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Author: Subject: Methyl Ethyl Ketone Peroxide
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[*] posted on 20-5-2002 at 20:06
Methyl Ethyl Ketone Peroxide


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.




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[*] posted on 20-5-2002 at 20:06


I recently prepared some methyl ethyl ketone peroxide. This time it was a higher isomer, it is a mix of a white crystaline solid, and the dimeric liquid isomer. I assume that the white crystaline solid is trimeric 2-peroxybutane. The reason for the formation of the solid form: I carried out the reaction at very low temperatures, and deacidified the methyl ethyl ketone peroxide before it was broken down to a lower isomer by the sulfuric acid. The temperature of the reaction: negative thirty degrees Celcius. If you do not want the solid form, I recommend allowing the methyl ethyl ketone peroxide to sit in a warm area (not extracted yet, of course, still mixed with water) for several hours before deacidifying. That should break down any trimeric 2- peroxybutane down into the preferrable liquid dimeric 2-peroxybutane form.



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[*] posted on 20-5-2002 at 20:06


Does the same ratios for dynamite work with AP instead of MEKP. Is this just an oxygen balance ? AP has a oxygen balance of -150% and AN 20%. Would the ratios be 10g AP & 75g AN.
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[*] posted on 20-5-2002 at 20:07


ive actualy made this before. and just curious, where did u get this info? your post is remarkably similar to a post made by a guy on the e&w forum before it went down. that was a good thread.

[Edited on 5/30/03 by Madog]
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[*] posted on 20-5-2002 at 20:07


That post was written in a text file on my computer... I simply copied and pasted it back in here.



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[*] posted on 20-5-2002 at 20:08


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.

A dimeric 2-peroxybutane / sodium nitrate dynamite:
44mL of dimeric 2-peroxybutane mixed with 51g sodium nitrate.

[Edited on 21-5-2002 by madscientist]




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[*] posted on 20-5-2002 at 20:09


Is it possible to make methyl ethyl ketone by adding ether to acetone.
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[*] posted on 20-5-2002 at 20:10


It depends what kind of ether you are using... there is isopropol ether,ethyl ether, propyl ether, methyl ether, butyl ether... and the list goes on seemingly forever. It might be possible to prepare methyl ethyl ketone from acetone and methyl ether; but this would probably be a reaction of the "high temperature, high pressure, exotic catalyst" type.



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[*] posted on 20-5-2002 at 20:10


Is there any other name for methyl ethyl ketone (like Acetone for dimethyl ketone) ?
Thanks
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[*] posted on 20-5-2002 at 20:11


Another name for methyl ethyl ketone could be isobutanone.I recently prepared some methyl ethyl ketone peroxide. This time it was a
higher isomer, it is a mix of a white crystaline solid, and the dimeric liquid isomer. I assume that the white crystaline solid is trimeric 2-peroxybutane. The reason for the formation of the solid form: I carried
out the reaction at very low temperatures, and deacidified the methyl ethyl ketone peroxide before it was broken down to a lower isomer by
the sulfuric acid. The temperature of the reaction: negative thirty degrees Celcius. If you do not want the solid form, I recommend allowing the methyl ethyl ketone peroxide to sit in a warm area (not extracted yet, of course, still mixed with water) for several hours before deacidifying. That should break down any trimeric 2-peroxybutane down into the preferrable liquid dimeric 2-peroxybutane form.




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[*] posted on 20-5-2002 at 20:12


*Dimethyl keton or aceton is called also propanone; methylethyl keton can only be named butanone or 2-butanone; never isobutanone!
Iso in a molecule means that one CH in a terminal chain position holds 2 CH3:
ex isobutane is CH3-CH(CH3)2
isopropanol is HO-CH(CH3)2
isopentane is CH3-CH2-CH(CH3)2
neopentane is CH3-C(CH3)3
(neo means that one C in a terminal chain position holds 3 CH3!).
By definition a ceton is R-CO-R' with R/R' different from H, so even if you think realy hard its is not possible to make a branched ceton with 4 C linked together since the CO has to be in second or third position to be a ceton (otherwise it is an aldehyde)!!!!

It is impossible to make a reaction between:
aceton and ether that will provide MEK!
CH3-CO-CH3 + CH3-CH2-O-CH2-CH3 -/-> MEK
Since CH3-CO-CH3 will dehydrate/crotonise on itself and ether will lead to CH2=CH2 and water!Even with catalyst it would be difficult since ether is quite resistant to chemical attack and ceton tends to polymerise (condensate).

Mixing CTAP with NH4NO3 will never reduce its sensitivity or power (it will only reduce a little its making cost)! Treat it as if it was plain pure CTAP --> little quantities!

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[*] posted on 24-5-2002 at 07:37


I think it does reduce some power ...

And if percentage of CTAP is lower then 10%, I think it even loses flame sensitivity (small particles of CTAP burn, but it no longer effectively transports flame to support deflagration to detonation transition)

Offcourse, I would never suggest of using large quantities of it, because I hardly thrust it myself ...

Also take into account the acidity of NH4NO3, and the way some peroxides react with acids.
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[*] posted on 28-5-2002 at 12:06


After some thought, I now believe that the solid form of methyl ethyl ketone peroxide is actually (CH3CO(O)CH2CH3)2. The liquid form is (CH3C(OOH)(O)CH2CH3)2. I will now explain what brought me to these conclusions.

The liquid form is not CH3C(OOH)2CH2CH3, because that is formed simply by the reaction of CH3COCH2CH3 and H2O2. No methyl ethyl ketone peroxide came out of solution upon mixing of H2O2 and CH3COCH2CH3; from this I can conclude that the liquid methyl ethyl ketone peroxide is not CH3C(OOH)2CH2CH3, and that CH3C(OOH)2CH2CH3 is water soluble.

I believe that the liquid form is actually (CH3C(OOH)(O)CH2CH3)2. That would explain the *very* slight solubility in water, and would explain its tendacy to burn, rather than detonate, when exposed to flame. (CH3C(OOH)(O)CH2CH3)2 should decompose this way when exposed to flame:

2(CH3C(OOH)(O)CH2CH3)2 --> 4CH3COCH2CH3 + 2H2O + 3(O2) + energy

That reaction would be exothermic enough to create all gaseous products, but not exothermic enough for an explosion. Combustion of the product gasses will then occur. This explains why liquid methyl ethyl ketone peroxide, when exposed to flame, simply burns, creating a towering pillar of orange flame for a brief moment.

8CH3COCH2CH3 + 4H2O + 6(O2) --> 10H2O + 10CO + 11C2H4

The C2H4 burning with atmospheric oxygen explains the pillar of orange flame.

(out of time, will finish this post soon)

[Edited on 30-5-2002 by madscientist]




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[*] posted on 16-8-2002 at 08:20


Any carbon rich molecule that has a negative OB when submitted to deflagration or detonation will produce orange/yellow flame!

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[*] posted on 12-10-2002 at 08:14


so we could probably assume that it is the liquid form of MEKP that is used as a catalyst(hardener) for polyester plastics, dissolved into something.

I recently bought a small bottle (100 ml) with a stated content of 30-40 % MEKP
for 3 € at Biltema (for our swedish members:) . It is only labeled Oxydizing but not flammable which makes me curious about which solvent is used.

Any ideas anyone?

/rickard
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[*] posted on 12-10-2002 at 09:37


Maybe they're using a chlorinated hydrocarbon as the solvent, such as CCl2CCl2? The MEKP sold in solution commercially is the trimeric form (or so I hear).



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[*] posted on 14-10-2002 at 12:06
hydrochloric instead of sulfuric ?


MEKP looks very interesting. A friend made it recently and was not very happy when each time he added the H2SO4 it 'hissed' drop by drop...It took him about 3 hours to add 5ml. Does this sound right ? Also, could HCl be used instead ?
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[*] posted on 14-10-2002 at 12:13


If the temperature of the reaction is kept low, I suppose HCl could be used.

As for adding the H2SO4, I suggest diluting it prior to adding it to the solution prepared by mixing MEK with hydrogen peroxide.




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[*] posted on 3-12-2002 at 20:00
excellent


Hey madog, im gonna post here like you suggested. I i bet the ammonium nitrate was still a little wet. My friend dried it out the night before bet he accidently left it out in the open too long. I was still hoping it would still work. Thanks, I'll take the KNO3 suggestion and play around with it a little. I can't wait till i get some money and time on my break to try this out. I too would like to try to make some nitroglycerine to compare the sensitivity of the two. You said it failed to be detonated with lead picrate? It doesn't sound too bad. I will try to make some to get use to it. My dynamite I will try to replicate the real stuff in look as much as I can. This is gonna be so awsome.
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[*] posted on 3-12-2002 at 21:02
yummy mekp


yah, ive been in love with this b00tyful substance for a while. very resourceful! my friends use to sensitize there activated an with AP but they never liked that. and lots of the time, if left alone for a while, it wouldnt work later on (moisture?). just the AP would det. with mekp theyve never had impartial detonations. whats the longest everyone has kept this stuff ? i think the longest they kept this stuff around (by itselt, not mixed with AN) was around 3 weeks. thing about this substance that slipped there mines was if its soaked in to something and lit, it will detonate. soaked == confinement. i saw a friend dip less than 2mm of a match stick in this stuff, took it out, lit it, and *bang* no more match stick, just sore fingers. be careful ;) has anyone found out how fast this stuff dets ?
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[*] posted on 4-12-2002 at 13:32
like you said


Binary mz, I your post you said it was a great substance. I wonder why there is so little talk of what i also think is a great explosive. It seems better then AP at setting off AN. In your post, did you say that you left the MEKP and AN dynamite out for a while and it still detonated even though AN is very hydroscopic(I think that is how you say it)? I assume the dynamite is not hydroscopic. How sensitive is MEKP and AN dynamite? What is the mixture ratio you use? I think that MEKP has a det velocity of 4500 to maybe 5000 meters per second. It has a supposed density of 1 and 1.18g/cm3 for AP and its velocity is 5300 meter/second. Does the mekp form anything dangerous after being around for a couple of weeks like AP does? My last thing i been wondering is does MEKP get all sensitive when frozen like NG does?
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[*] posted on 4-12-2002 at 14:02


the lead picrate failed to detonate PETN.

the reason why nitro gets sensitive when its partialy frozen is because it gets chunks of ice in it to cause friction, its like if u threw gravel in it.




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[*] posted on 4-12-2002 at 14:04


the lead picrate failed to detonate PETN.

the reason why nitro gets sensitive when its partialy frozen is because it gets chunks of ice in it to cause friction, its like if u threw gravel in it.




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[*] posted on 4-12-2002 at 15:49


Yeah i know the reason for NG becoming sensitive is the little peices that freeze in it. So i guess freezing MEKP is like having little peices of the solid isomer of MEKP in it. If you threw non absorbant material into NG would it become sensitive, if not then why does frozen NG become sensitive? Is this true about MEKP? I want to be sure cause I am planning to make MEKP dynamite and store it in waterproof container outside it the woods. This is to be sure that when I retrive it won't be all sensitive and go off. Where I live it now goes below freezing every night.
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[*] posted on 4-12-2002 at 17:21


if u throw stuff like pebbles into NG it will of course become sensitive. i have heard of people shoveing detonators into dynamite and haveing it detonate, completely frozen NG is extremely hard to detonate. i have never heard of anyone detonateing it, i dont know the freezeig point of MEKP, but i would expect it to be low.



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