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PETN Synthesis!

2Bis[(Nitrooxy)-methyl]-1,3propanediol dinitrate (ester), Pentaerytritol Tetranitrate, 2,2-


bisdihydroxymethyl-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: Materials:
98% Concentrated Sulphuric Acid (H2So4(l)) Two clean glass beakers
70% Concentrated Nitric Acid (HNO3(aq)) Pipette
Acetone Stirring Rod
Pentaerythritol Watchglass
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.

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.
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2. A second ice bath is prepared to be used for emergency cooling of the mixture should its
temperature become too high.

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

After 10 minutes of mixing, the mixture is a white thick syrup: 10 minutes of mixing, the mixture is

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4. Mixing is continued for 10 minutes after the last of the pentaerythritol is added. The mixture
is then put in a hot water bath and heated to 45½C for 25 minutes. This will considerably
increase yield by nitrating most sulfoesters into PETN. It is important to keep the temperature
at or below 45C, maintain stirring and watch for any signs of runaway nitration. (This step is
not needed, but will result in a much better yield).

5. 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. Care must be taken to slowly and
evenly add the mixture to water, as the excess H2SO4 in the mixture will cause a temperature
rise that can lead to decomposition of the final product.

The PETN is filtered and washed with cool water and then neutralized with hot sodium
bicarbonate solution.

7. 200ml of acetone are heated to 50�C. And the PETN is stirred into it until all of it has
dissolved (solubility: 58gr/100ml acetone at 50C). Excess acetone is needed, due to excess
water in the PETN. Drying the PETN prior to this step will minimize the amount of acetone
needed.

8. The PETN / acetone mix is then filtered and poured into a beaker containing 600mL of ice
cold water, causing the PETN to precipitate to the bottom as fine crystals.

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9. After settling, excess water and acetone are decanted and the remaining PETN can be
filtered out
After filtering, the PETN was put on a small Petri plate and dried.

Results:
The dry product weighted ~22 grams, which is a ~91% yield. Most losses seem to occur
during filtering and during the acetone purification phase. Below a picture of the finished
product can be seen:

Some Merck Data:


More sensitive to shock than TNT, practically insoluble in water, soluble in Acetone + Alcohol,
melting point 140C. (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.
With added H2SO4, there must still be some water in the mix, or oxidation will occur. At the
start of this procedure, the water content is 20%, at the end it rises to 30%. Increasing the
amount of pentaerythritol will increase the water content at the end of the reaction, thus
probably lowering the yields because of the oxidation of the end product.

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