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Mononitrotoluene
Outline
Despite what some preceding documents may have stated, crude 2,4,6 TriNitroToluene can be prepared from less concentrated, more commonly available, easily produced acids. The process is a modified three step nitration, whereby Toluene is converted into MonoNitroToluene, Dinitro, and finally Trinitro by the addition of fresh portions of Mixed Nitric/Sulfuric Acid. An external source of heat is neccesary.
Purification is accomplished through the usage of a boiling water liquidation, whereby impurities float to the surface, which are easily decanted. It can be scaled up or down depending upon material availability.
Materiels
Sulfuric Acid 99~%
This can be found in Home Depot, In white plastic containers, marked "Instant Power Drain Opener" marketed By Scotch Corporation Of Dallas, Texas - 64Oz containers of concentrated sulfuric acid found in the plumbing section. It is of 93% purity.
It must be concentrated via heating at 100C+ For 10 minutes. Water will boil off yielding theoretically pure H2SO4 - This should be done OUTSIDE, as all experiments should be. Nitric Acid 70~99 % Concentration
The ~70% Materiel is available commercially, 99~ material is available via 88~C distillation of Potassium or Sodium Nitrate with Sulfuric Acid. The 70% materiel will work, although yields will be less.
Toluene
This is found in the Solvent section of Home Depot in gallon cans. It is used as a specialty solvent. ACE may carry it if it is unavailable in Home Depot
3 Glass, heat resistant containers(Pyrex, Kimax Beaker or Flask Preferably)
Acid Resistant Volume Measurement device(Graduated Cylinder Or Etched Beaker)
Glass Stirring Rod
Plastic Spaluta
Plastic Baster
Heat Source
Thermometer(Optional) This item would greatly increase reproducibility - But TNT Will still form without careful temperature control and based on subjective sensory perception. Celsius has been included for those who do have the luxury of a thermometer. TNT is not a sensitive HE and thus there is no danger of temperature based runaway reactions leading to detonation.
Procedure
Measure Out 300 Milliliters Of ~99% Sulfuric Acid into the heat resistant glass container. It should be able to hold at 1000 ML. Add To This 100 Ml Of Nitric Acid 70%. If One is using 99~ Distillation Acid then 75 ML Of That should be used. Or .75
This is the standard ratio 3/1 Or .75 If 99~ Acid is used. Heat will be generated upon the Nitric acid mixing with the Sulfuric acid and a cloud of barely visible white N0x should be seen wafting over the vessel. Now One adds 100 Milliliters of Toluene. Upon The Toluene contacting the mixed acid, it will convert to a yellowish/Red oil which will float on the surface of the acids - Large Amounts of heat will be generated - This is Good. Just let the vessel sit alone untouched reacting for 2 hours. A very noticeable odor shall appear - This is due to MNT. Do NOT confuse this with the odor of Reddish/Brown N02 which may begin to bubble off the beaker when the reaction temperature reaches a climax. Some reckon it smells like "shoe polish", While others relate to it smelling "Almondish". Personally, it has a completely distinct smell that i do not feel is adequately characterized by any particular description. Let it react for 2 hours
The MNT will be a Aromatic oil on the surface of the acids. It should now have turned cold - Temperature must now be maintained externally. With a bunsen burner, alcohol lamp, or other heating device, heat the beaker to 80C~. If you lack a thermometer, It should be heated to the temperature of the beaker during the vigorous reaction. By this i do not imply one wait around while it is reacting, as Volumes of Nitrogen Dioxide, a reddish Brown gas, is produced, which is quite toxic and will produce pulmonary edema which may go unnoticed for a week, at which point one may die. This does not mean you will die if you take a little whiff, No, But common sense dictates that one should distance themselves from the vessel while it is reacting and avoid inhaling any fumes. It is heated externally for 30 minutes. Now using the Plastic Baster, suck up as much of the now dilute acid from the container and transfer to another suitable container for recycling(See Below) Or should be disposed of properly. Try not to get any of the MNT in with the acid, this will take practice. Now In another container mix another batch of 3/1 acid and add this to the MNT. Repeat above steps involving 2 hour wait and 30 minute external heating. Remove spent acid and add to portion of spent acid recovered form MNT nitration. The DNT will be a Yellow oily liquid, or a waxy yellow solid. Now Comes the final nitration. To The DNT is added a fresh portion of 3/1 acid.
The vessel will get hot and when it cools after 2 hours yellow needles may be visible in addition to some DNT. After allowing the vessel to react for 2 hours, external heating should be applied for 1 hour. When heating is removed the insoluble oil floating on the surface will solidify as it cools, forming a yellow crystalline cake, with many yellow needles embedded into it - This is TNT. Earlier methods involved filtration, but due to economic reasons good filter paper is not used, instead coffee filters - Since corrosion of the cellulose based filters has been shown, a spatula is used to "Fish out" The cake from the surface of the acid and into a separate plastic container like a cream cheese container. This can be done by tilting the container gently and sliding the cake along the side of the vessel and into the empty plastic container.
Purification
The empty cup with the fragments of cake, acid, is covered in about 150 ML Of boiling water - This will melt the TNT into a puddle under the water and cause insoluble droplets of DNT impurity to float onto the surface as an oil. Any Acid Will dissolve in the water. Let this cool, drain off the water and remove the "Wet Cast" TNT from the container, preferably plastic "I Can't Believe Its Not Butter" container, which bends easily allowing the TNT to loosen and fallout without cracking it. Place it on layers of paper towel to dry, as TNT will exude a yellow oil. Puddles of such exudate can be found in munitions dumps across the country. You will notice the paper towels colored yellow.
Allow the TNT to lay undisturbed on the towels, and if neccesary fresh portions of towel should be used to dry it. Later Castings should be done dry using a bath of boiling water surrounding a dry container with the TNT in it. One should not worry too much about possible safety dangers, as TNT is fairly difficult to initiate accidentally. Although it is better to be cautious around explosives paraphernalia.
My MNT, is a yellow waxy solid at about 30 celsius, however when i looked up the msds it said that melted at -16 celsius or something like that. Maybe there are DNT impurities in it? As well some of it is long clearish yellow needle shaped crystals, Im really thinking that it is just contaminated with dnt or tnt which is no problem because i will have a dream about turning it into tnt.
BTW. Used 70% conc. nitric, and 99% sulphuric.