One set of pretty straightforward instructions for making acetone peroxide, the compound currently believed to be at the heart of the UK terror hysteria currently underway (and the previous terror hysteria, as well).
Acetone Peroxides are very unstable chemicals. If handled at all, they should be treated with great care and only synthesized in minute quantities. This refers to triacetone triperoxide (TATP), sometimes refered to as tricycloacetone peroxide (TCAP). The reaction must be done under 50 °F (10 °C) to yield triacetone triperoxide.
TATP is widely considered to be too unstable to synthesize safely in standard laboratory facilities, though small quantities (under 1 gram) are occasionally synthesized for research purposes, and for testing and calibration of detection equipment.
* 3% H2O2 – Available almost anywhere as a 3% antiseptic solution in water called “Hydrogen Peroxide” or “Peroxide”.
35% Hydrogen Peroxide solutions can be found in most hardware stores in wood bleaching kits.
This will produce much greater yields and is safer than boiling the 3% solution.
* 2-Propanone – Available as paint-thinner, from hardware stores. Often in cans labeled simply as “Acetone.”
Both Home Depot and Wal-Mart carry pure Acetone in the paint section.
* H2SO4 – Sulfuric acid available in motorcycle battery KITS. These can be found at wal mart And almost any auto parts store.
* Glass thermometer
* Glass eyedropper
* Glass beaker
* Safety equipment, minimally including heavy leather gloves, impact-resistant goggles, hearing protection, and face shield.
As with other reactions that pose the risk of explosion, synthesis should not be performed in an enclosed area.
Before beginning the synthesis procedure, you should put the H2O2 and 2-Propanone in a refrigerator for several hours. This will speed up the procedure.
Once the several hours have passed, prepare an ice bath for the glass beaker. Pouring a small amount of water around the beaker with plenty of ice seems to work well, as the cold water will surround the beaker better than the ice alone.
If the quantity of 2-propanone in your posession is sufficient, it may be desirable to utilize it in a more effective form of cold bath for the reaction. Instead of an ice bath, one may substitute a container filled with 2-propanone, cooled by small amounts of CO2 in solid form (dry ice). This mixture can be cooled to temperatures very well below the normal freezing point of water, thus making it possible to more easily restrict the temperature of the reaction.The cooling is acheived by placing the CO2 in small amounts at a time into the solution and allowing them to sublime, thus cooling the 2-Propanone. However, be extremely careful with this cold bath! 2-Propanone is very flammable and will irritate skin and eyes. Also, since the bath is cooled to well below water’s freezing point, touching the liquid could cause instant freeze burns and/or frostbite. Never touch this solution with unprotected skin!
For a safer synthesis, you may choose to skip the step of concentrating the H2O2 and use the 500mL 3% H2O2 as is in the actual reaction. It is highly recommended that amateurs not attempt to concentrate 500mL 3% H2O2 below 150mL, as concentrated H2O2 can cause fire.
Put 500mL H2O2 in a glass beaker, and slowly boil it down to about 100-250mL. Warning: Boiling H2O2 can cause explosion. Keep the temperature below 302 °F (150 °C) to prevent the boiling of H2O2. Do not raise the temperature past 212 °F (100 °C). The goal is to lightly boil away the water in the H2O2, leaving a purer form of H2O2. Once you have concentrated the H2O2, take it off of the heat and allow it to cool.
Warning: H2O2 that is too concentrated is unstable. Do not allow the heated mixture to boil away below 80mL, or one is risking an instant fire from the concentrated H2O2.
Warning: Concentrated H2O2 may not be poured onto the ground. Concentrated H2O2 will cause fire when poured out, and allowed to sit for extended periods of time. If one has concentrated H2O2 on hand, and does not want to proceed with the dicycloacetone peroxide synthesis, then one may dump the concentrated H2O2 into a liter of water.
Put the H2O2 into the beaker in the ice bath, and add 60mL chilled 2-Propanone. Measure the temperature of the liquids with a thermometer and wait for it to drop to around 40 °F (4.4 °C). Using a glass eyedropper, slowly add 15mL H2SO4. Monitor the temperature closely while adding the H2SO4, if the temperature gets around 50 °F (10 °C), quit adding the H2SO4. Failure to quit adding the H2SO4 when the temperature rises may risk explosion. There will be a slight temperature rise during the addition of H2SO4; this is why the adding of the H2SO4 must be done slowly. If the H2SO4 is added too quickly, it will not have time to create the proper peroxysulfuric acid; this may cause explosion.
When all of the H2SO4 has been added, stir the mixture for about 15 minutes. After 15 minutes, place the reaction mixture into a refrigerator for about 24 hours. A white crystalline solid will result. This crystalline mass can then be filtered out with filter paper. When the crystalline mass has been filtered, pour 400mL of water over it to wash the acid residue away. Set the crystalline mass out to dry. The crystalline mass is tricycloacetone peroxide. If you did the reaction above 50 °F (10 °C), you will have the much unpleasant dicycloacetone peroxide.
Warning: This final crystalline mass is very sensitive when dry, it’s friction sensitivity can be as low as .1NM. Proper care must be taken with the final crystalline mass, as it is highly unstable.
For safety, separate the crystalline mass onto paper plates at 1 gram per plate; this will greatly reduce the risk of explosion. If a problem were to occur, the one gram on one of the plates would be less likely to hurt you.
Storing acetone peroxide is not recommended, because it quickly sublimes. But if it must be stored, it is recommended that it is stored under water and in a container without a cap with threads, as opening it could result in an explosion from crystalized acetone peroxide.
TATP and DADP neither detonate nor deflagrate; they are rare entropy explosions. The effect is from rapid dissociation of weak atomic bonds within the acetone peroxide molecules, not from a chemical reaction as seen in all common explosives. Acetone peroxides require neither heat to form nor do they release heat when they dissociate; the effect is similar to the solid-to-gas reaction that deploys automobile air bags.
Each solid molecule of TATP dissociates directly into 4 gas-phase molecules. It is held together by three weak O-O bonds in a ring formation with three H2C and three CH2 molecules. Dissociation may be initiated by heat, pressure, or impact. The first dissociation creates enough pressure to cause surrounding TATP molecules to dissociate. The heat created by friction may initiate a reaction between atmospheric oxygen, the resultant ozone molecule, and the three hydrocarbon molecules.
Like TATP, each solid molecule of DADP also dissociates directly into gas-phase molecules. DADP’s dissociation results in one O2 molecule and two of the same hydrocarbon molecules as TATP. Since O2 is more stable than O3, DADP will dissociate more readily than TATP.
The pressure produced in just the dissociation of TATP molecules is about 80% greater than pressures seen in the detonation of the same mass of TNT.
Like all knowledge, this is power; use responsibly, i.e. not at all.