PETN Synthesis!

2Bis[(Nitrooxy)-methyl]-1,3propanediol dinitrate (ester), Pentaerytritol Tetranitrate, 2,2bisdihydroxymethyl-1,3-propanediol tetranitrate, nitropentaerytritol, penthrit, niperyt, Lentrat, Hasethrol, Perityl, Terpate, Subicard, Pentryate, Pentitrate, C5H8N4O12 or simply PETN(1), this compound finds both medicinal use as a coronary Vasodilator (often mixed with lactose to reduce sensitivity) and extensive use in the explosive industry, as a very high power booster in blasting caps and also as the filler in detonating fuse (DetCord, Primacord)*. Reagents and Materials: Reactants: 98% Concentrated Sulphuric Acid (H2So4(l)) 70% Concentrated Nitric Acid (HNO3(aq)) Acetone Pentaerythritol Distilled Water (l) Sodium Bicarbonate (NaHCO3(s)) Synthesis: The ratios used for this synthesis are as follows: 34 ml of 65% HNO3 24,8 ml of 96% H2SO4 10,0 g of Pentaerythritol All the chemicals used in this synthesis can be seen below: From left to right: 65% Analytical Grade Nitric Acid, 98% Analytical Grade Sulphuric Acid, 99,5% Analytical Grade Acetone and 99.8% Extra Pure Pentaerythritol. The petri dish contains 10 grams of pentaerythritol. Materials: Two clean glass beakers Pipette Stirring Rod Watchglass

1. A cold-water bath was prepared and used to chill A 200ml wide necked flask containing nitric acid. 24,8 ml of sulfuric acid were pipetted into the flask and the mixture was allowed to further cool by adding ice and salt to the cold water bath. 1

2. A low starting temperature is key in this synthesis and should the temperature rise above 0C at any time. Should runaway nitration occur (evidenced by the evolution of brown N2O4 / NO2 gas) the mixture should be immediately poured into cool water. the mixture is a white thick syrup: 10 minutes of mixing. the mixture is 2 . A second ice bath is prepared to be used for emergency cooling of the mixture should its temperature become too high. 3. At 5�C it became a thick slurry. After 10 minutes of mixing. With the mixed acids at or below 25½C. The mixture can be seen to thicken as nitration occurs and the temperature rises. 2 grams at a time. re-chilling will be necessary prior to further addition of the pentaerythritol. It is important to constantly stir the acid mixture during the addition as localized heating will occur during nitration. 10 g of pentaerythritol are added.

(This step is not needed. 200ml of acetone are heated to 50�C. It is important to keep the temperature at or below 45C. Care must be taken to slowly and evenly add the mixture to water. The PETN / acetone mix is then filtered and poured into a beaker containing 600mL of ice cold water. And the PETN is stirred into it until all of it has dissolved (solubility: 58gr/100ml acetone at 50C). The mixture is then diluted with 450 ml of ice cold water and excess water is decanted after the crystals settle so as to ease the filtering of the product. Mixing is continued for 10 minutes after the last of the pentaerythritol is added. Drying the PETN prior to this step will minimize the amount of acetone needed. maintain stirring and watch for any signs of runaway nitration. The PETN is filtered and washed with cool water and then neutralized with hot sodium bicarbonate solution. causing the PETN to precipitate to the bottom as fine crystals. The mixture is then put in a hot water bath and heated to 45½C for 25 minutes. as the excess H2SO4 in the mixture will cause a temperature rise that can lead to decomposition of the final product. 3 . 7. This will considerably increase yield by nitrating most sulfoesters into PETN. but will result in a much better yield). 5. due to excess water in the PETN.4. Excess acetone is needed. 8.

thus probably lowering the yields because of the oxidation of the end product. Below a picture of the finished product can be seen: Some Merck Data: More sensitive to shock than TNT. or oxidation will occur. After settling. 4 . (1) The maximal amount of water in the mix cannot exceed 30% due to nitric acid's properties as a strong oxidizing agent between the 50-70% concentration range. Most losses seem to occur during filtering and during the acetone purification phase. the PETN was put on a small Petri plate and dried. the water content is 20%. soluble in Acetone + Alcohol. melting point 140C. which is a ~91% yield. Increasing the amount of pentaerythritol will increase the water content at the end of the reaction. at the end it rises to 30%. With added H2SO4. practically insoluble in water. excess water and acetone are decanted and the remaining PETN can be filtered out After filtering. At the start of this procedure.9. Results: The dry product weighted ~22 grams. there must still be some water in the mix.

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