Methyl Ethyl Ketone Peroxide
I went to the hardware store and, next to the impulse buys, there was some acetone, tolulene, and some methyl ethyl keytone. I already had purchased alot of acetone, so I bought some tolulene and methyl ethyl keytone. I plan on making Tri-Nitro-Tolulene (TNT), and Methyl ethyl keytone peroxide. I already had some sulfuric acid and 35% h202!
I already have a few TNT syths, so I decided to include a recipe for MEKP.
Alot of people are always wondering about this as an explosive. Here is a synthesis I found.
PREPARATION AND PROPERTIES OF METHYL ETHYL KETONE PEROXIDE
The three most common forms of methyl ethyl ketone peroxide are:
MONOMERIC: C4H10(O)4
DIMERIC: C8H18(O)6
ANHYDROUS DIMERIC: C8H16(O)4
The anhydrous dimeric form is the preferable form to create; it is more powerful and less sensitive to shock. Bot hforms are very sensitive to heat. Anhydrous dimeric methyl ethyl ketone peroxide takes many times as sharp of a blow from a hammer to initiate detonation than with trimeric acetone peroxide. This is due to several factors:
(1) It is an oily liquid, not a solid, A solid will not shift shape to fit its container, as will a liquid. Thus, when trimeric acetone peroxide is struck with a hammer, the crystals shatter, causing decomposition; when anhydrous dimeric methyl ethyl ketone peroxide is struck with a hammer, it will shift shape significantly, often avoiding decomposition.
(2) The C-O-O-C group is better shielded in anhydrous dimeric methyl ethyl ketone peroxide than in trimeric acetone peroxide. Thus, random energy surges will be less likely to affect the C-O-O-C group enough to break all of the bonds in the group, which would result in exothermic decomposition, likely starting a chain reaction; this would be perceived as detonation.
(3) There is less stress on the peroxide groups in anhydrous dimeric methyl ethyl ketone peroxide than in trimeric acetone peroxide (bond stress is mostly responsible for monomeric acetone peroxide's incredible instability, and anhydrous dimeric acetone peroxide's relative instability when compared to trimeric acetone peroxide).
(4) The decomposition to an exothermic stage of decomposition of a single molecule of anhydrous dimeric methyl ethyl ketone peroxide requires more energy than with a single molecule of trimeric acetone peroxide. (5) Less energy is liberated from the decomposition of a single anhydrous methyl ethyl ketone peroxide molecule, causing it to be less likely that detonation will occur from the decomposition of just a handful of anhydrous methyl ethyl ketone peroxide molecules. Perhaps the most valuable property of methyl ethyl ketone peroxide is the fact that it can be stored for a long period of time. Chemical decomposition does not proceed beyond the monomeric form, with the obvious exception of deflagration and detonation. Autonomous chemical decomposition is very slow when not in the presence of hydrogen peroxide (which causes the anhydrous dimeric form to begin to decompose slowly into the monomeric form). Because of this, it is wise to prepare anhydrous dimeric methyl ethyl ketone peroxide in an excess of methyl ethyl ketone (this fact has been factored into the below instruction on preparation of methyl ethyl ketone peroxide). Anhydrous dimeric methyl ethyl ketone peroxide is a thick, oily liquid. The anhydrous dimeric form, when pure, possesses a sharp, sour, acidic "burning" odor. The procedure for preparation that will soon be discussed will produce mostly the anhydrous dimeric form.
PREPARATION OF ANHYDROUS DIMERIC METHYL ETHYL KETONE PEROXIDE
CHEMICALS NEEDED: -40mL 27.5% H2O2 solution (other concentrations may be used; the volume of hydrogen peroxide solution will need to be adjusted accordingly; the quantity of sulfuric acid used will also need to be adjusted) -25mL Methyl Ethyl Ketone CH3COCH2CH3 (sold as a solvent at hardware stores; keep in mind that it will dissolve most plastics) -5mL 98% sulfuric acid (other concentrations may be used, the volume of sulfuric acid will need to be adjusted accordingly) -200mL NaHCO3 solution
1) Place 25mL of methyl ethyl ketone in a 100mL beaker. Place this beaker in an ice bath at temperatures ranging preferrably from -10 to 5 degrees Celcius; the lower end of the described recommended temperature range is preferrable.
2) Place 40mL of 27.5% H2O2 solution in a 100mL beaker. Place this beaker in an ice bath at temperatures ranging preferrably from -10 to 5 degrees Celcius; the lower end of the described recommended temperature range is preferrable.
3) Wait fro the temperature of both the methyl ethyl ketone and the temperature of the 27.5% H2O2 solution to fall into the recommended temperature range. Then, pour the beaker of methyl ethyl ketone into the beaker of hydrogen peroxide solution. Stir this solution for thirty seconds.
4) Add 5mL of 98% sulfuric acid slowly, drop by drop, taking care to keep temperatures within the recommended temperature range, into the beaker containing the monomeric methyl ethyl ketone peroxide. If the temperature rises above 5 degrees Celcius, stop adding the sulfuric acid immediately.
5) After all of the sulfuric acid is added, wait 24 hours. It is highly recommended to attempt to keep the temperatures within the recommended temperature range during the entirety of every step of the prepataion (this is a very common mistake made when attempting to make trimeric acetone peroxide; most will not bother to keep the temperatures around zero degrees Celcius while waiting 24 hours or so for the reaction to complete; the result of that is far less stable acetone peroxide due to lower yields of the trimeric form and higher yields of the dimeric form).
6) The beaker should now have two layers; a thick oily layer on the top, and a translucent white, relatively thin liquid on the bottom. The thick oily layer on top is the anhydrous dimeric methyl ethyl ketone peroxide. All traces of acid must now be removed. Pour this beaker into a 300mL beaker. Then slowly add 200mL of NaHCO3 solution. Stir vigorously for five minutes; try to keep the size of the pockets of the oily liquid (the anhydrous dimeric methyl ethyl ketone peroxide) as small as possible when stirring.
7) Most of the anhydrous dimeric methyl ethyl ketone peroxide will now begin to sink to the bottom of the beaker. Extract it with a syringe. Some will also remain on the surface; extract this also with a syringe (it is possible to isolate the anhydrous dimeric methyl ethyl ketone peroxide by decantation, but this process can be very time consuming, frusturating, and will not be able to harvest nearly as much of the anhydrous dimeric methyl ethyl ketone peroxide as the syringe extraction method). If you wish to further deacidify the anhydrous dimeric methyl ethyl ketone peroxide, place it in an airtight aluminum container, in an ice bath (extremely important!). Leave the methyl ethyl ketone peroxide in the airtight aluminum container until bubbles no longer form. A safer alternative to this process is to add noon-crumpled pieces of aluminum foil to the anhdrous dimeric methyl ethyl ketone peroxide (also in an ice bath); however this will often make it difficult to recollect all of the anhdrous dimeric methyl ethyl ketone peroxide, due to it sticking to the pieces of aluminum foil; it can be very difficult to remove from that surface.
9) Now pour the deacidified anhydrous dimeric methyl ethyl ketone peroxide into an open glass, or plastic (not made of a polyhydrocarbon plastic!). Let it stay in the open at temperatures around 15 degrees Celcius to allow most of the water to evaporate off.
10) Now that the anhydrous dimeric methyl ethyl ketone peroxide is dehydrated, it is ready for use.
STORAGE: Pour the anhydrous dimeric methyl ethyl ketone peroxide into a sealed plastic container (not made of a polyhydrocarbon plastic!) for storage. The reason for sealing it is to prevent loss of anhydrous dimeric methyl ethyl ketone peroxide due to evaporation. The lower the temperatures are during storage, the better, with the exception of temperatures so low that it freezes the anhydrous dimeric methyl ethyl ketone peroxide. Density of MEKP = 1.0g/cm3 Freezing point = approximately -5 to -10 degrees Celcius Dimeric 2-peroxybutane explodes upon contact with concentrated sulfuric acid. It seems that dimeric 2-peroxybutane (MEKP) is more stable than previously thought. It does not explode unless severely shocked. I have tried to explode as much as 4mL using only fuse, and that resulted in nothing but a tall pillar of flame. It does explode with a sharp crack when hit *hard* with a hammer. I suggest using aqueous ammonia instead of sodium hydrogen carbonate for neutralizing acid. A dimeric 2-peroxybutane / ammonium nitrate dynamite: 11mL (or grams) of dimeric 2-peroxybutane mixed with 100g of ammonium nitrate.