megalomania
May 10th, 2003, 09:24 PM
Morrigan
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Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-08-2001 07:31 AM
--------------------------------------------------------------------------------
I am trying to make some picric acid for a booster.
Here’s what I have, all chemically pure :
about 61 grams phenol, pink – yellow crystals.
100 ml Sulfuric acid, ranging in concentration from 95-98%
800 ml nitric acid, concentration 65%.
The lab recipe on mega’s site uses phenol in volumes and is just a little more complicated than a recipe I found in a chemistry handbook. It says:
(Translated out of Dutch)
sulphonate (-> not sure I translate this right) 100 grams phenol with 100 grams conc. H2SO4 on a water bath until the product is completely soluble in water. Then add this solution slowly while stirring to 500 grams conc. HNO3. When the reaction reaches completion heat on a water bath; let it cool down when no more nitrogen oxides form, poor of most of the acid and purify the picric acid by re-crystallization.
This process is clear to me except the first part where the phenol needs to be “sulphonated” with H2SO4. On mega’s site the phenol is being refluxed, I do not have the lab equipment necessary for this. Who knows what the first step is about and how it could be done with minimal lab resources, flask, beaker exc.
thanks.
Mr Cool
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From: None of your bloody business!
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posted 02-08-2001 07:50 AM
--------------------------------------------------------------------------------
Doesn't it just mean you add the phenol to the H2SO4, and heat until it's dissolved?
wantsomfet
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Posts: 236
From: EU
Registered: JAN 2001
posted 02-08-2001 09:29 AM
--------------------------------------------------------------------------------
If you start from phenol to produce picric acid, the problem is that much of the phenol is oxidised before its nitrated resulting in a poor yield.
To prevent this the phenol is sulfonised/sulphonated(?) to phenol-2,4 disulfonacid (translated from german...) by dissolving in H2SO4 and heating to 100 C for ca. 1 hour. Thats the industrial process, works fine at home, too.
Here's the link to the original document (fucking omikron-opages...)
http://www.omikron-online.de/cyberchem/cheminfo/0484-lex.htm
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Morrigan
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From: The Netherlands
Registered: OCT 2000
posted 02-08-2001 03:07 PM
--------------------------------------------------------------------------------
Does that also mean that it oxidizes when stored in a container that is not completely air tide? And if so will it become useless?
wantsomfet
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Posts: 236
From: EU
Registered: JAN 2001
posted 02-08-2001 05:14 PM
--------------------------------------------------------------------------------
The phenol isn't oxidised from laying around, i mean when you actually nitrate it. If you dissolve the phenol and add the HNO3 after that (without the heating shit) much of the phenol is oxidised. Therefor the heating procedure.
If not stored airtight it will draw moisture from the air and become liqid after a while....
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Morrigan
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Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-09-2001 02:38 PM
--------------------------------------------------------------------------------
I guess your right. Thanks for helping out. If I heat the H2SO4 it will start fuming big time, so I am gonna lose a significant amount of acid over one hour if I heat it in a flask or beaker, and if I heat it in a closed container I am pretty sure its gonna pop. How do you do it?
Thanks.
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-11-2001 07:14 AM
--------------------------------------------------------------------------------
When i dream of producing PA, i use 96% H2SO4. First time after adding phenol i put it in a water bath and added boiling water every few minutes for about an hour, no fumes observed. No i have a lab-heatplate i put the flask on it and heat to ~85 C for 2 hours, works fine for me & without fuming.
Temp is lower than suggested, but i doubled the time so i think it's OK.
Hope this helps.
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Morrigan
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From: The Netherlands
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posted 02-11-2001 09:28 AM
--------------------------------------------------------------------------------
I can easily get a hot plate so I guess I’ll start dreaming soon, using the recipe I gave above. One more thing, what ratios did you dream about? And how is your yield.
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-13-2001 10:23 AM
--------------------------------------------------------------------------------
Just found this procedure for PA production on the page i linked above, it involves only phenol and *diluted* HNO3. Haven't tried it, but it sounds very nice - no need of H2SO4 or concentrated HNO3. I translated it from german, so don't complain
"1g phenol is liquefied(?) by a drop water. This liqid is added *dropwise* and carefull in a 100ml beakerglass to 10ml HNO3 (density 1.30, ca. 48 weight-% HNO3). The mixture will heat up & perhaps release some NOx, work with good ventilation & stir all the time. After complete addition of the phenol the mixture is carefully boiled for a short time, it should look dark-orange. Don't let all liqid evaporate, if too dry add a bit H2O.
While cooling the crude picric acid will fall out of solution. Put the substance on a filter and wash with icecold water. Now the PA can be recristallized from H2O. Yield: about 2g wet PA."
------------------
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Jhonbus
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Posts: 351
From:
Registered: SEP 2000
posted 02-13-2001 02:15 PM
--------------------------------------------------------------------------------
A trick we used for refluxing when it didn't really matter to lose some vapour (non-toxic) was to put a glass funnel in the top of a (tall) beaker that the liquid was heated in. Then vapour would condense on the funnel and run back into the liquid. It's not very efficient but it saved us having to get all the quickfit out.
Morrigan
Frequent Poster
Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-15-2001 01:35 PM
--------------------------------------------------------------------------------
Could anybody tell me a safe and efficient way to store picric acid? (should have thought of this earlier...)
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-15-2001 04:41 PM
--------------------------------------------------------------------------------
Store it under dest. H2O, thats the common way...
http://www.tc.gc.ca/canutec/en/articles/documents/picric.htm
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Mr Cool
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From: None of your bloody business!
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posted 02-16-2001 03:44 PM
--------------------------------------------------------------------------------
Fill the funnel with glass beads or small pieces of glass tubing to condense more of the vapours. A large filtration column full of glass tubing is very good.
Morrigan
Frequent Poster
Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-17-2001 01:16 PM
--------------------------------------------------------------------------------
S.O.S
I just did an attempt to produce picric acid. Here’s the whole story:
Apr. 61 grams of very pure phenol where putted in a 500 ml Erlenmeyer flask.
To this 35 ml of conc. H2SO4 was added. This mixture was heated on a water bath at 90 C for over an hour. It turned into reddish liquid. I didn’t allow this liquid to cool down and added it to 222 ml conc. HNO3. The reaction was very volatile and produced huge amount of NOx. Since it also splattered a lot I decided to cool the liquid down to about 10 C. Than I added the remaining HNO3 to the Erlenmeyer to keep the splattering inside it. NOx production was little. I then heated to total mix to 90*C until the huge clouds of NOx disappeared, what I was left with was a very red solution with a viscose black liquid on the bottom. I cooled it down and noticed that when a drop of this solution was added to water it turned the water completely lemmon yellow like PA should do. This stained everything: rags, paper, and wood, even my skin (I was wearing protective gloves but I got some on my arm)
The red solution was allowed to cool, tiny yellow crystals formed but not in large quantities, the black liquid turned black-red and real sticky, now it is like clay. After some time more yellow crystals formed but not by far as much in mass as the black stuff. What is this black clay? I think that the yellow snow-like crystals that precipitated out of the solution is PA but I have no clue about the black-red-brown stuff, could it be dinitrofenol? Can somebody tell me what went wrong? And can I nitrate it further to PA by using conc. H2SO4 and KNO3?
I breathe in some NOx and got PA on my skin, I surely hope that I didn’t got poisoned?
Anthony
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Posts: 2306
From: England
Registered: SEP 2000
posted 02-17-2001 01:25 PM
--------------------------------------------------------------------------------
Did you drown the solution in ice water to precipitate the PA?
I guess if you didn't die when you were inhaling the NO2, then you won't die later.
Mr Cool
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From: None of your bloody business!
Registered: DEC 2000
posted 02-18-2001 07:33 AM
--------------------------------------------------------------------------------
Black stuff could be a sludge of carbon (formed by the dehydration of phenol by H2SO4)in the acid, or it could be a nitrophenol or other nitrated aromatics.
wantsomfet
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Posts: 236
From: EU
Registered: JAN 2001
posted 02-18-2001 08:29 AM
--------------------------------------------------------------------------------
I think you should have cooled the phenol / H2SO4 mix a little bit (let's say to 30 C) before adding the HNO3. You lost big amounts of your HNO3, when the Nox was formed. And i think it isn't necessary to heat the mix after the HNO3 addition. The HNO3 will heat the shit up enough, just let it stand for 60 minutes or so...
Next time try adding the HNO3 very slowly in a room temp phenol/H2SO4 solution...
I personally will turn to the acetylsalicylic acid method, cause phenol is too expensive were i live... (~8 USD per 100g)
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atropine
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From: wales
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posted 02-18-2001 09:22 AM
--------------------------------------------------------------------------------
i will buy some phenol off you for that ammount no problem. It is not illegal here but it as rare as rocking horse shite.
Morrigan
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Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-18-2001 10:03 AM
--------------------------------------------------------------------------------
The black stuff is flammable so my best bet is that it is a mix of nitro & dintrofenol, maybe something completely different but still aromatic I hope. I will try too nitrate it again sometime cause it is way to much to be just a byproduct and as far as I know this reaction has no liquid or solid byproducts. It made quite a mess when I added one drip of HNO3, poef, lots of NOx, I hate the color and smell of that shit. Anyway I have a reasonable quantity of crystals now, still a very shitty yield though, and more important I am still alive and kicking.
I didn’t bought the phenol, I was as free to borough it from the organic lab, I took it out of a 5 kilo jar so nobody will miss it.
If anybody is gonna try to go the phenol way than I would advise you too wear special gloves, goggles, do it in a well ventilated area and take your time. You will know what I mean when you find yourself in the middle of a orange red cloud…
[This message has been edited by Morrigan (edited February 18, 2001).]
simply RED
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Posts: 240
From: HELL
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posted 02-18-2001 04:31 PM
--------------------------------------------------------------------------------
What will be the best concentration of nitric acid used in the process?
Morrigan
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Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-19-2001 09:27 AM
--------------------------------------------------------------------------------
The higher the better, but concentrated should work
PHILOU Zrealone
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From: Brussels,Belgium,Europe
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posted 03-15-2001 03:32 AM
--------------------------------------------------------------------------------
I don't understand the guy! We give him a recipe and he doesn't follow it;
usually aromatics need for 1g at least 2g conc HNO3 and 6g conc. H2SO4. So you really think you can make TNP with 61g phenol, 35g conc H2SO4 and 222g HNO3....
I once did a mix of 1g phenol and 2ml of HNO3(70%) and it blew out of the test tube in less than 1/2 second in a hot bubbling black brown pasty liquid (I was nearly burned... so be carreful guys). Why did I did this, simply because I knew phenol was much more reactive than benzene or toluene (which are nitrated by conc HNO3/H2SO4) thus I tought 70% without H2SO4 could work to give me first nitrophenol or dinitrophenol... actually phenol is so reactive that a lot of heat is released and decompose HNO3 in NyOx instantaneously; results are a little TNP, some DNP and NP aside with oxydation products of phenol like quinons... the all thing makes a black pastefrom which products are difficult to separate
BTW:
NP, DNT and TNP all three are white-yellow cristalls and does color skin, water and basic solution in yellow... so it is no proof of TNP being there.
------------------
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Morrigan
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Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 03-15-2001 08:10 AM
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First of, yes I have been ignorant. I recently checked out Vogel Third edition (10gr Phenol-23gr H2S04-55gr HNO3, so you are right about the ratio’s) I was completely wrong throughout the process. The amounts were too big, the ratios wrong and the HNO3 added to fast. I wanted too much at once and to fast and I felt the consequences. I hope and think I learned a lot out of this Kewl attempt. I hope I didn’t insult anybody. I got rid of all the reaction products since purifying was useless. I thought it would be an easy reaction and therefor I didn’t bothered too much with the whole process. This was painfully wrong and now I could smack myself down with a hammer for wasting the chemicals and risking my health.
PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 03-15-2001 10:14 AM
--------------------------------------------------------------------------------
And your life!!! 61g of TNP in a first shot is quite suicidal....never forget better make several little batches than a big one!!!! On a small batch cooling is much more controled an manageable than with a big batch!!!!
The main problem in this field is that everybody (me,you,...included) learn one day of another to follow the safety rules mainly because of an accident, a runaway, an explosion or a detonation...it is often when you think you masterise the all process that taking less care, making a scaling up without thinking to the effect on heat dispersion, cooling efficience, stirring efficience, that the explosive devil kick you in the back to remind you who is the real boss...
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
pete
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Posts: 56
From: u.k
Registered: JAN 2001
posted 04-02-2001 02:38 PM
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I have been reading about others atempts to make picric acid, so i will post my attemps. I took loads of asprin tabs, dissolved then in alcohol extreacted the bit we are looking for( i know what its called but can not spell it, sorry). I took 40 grams of this dry material and added it to 150 ml of 98 percent conc sulphuric at 120 degrees cel. It smoked a little, after sturring the black liquid was heated till it started to smoke again. The heating was stopped, now small amonut of NaNO3 was added in a maner to prevent over flow due to foaming and to maintain the solutions temp. The addtion was continued till the solution went solid, from Na2SO4 ptt etc. This was then left to cool, to this was added 300 ml of ice. After the ice has melted and a good stir the mix was filltered, the filtrate was washed with 200 ml of cool water. The filtate was then press dried, before recrystalation from ethyl alcohol. This was dried throughly in a desicator, the product weighed 36.3 grams. It was found to be pure, and reacted just as it would be expected to.
Anthony
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Posts: 2306
From: England
Registered: SEP 2000
posted 04-02-2001 03:13 PM
--------------------------------------------------------------------------------
How could you have nitrated the phenol to picric acid without a nitrate or HNO3?
wantsomfet
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Posts: 236
From: EU
Registered: JAN 2001
posted 04-02-2001 07:05 PM
--------------------------------------------------------------------------------
Isn't NaNO3 a nitrate...?
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Anthony
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Posts: 2306
From: England
Registered: SEP 2000
posted 04-02-2001 07:47 PM
--------------------------------------------------------------------------------
I'm really on a roll today... I need to get my eyes checked, that "3" in NaNO3 looked like a "H".
See what this forum colour scheme has done to my eyes?!
Frequent Poster
Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-08-2001 07:31 AM
--------------------------------------------------------------------------------
I am trying to make some picric acid for a booster.
Here’s what I have, all chemically pure :
about 61 grams phenol, pink – yellow crystals.
100 ml Sulfuric acid, ranging in concentration from 95-98%
800 ml nitric acid, concentration 65%.
The lab recipe on mega’s site uses phenol in volumes and is just a little more complicated than a recipe I found in a chemistry handbook. It says:
(Translated out of Dutch)
sulphonate (-> not sure I translate this right) 100 grams phenol with 100 grams conc. H2SO4 on a water bath until the product is completely soluble in water. Then add this solution slowly while stirring to 500 grams conc. HNO3. When the reaction reaches completion heat on a water bath; let it cool down when no more nitrogen oxides form, poor of most of the acid and purify the picric acid by re-crystallization.
This process is clear to me except the first part where the phenol needs to be “sulphonated” with H2SO4. On mega’s site the phenol is being refluxed, I do not have the lab equipment necessary for this. Who knows what the first step is about and how it could be done with minimal lab resources, flask, beaker exc.
thanks.
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 02-08-2001 07:50 AM
--------------------------------------------------------------------------------
Doesn't it just mean you add the phenol to the H2SO4, and heat until it's dissolved?
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-08-2001 09:29 AM
--------------------------------------------------------------------------------
If you start from phenol to produce picric acid, the problem is that much of the phenol is oxidised before its nitrated resulting in a poor yield.
To prevent this the phenol is sulfonised/sulphonated(?) to phenol-2,4 disulfonacid (translated from german...) by dissolving in H2SO4 and heating to 100 C for ca. 1 hour. Thats the industrial process, works fine at home, too.
Here's the link to the original document (fucking omikron-opages...)
http://www.omikron-online.de/cyberchem/cheminfo/0484-lex.htm
------------------
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Morrigan
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Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-08-2001 03:07 PM
--------------------------------------------------------------------------------
Does that also mean that it oxidizes when stored in a container that is not completely air tide? And if so will it become useless?
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-08-2001 05:14 PM
--------------------------------------------------------------------------------
The phenol isn't oxidised from laying around, i mean when you actually nitrate it. If you dissolve the phenol and add the HNO3 after that (without the heating shit) much of the phenol is oxidised. Therefor the heating procedure.
If not stored airtight it will draw moisture from the air and become liqid after a while....
------------------
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Morrigan
Frequent Poster
Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-09-2001 02:38 PM
--------------------------------------------------------------------------------
I guess your right. Thanks for helping out. If I heat the H2SO4 it will start fuming big time, so I am gonna lose a significant amount of acid over one hour if I heat it in a flask or beaker, and if I heat it in a closed container I am pretty sure its gonna pop. How do you do it?
Thanks.
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-11-2001 07:14 AM
--------------------------------------------------------------------------------
When i dream of producing PA, i use 96% H2SO4. First time after adding phenol i put it in a water bath and added boiling water every few minutes for about an hour, no fumes observed. No i have a lab-heatplate i put the flask on it and heat to ~85 C for 2 hours, works fine for me & without fuming.
Temp is lower than suggested, but i doubled the time so i think it's OK.
Hope this helps.
------------------
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Morrigan
Frequent Poster
Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-11-2001 09:28 AM
--------------------------------------------------------------------------------
I can easily get a hot plate so I guess I’ll start dreaming soon, using the recipe I gave above. One more thing, what ratios did you dream about? And how is your yield.
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-13-2001 10:23 AM
--------------------------------------------------------------------------------
Just found this procedure for PA production on the page i linked above, it involves only phenol and *diluted* HNO3. Haven't tried it, but it sounds very nice - no need of H2SO4 or concentrated HNO3. I translated it from german, so don't complain
"1g phenol is liquefied(?) by a drop water. This liqid is added *dropwise* and carefull in a 100ml beakerglass to 10ml HNO3 (density 1.30, ca. 48 weight-% HNO3). The mixture will heat up & perhaps release some NOx, work with good ventilation & stir all the time. After complete addition of the phenol the mixture is carefully boiled for a short time, it should look dark-orange. Don't let all liqid evaporate, if too dry add a bit H2O.
While cooling the crude picric acid will fall out of solution. Put the substance on a filter and wash with icecold water. Now the PA can be recristallized from H2O. Yield: about 2g wet PA."
------------------
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Jhonbus
Frequent Poster
Posts: 351
From:
Registered: SEP 2000
posted 02-13-2001 02:15 PM
--------------------------------------------------------------------------------
A trick we used for refluxing when it didn't really matter to lose some vapour (non-toxic) was to put a glass funnel in the top of a (tall) beaker that the liquid was heated in. Then vapour would condense on the funnel and run back into the liquid. It's not very efficient but it saved us having to get all the quickfit out.
Morrigan
Frequent Poster
Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-15-2001 01:35 PM
--------------------------------------------------------------------------------
Could anybody tell me a safe and efficient way to store picric acid? (should have thought of this earlier...)
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-15-2001 04:41 PM
--------------------------------------------------------------------------------
Store it under dest. H2O, thats the common way...
http://www.tc.gc.ca/canutec/en/articles/documents/picric.htm
------------------
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Mr Cool
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Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 02-16-2001 03:44 PM
--------------------------------------------------------------------------------
Fill the funnel with glass beads or small pieces of glass tubing to condense more of the vapours. A large filtration column full of glass tubing is very good.
Morrigan
Frequent Poster
Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-17-2001 01:16 PM
--------------------------------------------------------------------------------
S.O.S
I just did an attempt to produce picric acid. Here’s the whole story:
Apr. 61 grams of very pure phenol where putted in a 500 ml Erlenmeyer flask.
To this 35 ml of conc. H2SO4 was added. This mixture was heated on a water bath at 90 C for over an hour. It turned into reddish liquid. I didn’t allow this liquid to cool down and added it to 222 ml conc. HNO3. The reaction was very volatile and produced huge amount of NOx. Since it also splattered a lot I decided to cool the liquid down to about 10 C. Than I added the remaining HNO3 to the Erlenmeyer to keep the splattering inside it. NOx production was little. I then heated to total mix to 90*C until the huge clouds of NOx disappeared, what I was left with was a very red solution with a viscose black liquid on the bottom. I cooled it down and noticed that when a drop of this solution was added to water it turned the water completely lemmon yellow like PA should do. This stained everything: rags, paper, and wood, even my skin (I was wearing protective gloves but I got some on my arm)
The red solution was allowed to cool, tiny yellow crystals formed but not in large quantities, the black liquid turned black-red and real sticky, now it is like clay. After some time more yellow crystals formed but not by far as much in mass as the black stuff. What is this black clay? I think that the yellow snow-like crystals that precipitated out of the solution is PA but I have no clue about the black-red-brown stuff, could it be dinitrofenol? Can somebody tell me what went wrong? And can I nitrate it further to PA by using conc. H2SO4 and KNO3?
I breathe in some NOx and got PA on my skin, I surely hope that I didn’t got poisoned?
Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 02-17-2001 01:25 PM
--------------------------------------------------------------------------------
Did you drown the solution in ice water to precipitate the PA?
I guess if you didn't die when you were inhaling the NO2, then you won't die later.
Mr Cool
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Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 02-18-2001 07:33 AM
--------------------------------------------------------------------------------
Black stuff could be a sludge of carbon (formed by the dehydration of phenol by H2SO4)in the acid, or it could be a nitrophenol or other nitrated aromatics.
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-18-2001 08:29 AM
--------------------------------------------------------------------------------
I think you should have cooled the phenol / H2SO4 mix a little bit (let's say to 30 C) before adding the HNO3. You lost big amounts of your HNO3, when the Nox was formed. And i think it isn't necessary to heat the mix after the HNO3 addition. The HNO3 will heat the shit up enough, just let it stand for 60 minutes or so...
Next time try adding the HNO3 very slowly in a room temp phenol/H2SO4 solution...
I personally will turn to the acetylsalicylic acid method, cause phenol is too expensive were i live... (~8 USD per 100g)
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atropine
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Posts: 129
From: wales
Registered: OCT 2000
posted 02-18-2001 09:22 AM
--------------------------------------------------------------------------------
i will buy some phenol off you for that ammount no problem. It is not illegal here but it as rare as rocking horse shite.
Morrigan
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Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-18-2001 10:03 AM
--------------------------------------------------------------------------------
The black stuff is flammable so my best bet is that it is a mix of nitro & dintrofenol, maybe something completely different but still aromatic I hope. I will try too nitrate it again sometime cause it is way to much to be just a byproduct and as far as I know this reaction has no liquid or solid byproducts. It made quite a mess when I added one drip of HNO3, poef, lots of NOx, I hate the color and smell of that shit. Anyway I have a reasonable quantity of crystals now, still a very shitty yield though, and more important I am still alive and kicking.
I didn’t bought the phenol, I was as free to borough it from the organic lab, I took it out of a 5 kilo jar so nobody will miss it.
If anybody is gonna try to go the phenol way than I would advise you too wear special gloves, goggles, do it in a well ventilated area and take your time. You will know what I mean when you find yourself in the middle of a orange red cloud…
[This message has been edited by Morrigan (edited February 18, 2001).]
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 02-18-2001 04:31 PM
--------------------------------------------------------------------------------
What will be the best concentration of nitric acid used in the process?
Morrigan
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Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 02-19-2001 09:27 AM
--------------------------------------------------------------------------------
The higher the better, but concentrated should work
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 03-15-2001 03:32 AM
--------------------------------------------------------------------------------
I don't understand the guy! We give him a recipe and he doesn't follow it;
usually aromatics need for 1g at least 2g conc HNO3 and 6g conc. H2SO4. So you really think you can make TNP with 61g phenol, 35g conc H2SO4 and 222g HNO3....
I once did a mix of 1g phenol and 2ml of HNO3(70%) and it blew out of the test tube in less than 1/2 second in a hot bubbling black brown pasty liquid (I was nearly burned... so be carreful guys). Why did I did this, simply because I knew phenol was much more reactive than benzene or toluene (which are nitrated by conc HNO3/H2SO4) thus I tought 70% without H2SO4 could work to give me first nitrophenol or dinitrophenol... actually phenol is so reactive that a lot of heat is released and decompose HNO3 in NyOx instantaneously; results are a little TNP, some DNP and NP aside with oxydation products of phenol like quinons... the all thing makes a black pastefrom which products are difficult to separate
BTW:
NP, DNT and TNP all three are white-yellow cristalls and does color skin, water and basic solution in yellow... so it is no proof of TNP being there.
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"Life that deadly disease sexually transmitted".
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Morrigan
Frequent Poster
Posts: 81
From: The Netherlands
Registered: OCT 2000
posted 03-15-2001 08:10 AM
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First of, yes I have been ignorant. I recently checked out Vogel Third edition (10gr Phenol-23gr H2S04-55gr HNO3, so you are right about the ratio’s) I was completely wrong throughout the process. The amounts were too big, the ratios wrong and the HNO3 added to fast. I wanted too much at once and to fast and I felt the consequences. I hope and think I learned a lot out of this Kewl attempt. I hope I didn’t insult anybody. I got rid of all the reaction products since purifying was useless. I thought it would be an easy reaction and therefor I didn’t bothered too much with the whole process. This was painfully wrong and now I could smack myself down with a hammer for wasting the chemicals and risking my health.
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 03-15-2001 10:14 AM
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And your life!!! 61g of TNP in a first shot is quite suicidal....never forget better make several little batches than a big one!!!! On a small batch cooling is much more controled an manageable than with a big batch!!!!
The main problem in this field is that everybody (me,you,...included) learn one day of another to follow the safety rules mainly because of an accident, a runaway, an explosion or a detonation...it is often when you think you masterise the all process that taking less care, making a scaling up without thinking to the effect on heat dispersion, cooling efficience, stirring efficience, that the explosive devil kick you in the back to remind you who is the real boss...
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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
pete
Frequent Poster
Posts: 56
From: u.k
Registered: JAN 2001
posted 04-02-2001 02:38 PM
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I have been reading about others atempts to make picric acid, so i will post my attemps. I took loads of asprin tabs, dissolved then in alcohol extreacted the bit we are looking for( i know what its called but can not spell it, sorry). I took 40 grams of this dry material and added it to 150 ml of 98 percent conc sulphuric at 120 degrees cel. It smoked a little, after sturring the black liquid was heated till it started to smoke again. The heating was stopped, now small amonut of NaNO3 was added in a maner to prevent over flow due to foaming and to maintain the solutions temp. The addtion was continued till the solution went solid, from Na2SO4 ptt etc. This was then left to cool, to this was added 300 ml of ice. After the ice has melted and a good stir the mix was filltered, the filtrate was washed with 200 ml of cool water. The filtate was then press dried, before recrystalation from ethyl alcohol. This was dried throughly in a desicator, the product weighed 36.3 grams. It was found to be pure, and reacted just as it would be expected to.
Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-02-2001 03:13 PM
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How could you have nitrated the phenol to picric acid without a nitrate or HNO3?
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 04-02-2001 07:05 PM
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Isn't NaNO3 a nitrate...?
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Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-02-2001 07:47 PM
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I'm really on a roll today... I need to get my eyes checked, that "3" in NaNO3 looked like a "H".
See what this forum colour scheme has done to my eyes?!