Morrigan
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posted 02-08-2001 07:31 AM
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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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posted 02-08-2001 07:50 AM
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Doesn't it just mean you add the phenol to the H2SO4, and heat until it's dissolved?


wantsomfet
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posted 02-08-2001 09:29 AM
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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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posted 02-08-2001 03:07 PM
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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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posted 02-08-2001 05:14 PM
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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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posted 02-09-2001 02:38 PM
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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
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posted 02-11-2001 07:14 AM
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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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posted 02-11-2001 09:28 AM
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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
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posted 02-13-2001 10:23 AM
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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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posted 02-13-2001 02:15 PM
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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
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posted 02-15-2001 01:35 PM
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Could anybody tell me a safe and efficient way to store picric acid? (should have thought of this earlier...)


wantsomfet
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posted 02-15-2001 04:41 PM
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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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posted 02-16-2001 03:44 PM
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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
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posted 02-17-2001 01:16 PM
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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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posted 02-17-2001 01:25 PM
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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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posted 02-18-2001 07:33 AM
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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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posted 02-18-2001 08:29 AM
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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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posted 02-18-2001 09:22 AM
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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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posted 02-18-2001 10:03 AM
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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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posted 02-18-2001 04:31 PM
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What will be the best concentration of nitric acid used in the process?


Morrigan
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posted 02-19-2001 09:27 AM
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The higher the better, but concentrated should work


PHILOU Zrealone
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posted 03-15-2001 03:32 AM
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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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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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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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pete
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From: u.k
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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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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
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posted 04-02-2001 07:05 PM
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Isn't NaNO3 a nitrate...?
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Anthony
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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?!

Alchemist
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From: Woodland hills,Ca.,L.A.
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posted 04-04-2001 10:09 PM
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Hello all,
Here is a good lab method that works;

Lab Preparation of Picric Acid

In a small test tube prepare a solution of 0.2 grams of phenol in 4 ml of concentrated sulfuric acid. By means of a dropping tube add this solution drop by drop to a 25 x 200-mm. test tube that contains a mixture of 4 ml. of concentrated nitric acid and 4 ml. of concentrated sulfuric acid. Set the large tube into a beaker of hot water (80�-100�) for 5-7 minutes and then pour the contents carefully into about 75 ml. of cold water. When the mixture has cooled, collect the precipitated picric acid upon a Biichner or Hirsch funnel and wash it with a little water. If desired, the picric acid may be recrystallized from 8-10 ml. of boiling water containing 1 ml. of concentrated hydrochloric acid. Picric acid melts at 122�.



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PHILOU Zrealone
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posted 04-06-2001 07:09 AM
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If I'm right, Alchemist meaned 2.0g and not 0.2g of phenol....
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Alchemist
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posted 04-06-2001 07:06 PM
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Opps, thats right, 2.0 grams not 0.2 grams. Sorry!!!!
Thanks PHILOU !

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Dhzugasvili
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posted 04-15-2001 05:18 PM
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I have made PA many times and with great yields, I could give my recipe if anyone expresses desire. But as for the sensitivity, brisancy, and storage properties of PA, It is very brisant, usually less than 1.5g of MF could detonate it if placed in a small tube made of paper. ONe time I made it and surprisingly enough, it was very NOT brisant, and I still follow the same procedure, I don't know the reason for this but will keep looking. IT is not too sensitive, but if you touch a PA crystal with the red hot part of a match, it will melt and detonate. I have crushed the whole yield to face powder consistency, and not experienced any problems besides a couple of stains. I have stored it up to three weeks with no problems or noticeable degradation, just keep it in a PLASTIC container, sealed would be good, water slowly dissolves it so forget storing with water.


Chainsaw
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From: Estonia
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posted 04-16-2001 10:30 AM
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today i tried to make PA... snow-like yellow crystals... like mess... showed as soon as i dumped acid-solution into cold water. i tried to filter this snow out but no use... this snow went through my filter and evenually i got pissed and throw it away.
I'd like to know if this snow was PA and if it was then how could i get it out... i used paper coffe filter.



wantsomfet
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posted 04-16-2001 07:25 PM
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Too much water - not enough PA.
Cool down to lower temperature.
If done right, you can filter PA through ordinary coffee filterpaper.

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Kroways
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posted 04-18-2001 05:52 PM
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All> If you make picric acid, try to make it pure(recrystalize it) and cast it. If it is cast(I haven't tried simple PA but a mixture of 65% PA with 30% tetryl and %DNT) the brisance is VERY HIGH. If I compare to a plastic obtained by mixing 80% PETN and 20% plastifier it is by at least 20% more brisant. DO NOT melt PA if you are not sure is is PA and if it is impure. If you add a small quantity of DNT(5% is enough) you lower the melting temperature and the process can be done on the water bath. Addition of some soluble salts with small molecular mass(for example NaNO3) is necessary to raise the boiling point of water. If it is done this way, you can be sure the temperature won't rise too high(pure picric acid detonates when heated to approx. 300�C) and the process is relatively safe. With a film can filled with cast mixture as above(65% PA, 5% DNT and 30% tetryl) i have made a 3cm hole in 15mm thick steel plate without any shaping(simple cylinder). If you use pure picric acid, the brisance will be slightly lower(by cca 5-10%) and it will be harder to detonate it(when cast, the density is about 1,65-1,7g/cm^3) due to high density. An apropriate amount(10g) of crystalline(pressed) PA should be used, if you don't have better booster(PETN, RDX, tetryl..) If you have any questions, don't hesitate to write me.
I have also tried a mixture of picric acid with anhydrous nitric acid. You maybe know it as "HELLHOFFIT" because some guy named Hellhoff invited it. This mixture contains 58% picric acid and 42% 95-100% HNO3. The VOD(do you call it so?) is cca 7600m/s and density about 1,5. It is actually a solution of picric acid in nitric acid, because if you stir it(temperature about 20�C) for a while the PA dissolves in NA. The brisance is almost the same as cast picric acid. BUT I DON'T KNOW ANYTHING ABOUT THE SAFETY AND SENSITIVITY. I have tried it only once and succeeded, but this mixture can be unstable and sensitive, so don't try to make it if you like your fingers/hands. The information I have about this solution is old and incomplete, so it was a risk to make it. If you have any additional info I would be very happy if you sent it to my e-mail address.
Other good use of picric acid is to mix it with ammonium nitrate by various ratios(from 10% to 50% of PA). If you use cca 100g of mixture like this(for example 20g of PA + 80g of pure and dry AN) you get a quite powerful booster, which is capable to bring almost ANY ANFO to detonation. I haven't had any failure with ANFO, when used similar boosters. It is neither necessary nor reccommended to press the mixture. It detonates reliably from a 0.5g lead azide detonator. Don't heat or try to melt this mixture, as the picric acid can react with AN forming nitric acid, which can lower the stability. You can store the dry crystalline mixture in a tight plastic container for several months. If you plan to store it longer, it will be always better to transform the acid to ammonium picrate. The mixture of ammonium picrate with AN is known as "Gromobij" and is very stable and safe. The potency of this mixture is quite high, when compared with anfo. If you want to make a cheap and safe explosive, try the mixture of 85% AN with 10% DNT and 5% Al. But that is another topic..
[This message has been edited by Kroways (edited April 19, 2001).]



Detonator
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posted 04-19-2001 04:47 PM
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I think using the Acetylslysalic acid for making PA is much easier!



Mr Cool
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posted 04-19-2001 05:43 PM
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If I want to store PA for a long time, I do it as a solution in alcohol and crystalise some out when I want to use it. It's very soluable in alcohol.
So that little bit of DNT helps the PA to melt? That sounds a lot safer than doing it pure. A similar thing can be done with KNO3/sorbitol rocket fuel. Adding a tiny bit of water allows it to be melted in a hot bath of slightly salty water.


Kroways
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From: Czech Republic
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posted 04-20-2001 05:48 PM
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Detonator> Much easier than what?? Than nitrating phenol? Pche(not translated)!

Mr Cool> Picric acid and bulk of other nitroaromates are absolutely stable. There is no need store a solution. If the product is clean(crystallized) in a tight container on a dark place, be SURE you can store it 10 years without change.
I haven't tried to add water to that mixture, it was always dry. Have you tried to add sulphur to stabilise the combustion velocity? It is a patent of our(Czech) modellers. The original composition is 64% KNO3, 27% sorbitol and 9% sulphur. It is ideal for smaller diameters, but the preparetion and filling is much more complicated in comparison with simple KNO3/sorbitol fuel. The mixture has a dough-consistency when sorbitol has molten, and the filling is a bit complicated. And you shouldn't overheat the mixture above melting point of sulfur(~115-120�C), because it forms drops and inhomogeneites. You are to heat above 100�C to be able to mix it thoroughly. All components must be powdered - of course SEPARETELY(?dasher? is ideal). If you make rocket motors of bigger diameters(>40mm), it is not necessary to add sulphur and the fuel performs well. The primary prerequisite are always KNO3 properties. Ideal vessel for keeping the temperature not too high above 100�C is a pot which is used to boil milk - it has double coating and you can pour whatever you want there. I use NaNO3 soulutions of various concentrations.

[This message has been edited by Kroways (edited April 20, 2001).]



Detonator
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posted 04-21-2001 01:30 AM
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Yes Kroways
Much easier than nitrating phenol, what do you think?


Mr Cool
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posted 04-21-2001 11:55 AM
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I read that PA can gradually change to a different allotrope that is less stable because of it's different structure. I don't mind storing TNT, TeNN, TNB etc etc etc


Cyware
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From: Nomatter
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posted 04-21-2001 05:47 PM
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If anybody is interested in a method for PA synthesis from salycilic acid , mail me at cyware2001@yahoo.mail.com


Anthony
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posted 04-21-2001 08:15 PM
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Why don't you post it here for all to see and so it can be discussed?


Alchemist
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From: Woodland hills,Ca.,L.A.
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posted 04-21-2001 09:58 PM
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Hello all,
Yes this sounds good. I have the basic's, but that all!

Salicylic Acid C6H4(OH)(COOH) + 3 Nitric Acid HNO3 --> Picric Acid C6H2(NO2)3OH.

Also using our favorite, Aspirin (Acetylsalicylic Acid)! It can easily be converted to Salicylic Acid as follows;

In a 100 ml flask mix 3 grams of Aspirin with a solution of 10 grams Sodium Hydroxide in 50 ml of water . Attach the flask to a reflux condenser and heat the contents of the flask to boiling for 15 minutes for hydrolysis of the Aspirin. Pour the solution into a beaker, cool it well in an ice bath and acidify it with dilute sulfuric acid. Collect the precipitated Salicylic Acid on a Buchner funnel, and either dry it in the oven or spread it out on a sheet of paper to dry in the air. After recrystallization from hot water, salicylic acid melts at 157�.

Thats it!


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pete
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posted 04-22-2001 05:01 AM
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Thanks, if you description works that will increase yields greatly for all of us, using asprin, it will stop loads of the oxidizing side chain reactions you get with asprin. I'm of to try this, nice one!!!
[This message has been edited by pete (edited April 22, 2001).]



Kroways
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posted 04-22-2001 05:17 AM
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Detonator> I havent't seen any prescript for making PA from aspirine, in which you could produce e.g. 100g PA from reasonable amount of reagents, for reasonable price. I purchased pure phenol for about 4$/kg and acylpyrine is about 50x more expensive. Acids cost less than 1$ a litre so the price of resultant PA is less than 5$/kg. Sorry but how do you produce drinking alcohol? I think purchasing whisky or beer is more convenient than distilling c2h5oh out of cough-drops) HAHA
Mr. Cool> I haven't read anything about the modification change. I suppose there isn't any need to be afraid of this. I can look in the books i have, so that this question can be answered.

[This message has been edited by Kroways (edited April 22, 2001).]



Anthony
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posted 04-22-2001 06:00 PM
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Could a 20% solution phenol (J's source) be sucessfully used for PA? If it would need concentrating what would be the best temperature to distill it at? Could be less expensive (can't buy in bulk here) and trouble some than aspirin.


Cyware
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Posts: 22
From: Nomatter
Registered: APR 2001
posted 04-22-2001 06:15 PM
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0,1 g of salycilic acid is added to 1 ml of nitric acid. A violent reaction will occur, with lots of NO2. After the reaction stops, the salicilic acid will be replaced by some small yelow crystals of nitrosalycilic acid on the bottom of the testube. If you'll add 1 ml of nitric acid again and boil the solution for 5 minutes, the crystals will dissolve and the resulted TNP can be precipitated by dumping the contents of the testtube in 10 ml of cold water.




Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 04-23-2001 01:08 PM
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Does anyone know of a UK source for pure phenol? (Anthony: where is J's source?)
I normally do it with aspirin, but yields are pretty crappy and I can't help thinking that the acetyl group and the carboxyl group or whatever it is on the phenol in aspirin might make some nasty impurities...
I can buy it from a chemical supplier I know of, but I was wondering if there was a better source since A.R. grade phenol is fairly expensive from this place, and it doesn't need to be that pure.

Another question: why have I never heard of TNB, trinitrobenzoic acid? I think it's produced in a method to make trinitrobenzene from TNT, but is benzoic acid nitratable?
All replies greatly appreciated.



Alchemist
Frequent Poster
Posts: 211
From: Woodland hills,Ca.,L.A.
Registered: NOV 2000
posted 04-23-2001 01:13 PM
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Hello Cyware,
What concentraion of Nitric Acid or S.P.?

P.S.,Where did ya find this info. What soure? Name of book, Web sight, etc.?

Thanks................

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Cyware
New Member
Posts: 22
From: Nomatter
Registered: APR 2001
posted 04-23-2001 05:08 PM
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I found this info in a chemistry book. It saids that the acid must be concentrated. I used 65 % nitric acid and it worked. Sadly, you need lots of acid...


Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-23-2001 06:14 PM
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MrCool, J mentioned it ages ago on the last forum but if you got his email the other day, it's in there.


Detonator
Frequent Poster
Posts: 133
From:
Registered: NOV 2000
posted 04-24-2001 01:54 AM
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From:
http://nettrash.com/users/megalomania/picric_acid.html
This procedure uses aspirin tablets instead of phenol. Crush 100 aspirin tablets to a fine powder. Put 500 mL of 95% ethyl alcohol in a 1000-mL beaker then add the aspirin powder. Gently heat the alcohol while stirring to dissolve the acetylsalicylic acid within the tablets for 15 minutes. Acetylsalicylic acid is the active ingredient in aspirin and a phenol derivative. Filter the still hot alcohol to remove any excess tablet filler. Now heat the solution to evaporate off all of the alcohol, leaving behind crystals of acetylsalicylic acid. When the crystals have dried, add them to a 1000-mL beaker with 700 mL of 95-100% sulfuric acid. Heat the acid and stir to dissolve the acetylsalicylic crystals. When all of the crystals have been dissolved, add 75 g of sodium nitrate or potassium nitrate. Add a few grams at a time then wait for the reaction to subside before adding more. The nitrate addition must be done in a well ventilated area as it produces deadly nitrogen dioxide gas. When all of the nitrate has been added, allow the mix to cool to room temperature, stirring it every few minutes. Pour it into 1500 mL of ice water to precipitate the picric acid. Decant about 1000 mL of the acid water mix then add another 1000 mL of water. Filter the solution to collect the picric acid crystals. You may purify the crystals as per method one. You will need a stirring rod or magnetic stirrer for mixing.
the end

I think its easier and doesnt take time.