TNP (Trinitro-Phenol [Picric Acid]) Synthesis from Phenol

[killer666]

I have searched for something like this but I haven't found anything. I have tried to make TNF from phenol, SA and ammonium nitrate, but the result was very disappointing. I dissolved 95g phenol in 300ml hot SA and let the mixture to cool(15 centigrade). Then I began to add slowly 240g NH4NO3 keeping the temperature lower than 20 centigrade. After all the nitrate was added I left the mixture for 15-20 minutes and them poured it in 1.5l cold water. The water became yellow and there was foam of TNF ot the top, but nothing more. What's wrog?

[VinniBOOM]

TNF? You mean TNP (Trinitrophenol).
If so, then here's my synthesis:

Slowly add 14 grams ASA (Acetyl salicylic acid) to 60ml of 98% H2SO4 at 70°C and then cool to 50°C. Now add 25 grams of KNO3 gradually and stirring the solution. You should not see the formation of NO2 fumes, just nitric acid vapours due to decarboxylation. When all the KNO3 has been added cool the solution to room temperature. Now dump it into half and litre of water with crushed ice and let the TNP crystals precipitate. They should be light yellow. Filter the crystals once the ice has melted. DO NOT heat the solution to speed up the process of the ice melting. The liquid is corrosive, be careful. The filtered crystals should then be added to 100ml of boiling water in a glass beaker (400ml) and after five minutes of boiling, cool them in a refrigerator, filter and leave them to dry.

Note: Extra TNP crystals can be made by heating the solution after they are filtered to crystallise more yield as some TNP crystals may have dissolved. However, it is not necessary.

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Is this an original synthesis developed by you, or one you COPY/PASTE'd from elsewhere? NBK

[VinniBOOM]

It was developed by me. Obviously I researched on the net, but didn't steal any shit from anywhere.

[Marck]

I have nerver seen a synthesis of TNP like that. The acethyl salicylic acid process will generate most of its own heat. The Phenol or salicylic acid synth. requires that the mixture is stirred and gently heated to 95 - 100 degree centigrade to nitrate TNP. A correct calculated synth. will increase the yield. I don`t have expierience if this can work with ammonium nitrate.

He, what should this mean you can not see the formation of NO2 fumes?

I would mean you need around 300 mL of 95 - 98% sulfuric acid to nitrate 14 g of ASA with KNO3. I don`t have expierience if this can work with ammonium nitrate.