decomposes at 25 °C
Trinitromethane, also called nitroform or TNMe, is typically used as an intermediate in the manufacture of other explosive compounds. It was first prepared by the action of concentrated nitric acid on acetylene back in 1900 or so. The Germans experimented with this process on a large scale in WWII for TNMe as intermediates for other explosives. The Hercules Powder Co. has a trademark they call Nitroform®, it is an agricultural product designed to release nitrogen into soil, it is not trinitromethane. Since TNMe is very acidic, it tends to form various neutral explosive salts. Most of the salts are used as propellants or are too unstable to use. TNMe has 137% of power vs. TNT. Keep this compound stored in a sealed glass container at 0 °C.
|ethyl ether||1000-mL Florence flask|
|hydrogen chloride gas||glass filter paper|
|hydrogen peroxide||graduated cylinder|
|methyl alcohol||stirrer/stirring rod|
Prepare a solution of 168 g of potassium hydroxide in 350 mL of water in a round-bottomed 1000-mL Florence flask, and cool to 5 °C with a salt-ice bath. While stirring, add 108 mL of 30% hydrogen peroxide to the solution. Next, add 117 mL of tetranitromethane at a rate which keeps the temperature at 20-25 °C, add while stirring. The temperature is then allowed to rise to 30 °C over 15 minutes. The bright yellow solid, that should have formed, is filtered to collect it using glass filter paper because of its high acidity, washed with anhydrous methyl alcohol, then anhydrous ethyl ether, and finally air dried to give 100% of the potassium salt of trinitromethane. The salt is suspended in anhydrous ethyl ether and anhydrous hydrogen chloride gas is passed in until the yellow color disappears. The white precipitate of potassium chloride is filtered off and washed with anhydrous ethyl ether. The ethyl ether is evaporated from the filtrate and additional washings at reduced pressure give 85-90% of crude trinitromethane which can be purified by sublimation. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature.
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