more problematic than nitrations of other hydrocarbons(I think it has something to do with the high electron density inside the ring) and thus require more nitric acid/catalyst, and so you just need a lot of sulfuric acid for their nitrations. Even so its lucky phenol can be trinitrated through one nitration unlike benzene, toluene, and xylene. Furthermore in using acetylsalicylic acid, some of the sulfuric acid is used to split of acetic acid and sulfonate the asa. Also this nitration proceeds at higher temperatures then say nitroglycerine, so more nitric acid decomposes into NO2 and water. I am not very familiar with powerlab and where they got their ratios, but it seems to me they don't have enough sulfuric acid.

blazter:
Your dissolved TNP would contaminate other nitrations if you attempted to reuse it for that purpose, however if you decided to use it to distill nitric acid, the picric acid would not distill over, and yet you would still be getting use out of your sulfuric acid.




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