"Method to synthetise AP
200 ml of 30% hydrogen peroxyde
150 ml acetone
50 ml of 30% hydrochloric acid
Procedure:
Mix your acetone with the acid, a nd cool the mix to 0-5 °C. The lowest the temperature is, the
best it is as the addition of h.p will release heat. Once that is done, slowly add the hydrogen
peroxyde, 20 mL at a time. The temperature should not be allowed to rise. You can for
example put some ice cubes in your mix, it dilutes it a bit, but it’s easy. Some ice cubes for
whisky come into glass tubes, for the whisky not to be diluted when the ice melts. That’s even
better. As there’s a lot of h.p to add, it’s easier to control the reaction than when you add the
acid to the acetone/h.p mix (but you can do it if you want). When addition is done, let your
mix sit for a few hours. There’s no real limit. I used to let it sit overnight, but it’s not
necessary, unless you use diluted chemicals: then you need to let the reaction happen for a
longer time.
White crystals should rapidly form and stay in suspension into the mix. At the end you should
get a full beaker of crystal soaked in a water/acid mix.
Filter out the crystals that should be TCAP. Coffee filters are ok, using a t-shirt is good too if
you have higher quantities of AP, since it will absord more. Wash the AP in a large beaker of
distilled water.You need to neutralize the
acid that is left in AP, for that put it a beaker with a
bit of sodium bicarbonate. You need to stir well, for the
acid blocked in the molecules that
have stuck together whil precipitating to be removed. Wash your AP again, and allow it to
dry. You should have pure AP.
You have made here normally 125g of pure AP. Theoretically...
With the filtering, dissolutions in water, non complete reactions, you surely have way less. This
depends on the number of time you washed it, the quantity of water you used, the method of
filtering. With experience one increases the yield.
Care with your freshly made AP !
Precursors: there’s not many things to say about them.
ÃÂ* Acetone is a common solvent you can buy in any drugstore, homestore… If you can’t, you
may find it in some nail polish remover, but be careful as it’s expensive, and some nail polish
remover contain no acetone (subtitutes are used, better for your nails), and there are many
other stuffs that may parasite the reaction.
ÃÂ* Hydrogen peroxyde is oxygenated water that you can buy in pharmacy, as antiseptic or as hair
bleacher. It should then be 3-6 %, just add some more to have the good number of moles in
the reaction. It is normally sold to everyone in drugstores, as a bleacher, to the concentration
of 30-35 %, and it will be far cheaper. Just ask if you can order some. Taxider mists and hair
shops should have some, you can ask there too.
ÃÂ* Hydrochloric
acid can be found in any store, it is pH relevant for swimming pools. It’s very
common. You may want to use another
acid instead of this, see in the Research/FAQ section
for that.
Research and FAQ
(mostly a FAQ for the moment though)
ÃÂ* Concentration of the hydrogen peroxyde
Using more concentrated H2O2 should not change the yield, as long as you put the same number
of moles in the mix: if you use 6% instead of 30%, just put 5 times more hydrogen peroxyde.
Some members have noticed that usually, they get better yields with concentrated H2O2. The fact
is water doesn’t stop the reaction, but the more in your mix, the slowest the reaction.
When using low conc. H2O2, be sure to let the reaction settle for a while, long enough for it to
complete.
Acid used
The
acid acts as a catalyst and about any strong
acid can be used in AP synthesis. Hydrochloric
and sulfuric
acid are also commonly used but some differences can be noted, and must be taken
into account.
Sulfuric acid: adding it will cause immediately a local overheating and ebullition. You must
add it drop-by-drop. A good solution to avoid a temperature elevation is to dilute your acid
and let it cool (e.g. from 95+ % to 30%).
Hydrochloric acid: easy to get, it may be the best suited
acid in this synthesis, regarding to its
low cost. It is safer too, as pouring the whole
acid at once in the mix will not cause (even
local) ebullition or overheating; however, the global temp of the mix will rise thus favoring
the formationof the dimer, or even producing tear gas. Don’t forget that it’s easier to keep the
reaction cool than cooling it down once the temperature has raised.
Toxicity
Pure AP is not toxic, doesn’t go trough the skin. I tried to eat some (very little quantity) and I
didn’t get any trouble. I tastes a bit like dust. The problem may only come from [unwanted
explosions

] the
acid kept in, if not well neutralized.
ÃÂ* Color
Normally AP is pure white. However colors may appear with impurities, for example rust if
you used an iron spoon to stir the mix. Impurities may also be due to impure reactants like
acetone from nail polisher.
Storing - Volatility
AP tends to sublimate very easily at normal temperature. It is therefore difficult to store. As a
personnal experience, I let 200 g AP on a plate for several monthes (about 4-5), and I lost
about half of the product. AP will also recrystalize on supports, make bigger crystals that are
more sensitive.
Storing AP is therefore dangerous. In an open container, you will lose some, and you can
imagine there are risks, due to impurities coming in, for example.
People tend to store it in air-sealed containers. Pure AP in an air-sealed container tends to
sublimate and recrystalize on the cap, so when you open it, the risk is that broken AP crystals
detonate and the whole pot too. This happened to a member.
An explanation is that with recrystalization the molecules of AP forms ionic bonds with each
other, and breaking these bonds release energy, sometimes enough to make the crystal
deflagrate.
Storing AP in a liquid limits the risks, even if still present. You can store it either in acetone
or water. You just need to make it dry then to recover your product:
With acetone, you can dissolve all your AP, then storage isn’t dangerous, just fire hazard.
With water, you AP will not dissolve (quasi not), and AP doesn’t sink, so you can put AP and
water in an air sealed container, then turn it upside-down. Therefore there won’t be any risk of
detonation when opening the cap: water prevented cristallization.
Try to let a minimum of air in your storage container, it also reduces the risks.
Storing AP is definitely risky. If you think it’s worth the risks, do it. But be aware that things
can go right 1000 times then 1001st they go wrong, and once is enough for you to go back to
the land of shadows… As one said, it’s not like the country is going to be taken over by aliens
and you need your AP right that instant to save the world.
Pressing AP
Pressing AP can be useful to make blasting caps, way more powerful than if not pressed. I
won’t speak about the precautions you need to take. Some press it with pencil. Note that
depending on your AP, you can press it only slightly, or dead press it. Make a few
experiments with some AP of the same batch before any attempt to press it. The more it’s
pressed the less air is in the cap, so the shockwave spreads easily, detonation is more
powerful. When pressed, AP is even more powerful than HTMD.
ÃÂ* Solubility
I tested TCAP solubility in water and acetone.
Results are not very precise, this is an idea.
I got:
· 0.4 gr TCAP in 700-800gr H20 @ 25°C, I stopped the experiment after having had
400mL of water, but compared to the quantity left non dissolved I think this is a good
approximation. Approximately it means about 0.55 gr TCAP in 1L H2O @ 25°C
· 15 gr TCAP in 60mL acetone @ 25°C. This is an approximation, a bit more could have
been dissolved but it took way more time to dissolve, so that should be globally a reliable
value. This means a bit more than 250gr TCPA in 1L acetone @ 25°C.
We see that AP dissolves very well in acetone, not much in water, so the addition of acetone in
your mix should be limited, even if you waste H2O2, rather than adding more aceto ne that will
globally result in a loss of AP. I think 2-3 mL more than the stoechiometric ratios should be
enough (still it will cause a more than 0.5-1 g loss). You can let the acetone evaporate before
filtering to avoid losses.
Note that these solubilities were tested at about 25°C, which is the temperature of water in
summer, for me, but of course it will be less at lower temperatures. For example, in your mix
during the reaction (which is somewhere between 5 and 10°C)."