HMTD is by far my favorite organic peroxide. It requires less attention during the synthesis than both acetone and MEK peroxide and is better in most cases than either of those two. It is easy to compress into detonators is more storage stable than the other two peroxides (but still, don't store it)
Warning! HMTD is very dangerous. It is unstable and powerful even when not confined. Never under any circumstances should it come in contact with metals of any sort. Never make this or any other explosives, just like I never have ;)
Here is the reaction that goes on in the vessel
(CH2)6N4 + 3H2O2 --catalyst--> (CH2)6N2(O2)3 + 2NH3
The catalyst takes the ammonia that is formed and converts it into an ammonium compound so that no ammonia gas is liberated. There are 2 main catalysts that can be used for this reaction. They are citric acid and hydrochloric acid. The type of catalyst used affects exactly what type of ammonium compound will be formed. There is also a less popular but just as effective (if not better) than citric acid and that is sulfuric acid.
Citric acid: 2NH3 + C6H8O7 ----> (NH4)2C6H6O7
Hydrochloric acid: NH3 + HCl ----> NH4Cl
Sulfuric acid: 2NH3 + H2SO4 ---> (NH4)2SO4
|Hexamine (Prep/OTC)||100ml Graduated cylinder|
|30% Hydrogen peroxide (27% can be used)||250ml Erlenmeyer flask|
50mls of 30% Hydrogen peroxide is measured out (56mls if you use 27%) in the graduated cylinder and is poured into the Erlenmeyer flask. 14 grams of hexamine is weighed out on the scale and then poured into the flask from above. The flask is swirled until all the hexamine is dissolved and you are left with a clear solution. Place this flask into a freezer and leave it there for 2-3 hours (or until the mixture has dropped below 5C). Once the contents have been chilled, weigh out 21 grams of citric acid. Add all your citric acid to the flask at once (the temperature isn't going to spike like it does with other catalysts when you add them too fast). Swirl this flask until all the citric acid has completely dissolved. You will now be left with a thick(ish), clear(ish) solution. Keep swirling for 10 more minutes and then place this flask in the freezer. Leave it in the freezer for 6 hours swirling occasionally. After 6 hours, move it to the refrigerator for another 6 hours swirling occasionally. After this 6 hours is up, take it out of the fridge and let it warm up to room temp for yet another 6 hours. When you take it out of the fridge there should be a lot of white crystals floating around. After the last 6 hour period is up, we need to filter and purify.
Filter out all the white crystals from the flask and throw some distilled water into the flask. Swirl it around to get any remaining crystals and filter those out in the same filter. It is recommended that you set this filter up for vacuum filtration right now, but is not necessary. If you do choose to use vacuum filtration, don't turn the vacuum on full power yet. Wash out the 250ml flask and then fill it to the 200ml line with distilled water. Pour all of this through the HMTD sitting in the filter (not all at once though). After all that has been run through, throw a couple pinches of sodium bicarbonate into the flask and fill once again to the 200ml line with distilled water. Pour all this through the HMTD in filter. After this, wash the flask out and then fill to the 200ml line with distilled water. Pour all of this through the HMTD (now you can see why vacuum filtration is recommended). You should now have very pure HMTD sitting in the filter. If you are using vacuum filtration, turn the vacuum on full power to suck most of the water out and leave it at this power for 4-5 minutes. Take the filter paper containing the HMTD out of the funnel and run litmus paper over any water still in the funnel. Run both types because too much base is just as bad as too much acid. If it is clean, lay the filter paper containing the HMTD on a paper towel (don't unfold the filter paper yet though). After a couple hours of drying, you can unfold the paper and spread the HMTD around a little bit to help speed up drying. It shouldn't take more than a day to dry completely. Never during this synthesis should you let the HMTD come in contact with metals.
Theoretical yeild = 20.8 grams HMTD
Here are the materials. From left tor right, back to front - Citric acid, Hexamine, 27% hydrogen peroxide, 250ml erlenmeyer flask, 100ml graduated cylinder, gram scale.
Measure out the 14grams of hexamine and 50mls (or 56mls if you use 27%) of your hydrogen peroxide.
Add your hydrogen peroxide to the flask
Dump the hexamine into the flask with the hydrogen peroxide
Swirl this flask until all the hexamine has dissolved into the hydrogen peroxide
Place this flask in the freezer for a couple hours to bring the contents of it down below 5C. After this happens, weigh out 21 grams of citric acid and pull the flask out of the freezer.
Add all the citric acid to the flask at once.
Swirl this until all the citric acid dissolves. You will be left with a clear(ish) solution in the flask.
Place this flask in the freezer for 6 hours and swirl it once in a while. After the 6 hours is up, move it to the refridgerator for another 6 hours, swirling it occasionally. Once this 6 hours is up, pull it out of the fridge and set it on a table to let it warm up to room temp. When you pull it out of the fridge, there should be a significant ammount of white crystals floating around in it.
After it is done reacting, it should look something like this (Of course, after swirling)
Now we must begin neutralization of the product. Here are the minimum materials you will need
From left to right, back to front: Sodium bicarbonate, HMTD mixture, glass funnel, red litmus (base), blue litmus (acid)
First we must dilute the HMTD mixture with distilled water by filling the flask up above the 200ml mark. The HMTD will not dissolve, but the citric acid and other crap will. This will also make filtration easier
Set up the glass funnel with some filter paper (I used coffee filters) in a big beaker for the concentrated waste water
Begin to pour in the HMTD mixture into the funnel.
Eventually you will get all of the mixture through there. It helps sometimes to lift up a side of the filter paper a little bit to let air through. Now we have an empty flask and the majority of the product.
Add some distilled water to the 250ml flask where the HMTD mix was to get the remaining crystals.
Pour this through the filter then set the funnel up in a vacuum filtration unit as shown below.
Clean the 250ml flask out and then fill to the 200ml line with distilled water. Turn the vacuum on (but not to full power, if you turn it to full power you'll start sucking the filter paper into the funnel and eventually rip the bottom open)
Pour the water over the HMTD in small portions until all 200mls have been poured through.
Throw in a couple pinches (about a spoonful) of sodium bicarbonate into the 250ml flask and fill to the 200ml line with distilled water. Swirl until all sodium bicarbonate is dissolved. Pour this through the filter the same as before. After this, wash the 250ml flask out and fill to the 200ml line with distilled water one more time. If your filtering unit is getting full, dump it then set it back up again. Run the 200mls of water through the HMTD and then turn the vacuum on high power to suck out any remaining water. Leave it at this high power for at least 4-5 minutes. Find something to stick the litmus paper into to test for acid and base (because too much base is just as bad as too much acid). DO NOT STICK THE LITMUS IN THE HMTD. The litmus paper step can generally be omited because the 600mls of water should have removed any acids. If it didn't... then I wouldn't want to go near whatever you used as a catalyst. After sucking out all the moisture, it should look like this:
Here is my litmus:
Take the filter paper out of the funnel and lay it on some paper towels. Don't open it up yet though. You can do that later
After a short while, you can open the filter paper up and spread it across some paper towels. Usually when you do this, the HMTD stays in one solid cone so you must break it up with a matchbook cover (the cardboard part, not the matches). It should look crumbly at this time
After it's dried for about 12-24 hours, you can crush it into a fine powder. Then weigh it (optional) to see what kind of yeild you go. Remember to subtract the weight of the filter paper from it or zero the scale in with an identical piece of filter paper.
As you can see, I got 14.5grams of HMTD. The theoretical yeild was 20.8 grams calculated from the ammount of hexamine needed. This gives a 69.7% yeild which is terrible in the chemistry world. I will retry this synthesis a couple more times and run different tests on the HMTD to see if I can improve the yeild.