Sciencemadness Discussion Board - Methyl Ethyl Ketone Peroxide

Methyl Ethyl Ketone Peroxide

Pages: 1 2 3 4

Zinc - 12-4-2008 at 14:17

And the MEKP I tried to make with 12% H2O2. It actually did work

There is a small layer of MEKP on top that I tried to ignite and it would burn slow. But there is a big blob of clear MEKP on the bottom of the jar that I didn't notice before. I tested it and it burns very good!!

And I tried to make MEKP with 30% H2O2. I used the ratios at the beginning of the thread. Only I used 19% HCl instead if H2SO4 (I adjusted the ratio). Within seconds 10 ml of MEKP formed. I tried to ignite it and it burns the slow way. Now I will let it stand a few days and test it then again.

[Edited on 12-4-2008 by Zinc]

StevenRS - 12-4-2008 at 14:46

And we have a winner! Yea, thats it.

497 - 13-4-2008 at 16:20

Yesterday I mixed roughly 60 ml of MEKP/AP with roughly 100g AN in a large plastic pill bottle. The mixture filled it about 2/3 full. I found a nice big partially rotten stump and shoved the bottle into the center rotten out part. It detonated completely with a fuse and produced a cloud of brown rotten wood dust. It worked quite well. Next I'm going to try with a more neutral OB. This will need a detonator though..

StevenRS - 13-4-2008 at 18:34

Be careful using a fuse with MEKP, it likes to soak up your fuse and go bang before you want it to.

And someone with more experience, tell me, would a 9:1 ratio of AN:MEKP need a detonator?

[Edited on 13-4-2008 by StevenRS]

497 - 13-4-2008 at 20:15

I know it soaks into fuses, that's why I simply stuck the fuse in and lit it immediately.

I guarantee 9:1 ratio will not go off with a fuse. I even tried it with a detonator (not a very powerful one mind you) and it still didn't detonate. I think the minimum *reliably* fuse sensitive ratio it something like 2:1 but it depends on the particulate size of the AN.

Right now I'm working on figuring out the ratio of MEKP to EGDN that is fuse sensitive. I think it will be much more effective that straight MEKP.

[Edited on 13-4-2008 by 497]

Zinc - 14-4-2008 at 02:28

As far as I know MEKP and MEKP/AP are storage stable. Are MEKP/AP/AN and MEKP/AN also storage stable? I believe they are but I want to make sure as I have 300 g of MEKP/AP/AN and I think I will not be able to set it of in the next few days (perhaps even a week).

And for the 9:1 ratio I always use 7-10 g of lightly pressed AP to detonate it.

[Edited on 14-4-2008 by Zinc]

497 - 14-4-2008 at 19:12

Although I have never stored it, I would guess your mixture is stable. Unless of course you have some weird impurities in it. Sometime someone should do some sensitivity testing on that mix. I would bet its pretty safe and insensitive if the AN is ground fine enough.

The other thing I want to try is taking the 9:1 mix and adding enough EGDN to make it pourable (and increase the power a lot).

The detonator I used was maybe 2 ml MEKP/AP. The charge was only contained in Al foil so that doesn't help either. Have fun with that 300 gram charge

Zinc - 15-4-2008 at 01:02

Yes the mix with EGDN is very interesting

I would like to try it myself but first I have to buy H2SO4 to make EGDN.

And yesterday I set of the 300 g charge. We buried it around 70 cm underground and ignited it with a car battery from around 25 m. The explosion was very nice. Earth was flying everywhere!! The resulting crater was 1.2 m wide and 40 cm deep (it was soft ground). Very nice

Zinc - 18-4-2008 at 13:44

I have seen a video of a member at this forum (Axt) that used it and it worked. Axt can you please say what did you use for the detonator?

Did anyone else tried that mixture?

Axt - 18-4-2008 at 15:11

I've never mixed EGDN with MEKP. I have 50:50 by volume with NM, in which it seems miscible but is surprisingly insensitive. A commercial #8 strength detonator gives no detonation, below is consecutive frames.

nm-mekp.jpg - 14kB

Formatik - 18-4-2008 at 18:30

Are there any specs of the cm shock sensitivity of MEKP?

In PATR2700 A44 shock sensitivity of cTATP is given as 500 g wt, 10 cm using Bureau of Mines apparatus, but with another, a French apparatus ("petit mouton") used 50 g wt from 15 cm to get detonations 50% of the time. The 500 g weight value is unrealistic for cTATP, using 90 g wt from a dropping height of 3 cm it can easily be detonated. Even using weights significantly smaller than that from about the same height, it will detonate that's why the petit mouton value is more realistic when it comes to its shock sensitivity. It's not hard at all to see why there are so many accidents with this compound.

For a comparison, mercury fulminate is 5 cm with 2 kg wt using Bureau of Mines apparatus, and 10 cm with 455 g wt using the Picatinny Arsenal apparatus. Lead azide is 12 cm with 2 kg wt, and another result was with 500g wt 30-40 cm (Hg(ONC)2 was 10.5 cm in this same test),etc.

Where does MEKP fall?

Axt - 18-4-2008 at 19:11

This really isn't suitable for primary explosives but I did some tests,
http://youtube.com/watch?v=scL7sLKcBS4
http://youtube.com/watch?v=P5577gDwQZI

Both acetone and MEK peroxides detonated with a drop of 0-5cm (the lowest setting). The "hammer" in this case has a far greater surface area then the industry ones thus dont try comparing heights/weights with those. For the test a thin layer was spread over the entire impact surface. Though it does provide consistant results for the likes of PETN I used as a standard, which required a drop of 40-45cm, and ETN was 30-35cm (it has 5cm increments).

I know of no other drop test figures for MEKP.

Formatik - 18-4-2008 at 21:12

Quote:

Originally posted by Axt
This really isn't suitable for primary explosives but I did some tests,
http://youtube.com/watch?v=scL7sLKcBS4
http://youtube.com/watch?v=P5577gDwQZI

Both acetone and MEK peroxides detonated with a drop of 0-5cm (the lowest setting). The "hammer" in this case has a far greater surface area then the industry ones thus dont try comparing heights/weights with those. For the test a thin layer was spread over the entire impact surface. Though it does provide consistant results for the likes of PETN I used as a standard, which required a drop of 40-45cm, and ETN was 30-35cm (it has 5cm increments).

I know of no other drop test figures for MEKP.

Nice. I take it that's a 2 kg weight? 2Kg is definetly enough to set off cTATP, but so is even a 50 to 90g or less weight falling directly on it from as little as 3 cm.

Axt - 19-4-2008 at 12:25

Nope its a 3kg weight, though as I said its working on an area thats probably >10x that of the industry apparatus, thus the reason for the high drop distance for PETN.

Zelot - 28-4-2008 at 16:56

Would you be able to use sodium bisulfate for MEKP instead of sulfuric or muriatic acid?

zeppelin69 - 28-4-2008 at 19:18

Unless there is something about sodium bisulfate that I am unaware of, I dont see how it would catalyze the reaction. The use of hydrochloric and sulfuric acids is for the H+ ions, these help the peroxide molecules bond to the ketones and form the larger cyclic molecules of TATP, DADP, and MEKP (diMethyl Ethyl Ketone diPeroxide).

Tin chlordes, (II ad IV) are the only salts that I am aware of that will actulay catalyze the reaction.

Zelot - 29-4-2008 at 06:06

On the Wikipedia for sodium bisulfate it says that a 1M solution can get to a pH of 1.4. It is also sold it 4 pound containers at Longs for decreasing the pH in pools.

chemoleo - 29-4-2008 at 17:43

But 7 % of sulfuric acid (~0.7 M) gives a much lower pH than that (around 0.3, the value I found for 5% (w/w)), check Henderson Hasselbach! The 7 % is based on the prep on page 1, first post, where 5 ml is in diluted in 70 ml total.

[Edited on 30-4-2008 by chemoleo]

Zelot - 2-5-2008 at 06:19

I do know that sulfuric acid is a very strong one. But that isn't the point. I was asking if I could use that because I don't have any other acids, like sulfuric, to use.

Axt - 2-5-2008 at 06:25

Do you really need a 5 page discussion on something that can very easily be tried, thus the word 'experiment'.

Zinc - 9-5-2008 at 15:31

There is one thing I would like to say about MEKP/AN. It is extremely important how the AN was prepared for it. If AN is made by recrystallization from a fertilizer, dried and then ground it wont work very well because when the AN is drying in the oven it melts in the water it contains. So when in solidifies it becomes compact and nonporous and even when ground up fine it doesn't absorb MEKP good. On the other hand if the AN is dried, ground up partially and then heated again (but not hot enough to melt), ground up a little more while hot and then finally ground when it cools it becomes much more porous and absorbs MEKP much better. You can also notice the difference between AN made with only one heating (much harder to ground, and the resulting powder looks like compact particles) and AN made with two "heatings" (much easier to ground and particles look fluffy).

grndpndr - 11-5-2008 at 16:00

Ive followed along wth great interest the majority of threads for some time w/o posting
save1, cocerning the 'Indian' hindu or muslim it wasn't clear and his post desiring instructions safely manufacturing large quantities of a dangerous peroxide(MEKP) from an amateur chemistry forum rather than hire a company specifically equipped to design and operate such an endeavor.Surely a joke with us the butt of the fun.As to myself I am no chemist simply an interested very safety minded former military/civilian powder monkey for seismic exploration/ observer who was considering the possibility of a MEKP/double base smokeless powder such as hercules bullseye pistol powder which of course contains Guncotton/NG,some moderators/stabilizers.But the main point being i believe the powder containing near 40%NG/60% NC.I had heard
that this powder would High order detonate if confined with a powerful detonator and strong confnement such as in a pipe bomb of water pipe.The concern is MEKP compatible for short periods of a few hours.Also i assume he solvent properties of mekp would make a plastic conisistency the mixtuer and would then density be such that something akin to glass microballoons/powderd styrofoam be rquired for detonation despite the MEKP content of 10%-20%. Thoughts gentlemen?

zeppelin69 - 11-5-2008 at 20:35

Are you saying you are concerned with MEKP's stablilty when mixed with DBSP? I would think you have nothing to worry about in that department. If you are still worried about it though, why take any unnecessary risks? Just mix the MEKP and DBSP on site and detontate it shortly after. What do you plan on using for the detonator?

grndpndr - 12-5-2008 at 16:59

IF I were considering such a project I would likely use a compound detonator;1gr ful mer/1-2 gr pricic acid pressed in AL tubing just to be absolutely sure the detonator as adequate for the job.Im curious if some sort of microballoons styrofoam would be needed to reuce density /increase sensitivity? Though te MEKP itself should act as booster?Also a guestimate of appropriate percentages MEKP/double base pistol powder likely bullseye and should I expect the MEKP to act as a solvent with the NC.

Bert - 13-5-2008 at 07:37

Some have partially softened Bullseye brand DBSP with acetone, aglomerated into a solid "stick" dried it and detonated unconfined with no additional sensitizers.

Al is a good choice for contact with picric acid, but a poor one for contact with Mercury fulminate.

I think we may be straying a bit close to use, rather than chemistry for this board. Roguesci.org being down tends to do that around here...

grndpndr - 14-5-2008 at 16:02

Ive tried to ensure it was understood my interest was purely theoretical and not of a practical nature but considering todays political climate almost any discussion seems to have a tendency to tug on some folks shorthairs.(not speaking about legitamite members with genuine interest in the science behind the subjects presented)XYZ types particularly and frankly i cant think of a place more lkely to be monitored and thus avoided by real bad folks.

Zinc - 7-6-2008 at 13:23

A few minutes ago I wanted to ignite around 1 ml of MEKP/AP (50:50). I poured it in a metal dish and ignited it with a torch. Strangely it only burned with a small blue flame. When I blew on it (around 2 seconds after igniting it) It went off with a loud bang and a short lasting fireball (much shorter lasting than with normal deflagration). I never saw that happen before!! Did it ever happen to anyone else? And does anyone know why did it happen? I ignited those amounts of MEKP/AP the same way many times and always it only deflagrated.

zeppelin69 - 7-6-2008 at 14:54

Well considering that I have NEVER heard the mention of an organic peroxide and unpredictablity in the same sentance, I am at a complete loss myself. Personaly, I would do more research in increasingly larger ammounts untill you solve this mystery. Who knows, maybe you will be recognized with a darwin award for your efforts. Good luck and God speed.

StevenRS - 18-6-2008 at 11:17

It sounds like there was still an organic solvent in the peroxide mix. It slowly burned off, heating the mixture, and then made a quick DDT when the solvent was all burned off.

Zinc - 18-6-2008 at 11:33

That is possible but I have ignited a few other samples from the same batch and they deflagrated like usually.

MEKP/AP-Smokelss powder

grndpndr - 22-6-2008 at 09:36

In an earlier post I suggested/a sked if anyone was aware of a mixture of AP or MEKP and DBSP.(Double base smokeless powder). found such thing in a collection of info I hd laying about softening DBSP w/acetoe and mixing AP in a ratio of 1-1/1-3.I would imagine MEKP would soften the powder by virtue of its solvent effect on powders.Tried plain MEK and it softend the powder to plastic consistency easily so I would have to assume MEKP would do the same.The perception of the articles writer was the plastique ap was ery powerful as the DBSP also detonated after the acetone dried of course.No menton was made of a detontor just fused but I would personly think at least .25/.50 gr AP/MF etc detontor to ensure optimum vod.I woud thnk that the detonation of the DBSP with its high nitro content and NC content the VOD would be greater than AP/AN alone.What would the proper % be with mekp and say bullseye for a balanced HE or is that an imposible request due to the unknowns of the powder?

497 - 22-6-2008 at 23:02

I wouldn't count on MEKP being a good solvent. I tossed some MEK on a styrofoam packing peanut and it was immediately reduced to sludge, then I did the same with 50/50 MEKP/AP and there was almost no effect... So the only way to know would be to test it.. but something tells me it wouldn't dissolve.

I think it would be better just to grind up the DBSP into a flour consistency and absorb the MEKP into it. I wonder if a coffee would detonate DBSP? I doubt it, I think nitrocellulose is too insensitive for that... maybe if there was a high enough nitroglycerin content?

Also does anyone have an idea of the OB of DBSP? I would think it would be near neutral to reduce corrosion and toxic gases?

[Edited on 22-6-2008 by 497]

PVCglue mistake

grndpndr - 23-6-2008 at 00:54

PVC is far more chemicallyresistant to NC I thnk.Anyway I made a lazy mistake and the PVC glue cntains ONLY MEK and it DID dissove smoke less powder.IF mekp wont dissoleve DBSP guy could plasticize wth acetone mix in te proper amount of mekp run through a fine screen to regranulate and dry?Though I dubt it would dry (the mekp) once in a mxture with DBSP only the acetone.Lots of possibilitys here
fun thougt to play with.

IIC bullseye brand pistol powder contains somewhere around 25%- 40% NG

Somethng of a downer when considering high exp.will sometmes dramaticaly increase VOD when added to a modrae vel HE.
patent 6214140/ april10 details using ammnium picrate as a cheap way to rid mlitary stocks of the obsolete HE.With a det vel of 7000mps it only added 1000mps to ANFO at a 40% concentration?Interesting patent though

[Edited on 23-6-2008 by grndpndr]

[Edited on 23-6-2008 by grndpndr]

497 - 28-6-2008 at 16:28

Yesterday (in a dream of course) I mixed roughly equal volumes of Hodgdon Longshot shotgun powder with MEKP/AP. Absolutely nothing happened. I then added about 4 times the mixture's volume of acetone. It formed a very pretty pearlescent black and silver mixture. After lengthy stirring it became mostly homogeneous and sticky. I then poured it in a thin layer onto aluminum foil. It is now drying.

I'm hoping it will evaporate the acetone quickly, but I'm afraid it will just form a dry skin on top and remain full of acetone. I'm not sure how that could be solved. A little acetone shouldn't hurt things much, just reduce sensitivity.

I think it would be easier just to absorb the MEKP/AP into powdered gunpowder. I don't know how to grind it safely though. Maybe slurried with water in a blender? And a long extension cord on it...

Also the way I synthesize my MEKP/AP is by putting a 1:1 Acetone:MEK mix and a 1:1.5 battery acid:50% H2O2 in the freezer. Once they're cold I add a little of the ketone mix to the beaker of peroxide/acid until the the temperature rises up to 5*C or so. Then I leave it in the freezer for a few more hours and repeat the process until all the ketones have been added. Then I suck it out and wash it with water and its ready to go. It gets good yields (maybe 65-80% based on ketones IIRC). I just did a batch that that has a theoretical yield of 480 grams. Have yet to measure yield. It will hopefully go into sensitizing a big load of AN and sensitizing DBSP for a booster.

EDIT: I just measured the yield of the MEKP/AP synth, 221 grams of nice clean clear MEKP/AP after washing with water twice. 46% yield, not too good, but I was in a bit of a hurry. I'm happy with it anyhow.

I also checked on my DBSP based plastic. It seems to have lost its acetone quicker than I expected. It now has a stiff rubbery consistency to it, maybe stiff enough to crack if pulled quickly. I don't know how much acetone is left because I never weighed it, but it doesn't look like much at all. If one wanted something easier to mold, a higher ratio of MEKP/AP would help. Also using straight MEKP would improve its elasticity. It seems promising for a cast primary or sensitive secondary depending on the ratio. It does present a challenge because it shrinks a lot when it loses the acetone. Not sure how to deal with that.

[Edited on 28-6-2008 by 497]

grndpndr - 29-6-2008 at 04:04

I would seem the mixture would be less sensitive w/o the ap
crystals and even if the mekp wasnt intimitately mixed with plasticized powder the point is a booster to more easily detonate a bullseye type powder with reported det vel of 6600mps w/o confinement and with a small cap.I wasnt aware mekp would evaporate rapidly but to prevent that Id simply put it in a sandwich ziplock bag until use relatively soon. also IIRC Ap crystals 1/1-1/3 were mixed w/ plasticized dbsp by way of acetone which when the ap/dbsp was intimately mixed was allowed to dry after shaping or casting to the shape desired and a hole for the cap formed.Doubt Id drill the hole however!LOL If anyone were to find out more say using a test plate
Id love to hear the results.

[Edited on 29-6-2008 by grndpndr]Patent using 40% ammonium picrate to anfo above added only 1000 fps not mps.

[Edited on 29-6-2008 by grndpndr]

[Edited on 29-6-2008 by grndpndr]

[Edited on 29-6-2008 by grndpndr]

[Edited on 29-6-2008 by grndpndr]

497 - 30-6-2008 at 04:18

There are no AP crystals involved. Personally I would never touch AP crystals, I like my fingers. AP is very soluble in MEKP so it never crystallizes. But, judging by a post on E&W the presence of AP does sensitize MEKP a bit even when dissolved.

MEKP does not evaporate fast at all. I have left open containers with a little MEKP in the bottom and came back many days later and its still there.

I think I used much more acetone to dissolve the DBSP than needed, 1:1 would be more appropriate I think. Dissolving DBSP in acetone and than adding MEKP/AP would be easier too.

I (or someone else) should do some sensitivity testing of the plastic, I'm a little scared of it, having no way of knowing its sensitivity.

I think for a booster it would only need 1:6 MEKP/AP:DBSP or so. Made pourable with minimum acetone and then cast around a detonator. Should work well.

My idea for explosive train is: 5g 1:1 MEKP/AP:DBSP ---> 200g 1:6 MEKP/AP:DBSP ---> 10,000g 1:1:3:3:22 MEKAP:Charcoal:DBSP:Al:AN

I want plenty of sensitizer in the main charge because I will probably end up using AN with 30% ammonium sulfate in it. I have all the materials needed, just lack the time and proper circumstances to try it any time soon.

Overall I think there is a lot of potential for powerful detonators and boosters made with MEKP mixed with other more powerful explosives. I hope this discussion isn't getting too practical, I'll try to keep it theoretical if I can.

[Edited on 30-6-2008 by 497]

Zinc - 30-6-2008 at 05:16

If I were you I would remove charcoal from the mixture. And that mixture should be used immediately after you make it as it contains Al and organic peroxides+metals=bad.

497 - 30-6-2008 at 12:06

Aluminum is passivated with an oxide layer that renders it quite innert to attack by such weak things as organic peroxides. Other more reactive metals would definately be a bad idea without further testing.

And why remove the ground charcoal? I used it mainly to correct the OB, and to sensitize it, I've seen multiple patents that state it helps sensitize AN. If you're thinking the Al will correct the OB, I'm going to be using pretty coarse Al that will probably not take part in the explosion, hopefully it will start burning afterward and ignite some fuels that are placed around the main charge to get a thermobaric effect.

Zinc - 30-6-2008 at 12:39

Yes charcoal sensitizes AN but much less than MEKP/AP, AL and DBSP. So in your mixture it is more of an desensitizer. And it decreases the oxygen balance in your mix (which is already oxygen deficient, especially with your AN containing 30% ammonium sulphate).

497 - 30-6-2008 at 12:50

No it is not already oxygen deficient if i calculated right.

15.5g AN produces 3g oxygen

6.6g NH4SO4 is OB neutral

1g MEKP/AP uses 1.7g

As I said earlier I don't think the course Al will have much of an effect on the OB, I could be wrong.

Unless the DBSP is quite oxygen deficient there is still a need for something to correct the OB. There are many things that could work, sugar, alchohol, ethylene glycol, diesel, etc. I picked carbon because it was the most concentrated OB reducer. Maybe there a better ways to do it.

1g C would use 2.6g oxygen, maybe a little too much, so less could be used, or something else more powerfully sensitizing maybe?

Edit: Its OK zink, it happens to the best of us. I did think about using fine Al, but alas I do not have any, nor have I seen any locally. And I don't have the time or desire to order it off the internet right now. Maybe someday. The only way would be to build a ball mill...

[Edited on 30-6-2008 by 497]

Zinc - 30-6-2008 at 13:38

You are right, I was wrong sorry.

Perhaps you could substitute a part of the coarse Al with fine Al?

grndpndr - 1-7-2008 at 03:07

Plastc sndwic bgs have never presented a problem w/decomposition.Polyhydrocarbon plastic is the one that has problms with MEKP/AP.AL is fine i you want a bright flsh and a bit more heave with your HE but it wont add any det velocity.If you want to make a dust bomb- FAE , If I recall 1b he-al/5lbs exp. dust-charcoal/flour/gasoline etc PM as i do think that qualifies as a practical app.

PS Sod nitrate/mekp also makes a nice dynamite a ratio of 44ml/gr mekp/50gr sodium nitrate is about right I believe. fertilizer grade sod nitrate adequate 15%n cost some 8-9$ at the local hardware 4lbs,works for nitrations as well Im told.
Im very interested but My aquaintance has become enamored of ammonium picrate-TNP-lead picrate firing train due to high vod/simplicity. VOD suitable for HEAT and platter charges.And as finances are tight what is suitable for the most applicatons takes precedence.

PS; exp dust is bagged and placed on top of HE and layer of coarse AL.4-7lbs overpressure kills and destroys stick built +
buldings.Small can 3 in x 1 1/2 he/al-5lbs flour,2lbs coarse flake AL,1/2 gall gasoline will destroy 2000 sq ft bulding.

[Edited on 1-7-2008 by grndpndr]

[Edited on 1-7-2008 by grndpndr]

[Edited on 1-7-2008 by grndpndr]

grndpndr - 18-7-2008 at 00:18

MEKP/DBSP,
if the Mekp doesn plastize the powder as expected i would simply put the powder in a coffee mill and reduce granule size(to stable for problems) and mix with mekp w/o acetone as a possible desensitizer in a sandwch bag and detonate immediately or save for week or less and detonate in that form.Same method used with Mekp and AN nd IF the DBSP gives ful VOD of 6600mps that would be a simpe OTC med/high velocity HE. Possibly suitable for platter charges possibly even cone SC/cylndrical SC?

497 - 19-7-2008 at 00:08

Well I'll let you try the DBSP in blender idea for yourself, considering the fairly high percent NG in it, I'm not about to take that risk. I would think it would be safe, but I'm not sure enough to do it, if you know what I mean. I like my hands the way they are...

I did however try a detonator using a DBSP/MEKAP mix. I took an 8 inch piece of 1/2 inch electrical conduit and welded one end closed and then filled it with straight DBSP and the added MEKAP until it seemed to be completely full. Then I epoxied the other end closed with wires passing through. A piece of stainless steel wire was used as a crude EBW since I didn't have nichrome. 24 volts from 2 lead acid batteries initiated it perfectly. It in turn initiated a booster of 150g DBSP + 50g MEKAP + 10g picric acid. The booster in turn nicely initiated 7 kg of sensitized 70:30 AN:Ammonium sulfate fertilizer. A good dream it was.

[Edited on 18-7-2008 by 497]

Zinc - 19-7-2008 at 00:57

Very nice!!

With what did you sensitize your fertilizer?

grndpndr - 19-7-2008 at 01:19

Nice test butTNP s seemingly pretty sensitive itself, ive used just a grm of lightly pressed fm seperated by a piece of tissue to detonate a comp detonator wth a several gram booster of TNP which should by itself be adequate booster at 7400mps.I really doubt ill need to reduce DBSP by mechanical means Im still of the opinon if MEK will plasticize NC powder why not MEKP?Or am i missing somethng?I dont have any great fear of DBSP as Ive been reloading most of my adult life never have I seen powder explode or even deflagrate from rough handling and ive tried a bunch of methods.
Still never a coffee blender w/DBSP!if the MEKP wont plasticize the bullseye the flake size of bullseye is very small anyway and I wuoldnt think a problem.I wonder if youve seen the differece in a witness plate using mekp and AN vs plain MEKP/AP? no comparison the mekp an dynamite holing the witness plate whle the plain mekp simply denting it.Very curius to see if a potentially more powerful composition of MEKP/DBSP will perform or dissapoint.

did I misread your post and you included/mix the picric acid in the booster/detonator with the mekp/DBSP?

[Edited on 19-7-2008 by grndpndr]

497 - 19-7-2008 at 01:26

I figured you'd like that. Lets see, I'll have to dig up the notepad file I wrote up to keep things organized.

I made plenty of effort to sensitize it. To roughly 15 pounds of fertilizer I added about 100g MEKP/AP, 390g R/C fuel (15% NM, 10% oil, 75% MeOH), 30g ground activated carbon. Then into the top 15% of it that was closest to the booster I mixed in 50g course aluminum (all I had

), 30ml 50% H2O2, 200g DBSP and a dash of CuSO4 for flavor. About 85% of the fertilizer was ground in a coffee grinder, the rest being left as prills. If I had more time and materials to sensitize it I would have detonated all 40 pounds of my fertilizer.

I placed several gallons of gasoline and acetone around it in hopes of getting a little thermobaric action, but alas, it didn't ignite.

I wanted to get a movie of it but my camera is at a friends house. It was impressive, the largest detonation I've ever witnessed. I was roughly 150 feet away behind my car and I still felt a good thump.

EDIT: Yes grndpndr I realize my detonator and booster were very much overkill.

There's a pretty big difference between "rough handling" and coffee grinder

And trust me on this one, MEKP will not dissolve DBSP or just about anything else as far as I've seen. There is a vary large difference between it and MEK. After all, does acetone peroxide dissolve things like acetone does??

But as I said earlier, MEKAP mixed with plain unground DBSP seems to work just fine.

[Edited on 19-7-2008 by 497]

grndpndr - 19-7-2008 at 06:41

MEKP/DBSP,Most impressed with ANFO details .Would have loved to winess.first Ive heard of actual use of a low % nitro race fuel.in the past year 80% NM was available only last year IIrc but 55% max as of present and this diffcult to get afaik case lots may be required.
Far different from strolling into auto speedshop and buying 98% for mixing hobby fuel at $40gall!

In any event the bullseyes very fine and it occured what effect an amount of ground AN/mekp/DBSP would produce.I ws thinking 20/25ml-grams mekp to 200 grms AN- 100gr/100gr DBSP?

You shoud have had an air fuel effect if the gasline had been placed on top of your HE with a little AL(what used to be called a dust explosive) with the amount of he used afew gallons of gas/coal dust 5-10lbs/5lbs flour shoulda been spectacular!!

A money-saving breakthrough?

DougTheMapper - 16-8-2008 at 15:33

I have a suggestion:

Suppose that instead of buying costly concentrated H2O2, or spending the time to distill it yourself, you made it?

I'm talking about sodium percarbonate. Pounds and pounds of it can be found as some OxyClean products, between 50-60% mixed with sodium carbonate. In water, sodium percarbonate yields hydrogen peroxide and sodium carbonate (which is already in there anyway if you're using supermarket sources).

The sodium carbonate/percarbonate mix needed to make sufficient quantities of MEKP (or TATP) might interfere with the filtration step of TATP because there will probably be too much leftover carbonate to be completely in solution. This filtered mix of TATP and sodium carbonate may be more sensitive than TATP alone, and could be highly dangerous. Personally, I favor MEKP over TATP because of lack of sublimation and ultra-high sensitivity.

Anyway, you'll need to go crazy at the acid catalyst step to neutralize all the carbonates. I use HCl, so I'd end up with a mix of NaCl, MEK, MEKP, H2O2, and venting CO2. Also, maybe a bit of NaClO, which would go to NaCl and O2 in the presence of H2O2. Hey wait - the conversion to NaCl might just make the TATP filtration possible! Just make sure to wash it well to get rid of those gritty salt crystals....

Because of the nonpolar nature of MEKP, (hence the floating layer on top), I don't think it would be affected too much by all the dissolved minerals in the production bath.

So, one would need MEK, OxyClean powder stuff, water, and hardware store HCl. I like it.

I need an expert opinion on all this - what do you think?

Thanks,
-Doug

[Edited on 16-8-2008 by DougTheMapper]

497 - 21-8-2008 at 17:40

I don't see why that wouldn't work as long as you neutralized all the acid. That would take quite a lot of acid, but it is cheap at the moment. You might run into problems if the MEKP sinks the the bottom and mixes with the precipitated salt. Might make separation hard and increase sensitivity. Using sulfuric acid might help with that, increasing the density of the aqueous layer. I suppose after the MEKP was formed you could just add tons of water and dissolve all the salt. Also dealing with the huge amount of foaming that would occur when neutralizing the Na2CO3 might be a pain. You'd just have to try it and find out.

Still it would be a very useful thing if concentrated peroxide becomes (more) regulated. They would have a much harder time regulating such a widely used cleaning product like OxyClean, etc. Hopefully there aren't impurities that would cause problems.

PS. Don't use a product that contains bleach (or add it), it may greatly sensitize the MEKP. It might also inhibit it, or form unwanted byproducts.

DougTheMapper - 23-8-2008 at 07:33

Suppose the MEK was repeatedly dripped through a column of sodium percarbonate, all at less than 0C, thereby converting it to MEKP?

Does the H2O2 need to be aqueous to facilitate the reaction?

If that worked, one wouldn't have to worry about lots of acid loss. I don't know if the reaction would even take place without the acid catalyst however.

497 - 24-8-2008 at 12:02

As far as I know the reaction requires acidic conditions to proceed. Then again I've never heard of anyone trying it in alkaline conditions...

I don't know if the reaction requires aqueous conditions, I've never seen it done otherwise.

I did have an idea that might reduce the amount of acid need: make a concentrated percorbonate solution and then cool it to 0*C or below, that will reduce sodium carbonates solubility to below 7g/100ml, but I don't know if it would precipitate regular sodium carbonate hydrate or reprecipitate the percarbonate. I imagine there is an equilibrium between precipitating hydrate or percarbonate, so it would depend on the concentration.. It is manufactured by spraying anhydrous sodium carbonate with >55% hydrogen peroxide solutions.

Leander - 24-8-2008 at 12:33

A friend of mine once concentrated some hydrogen peroxide to a concentration of ~55% and prepared TCAP with conc. H2SO4 as a catalist. The yield was somewhat lower than the 'traditional' method with the exact same molar ratio's of H2O2/Acetone/Acid, only with a much higher water content. So my guess is that the aqueous environment is necessary, although I can't really explain it scientificly.

[Edited on 24-8-2008 by Leander]

497 - 24-8-2008 at 17:00

In the conditions you just gave there would still be plenty of water present. Maybe less than normal, but still plenty, and things that require aqueous conditions don't always require a lot of water, just a little.

I suppose if nothing happened when you mixed dry percarbonate with MEK, you could always try dissolving some water in the MEK...

I'm pretty sure the acid is required to catalyze the reaction though. I calculated a (room temp) saturated solution of percarbonate could make a 5% H2O2 solution. You could try using NaHSO4 to acidify, it is cheap and OTC in large quantities. The resulting Na2SO4 has a low solubility at 0*C so most of it could be removed by filtration before adding the MEK. That might not be a bad way to prepare H2O2 solutions in general. Through repeated "dissolve percarbonate-acidify-filter-repeat" it may be possible to produce fairly concentrated H2O2. You may run into problem with impurities in consumer percarbonate. Also some of it may be treated with 150*C air to decompose the H2O2 and create pressurized microbubbles of O2 in the crystals that result in a desirable foaming action when dissolved.

There are MANY other perhydrates (aka peroxyhydrates) besides sodium carbonate perhydrate. See US patent 3140149, it has a pretty long list of them (some new ones discovered since then). Even one salt, Na3PO4 for example, can have a large number of different perhydrates or perhydrate/hydrate adducts. Some of them my be explosive on their own. I think the highest H2O2 content one I found so far is K4P2O7*7H2O2.

[Edited on 24-8-2008 by 497]

DougTheMapper - 23-5-2009 at 15:27

Hello again -

I've finally rekindled my interest in chemistry, and I have a few questions I'd like someone with a more qualified opinion than myself to answer.

I plan to use HCl in place of the H2SO4 in this synthesis. Because HCl only has one protonizable hydrogen as opposed to H2SO4, do I need twice as much to achieve the same acidity? (I've already compensated for the difference in concentrations.)

Also, it is extremely economical and convenient for me to purchase 3% H2O2 at the local dollar store. Unfortunately, this makes the reaction vessels rather large and watery. After the 24 hour chill period, do you think it is possible to use a syringe to extract the large amount of acidic water under the MEKP prior to the acid neutralization step? This would save me a lot of money in bicarbonate.

Also, instead of leaving the prepared MEKP out to lose water, what about washing it over some anhydrous MgSO4? I'd rather not have any accidents... Perhaps I should store it in a container with a bag of MgSO4(anh.) suspended above the liquid.

Thank you very much,
DTM

[Edited on 23-5-2009 by DougTheMapper]

Leander - 24-5-2009 at 03:07

The PH scale is based on the molar ratio of H+ in solution. 1 mole of H2SO4 gives 3 moles of H+, while 1 mole of HCl gives 1 mole of H+.

3% H2O2 is probably not going to work, because it dilutes the reactants so bad that the reaction simply doesn't runs to completion.

Separation is fully based on the density of the spent acid/H202 mixture. My Mekp actually floated on top of the spent acid, and then sunk again after draining with water. When using concentrated chemicals the MEKP can simply be decanted off, and then neutralised. Neutralising all of the acid is indeed quite a waste.

Further making large amounts of MEKP is really dumb. The stuff is so sensitive that 2-3 drops soaked in tissue paper can be set of with a 200 gram hammer from 3cm height. I never made it again after discovering that.

[Edited on 24-5-2009 by Leander]

497 - 24-5-2009 at 20:37

Quote:

The stuff is so sensitive that 2-3 drops soaked in tissue paper can be set of with a 200 gram hammer from 3cm height.

I think most of the danger can be avoided by only using plastic containers and tools to manipulate it. It is far harder to get it to detonate from plastic on plastic impact..

DougTheMapper - 30-5-2009 at 11:04

As always, I am extremely cautious. At no point will any MEKP be contained in glass or metal, and containers used will be spotlessly clean and not have snap lids.

Synthesis Complete

DougTheMapper - 6-6-2009 at 16:33

Having failed to locate a source for >3% H2O2 solution, I tried the following with much success:

460ml 3% H2O2
31ml MEK
20ml 31.45% HCl

I started by measuring all the reactants and chilling the acid and MEK in the freezer. I then simmered the H2O2 for several hours (without boiling) in a clean container until only 75ml remained.

I chilled the 75ml H2O2 in the freezer. I then combined the cold H2O2 and MEK in a 200ml flask, and slowly stirred in the acid. The mixture immediately clouded and large globules of insoluble material rose to the surface. I placed said flask in the refrigerator at 2 degrees C. After several hours, the mix had separated fully, leaving a milky bottom layer underneath a clear top layer. A sample of the top layer was drawn for analysis, and detonated with an earsplitting crack when hit with a hammer on an anvil.

I plan to wait the full 24 hours to let any remaining reactants do their job. At this point, I will draw off as much as possible from the flask and deacidify it in a NaHCO3 bath. It will then be transferred to a container placed in a bell jar with anhydrous MgSO4 for desiccation.

Yield is TBD, but I would estimate c. 20ml. Further bulletins as events warrant.

-DTM

Isolation Complete

DougTheMapper - 8-6-2009 at 08:13

Hello everyone, it's me again, and it's time for a follow-up.

I learned some lessons during the isolation process which I'll share for the benefit of future chem enthusiasts traveling this road.

First off, I'm pretty sure I used too much HCl. After all, it's only the catalyst. This caused big problems during neutralization when my bath became nearly half a liter in volume to fully neutralize 25ml of MEKP. I doubled the acid content in the instructions so I would have the same hydrogen ion concentration (H2SO4 vs. HCl), and paid for it in the end. I will try my next batch with half the HCl and post results.

I would also recommend neutralizing in a clean florence or volumetric flask, then adding water to push the MEKP (which floats) into the neck for easier extraction. I was left trying to suck a 3mm layer of MEKP off 500mL of bicarb. solution in a beaker, which was neither fun nor efficient. I ended up using a plastic paddle to dam up the MEKP as I poured the solution out from under it. I lost a bit that way, and MEKP has a strange habit of sticking to glass. I lost a good amount on the walls of the beaker, not to mention the stench of all that exposed MEKP-covered surface area.

If done in the flask, I wouldn't expect odor to be problematic. In my unfortunate case, however, it was quite prolific. It smells like MEK mixed with sage and pepper. It's quite unique.

Anyway, I managed to recover about 10mL after my smelly fiasco was over. I am certain, however, that I could have recovered at least 20 if not for poor equipment choice.

One last note: everything with MEKP on it has to be rinsed in MEK (or some other solvent) to remove it. Water is completely ineffective. I have not tried soap, but I plan to next synthesis.

The final product is as expected - detonates loudly when struck with a hammer, undergoes rapid deflagration when heated and unconfined in small amounts. It resembles light mineral oil in both color and viscosity.

-DTM

grndpndr - 18-8-2009 at 08:12

Ill post my 2cents as having success with 3% Hydrogen peroxide.Yield would be considered atrocious but as used to get an first hand Idea as to its properties It was a successful inexpensive lab.
That gave rise to other experiments,foremost an oxidizer, AN 100gr and MEKP 11gr/ml (OB) that could be a useful simple booster for difficult safety exlosives.A simple rehash for sure but someone may percieve different uses, materials- addittions.

[Edited on 18-8-2009 by grndpndr]

User - 18-8-2009 at 08:58

Indeed quite remarkable that 3% is strong enough to drive the reaction.
Not that i like organic peroxides but still I wonder if other explosive peroxides could be made using such low concentrations.
Also, often hydrogen peroxide in the stores arnt in a cool/dark place and could well be there for months , making the concentration even lower.

grndpndr - 21-9-2009 at 17:24

I would think a large turkey baster would work assuming the acid concentration didnt wreak havoc with the plastic components.
When down to the last of the liquor/mekp I placed it in a seperatory funnel.At the time 2000-2002 I was careless enough to stir not as carefully as I should have with glass on glass containers /stir
stix.:Fortunately no Darwin award that year!My peroxide year
well say,little ap as Im a chicken at heart w/no heart for pressing AP into dets even though very littles required for mekp/AN.Last of the peroxides for me but I did like the MEKP,the idea of a liquide explosive added to AN reminded one of a kinepack mix, sadly the brisance wasnt there.Neither is the AN/NM easily available anymore

[Edited on 22-9-2009 by grndpndr]

Second Synthesis

DougTheMapper - 8-10-2009 at 20:39

I use a 10mL syringe with a curved tip that I got when I had my wisdom teeth removed. I, as with grndpndr, am a chicken when it comes to sensitive stuff like this. I work behind quite a shield.

Anyway, I isolated the stuff for the second time a few days ago, this time in a round-bottomed flask. The reaction bath was about half of this 250mL flask, and the neutralization solution was added in excess until the MEKP was forced into the neck of the flask. extraction was a breeze, and yield was considerably higher than my last iteration. Oh, and I also used HALF the HCl this time with no perceptible change in yield.

The flask is covered in condensation. The MEKP was foggy until it sat in the orange collection vial for about a day, where it became totally clear with a small bead of water at the bottom, which was removed with the syringe.

I have recently acquired about 40g of AN, and I plan to make an 8:1 AN/MEKP charge this weekend. Pics and vids will be available.

[Edited on 9-10-2009 by DougTheMapper]

grndpndr - 19-11-2009 at 05:48

Theres a topic in reagents and appaatus regarding concentrating H2O2.from what Ive gathered unless your shooting for unnescessarily high % for these peroxide synthesis the simplest method is likely freezing.It has been in my limited experience.It will likely involve some guesswork as to the ultimate concentration at least in my case but I would think it would be relatively accurate/effective to 30-35% and higher,maybe not advisable for us beginners(higher 35%H2O2)That at least would cut down on quantities
involved as well as improve yield guite a bit(over 3%H2O2) but still a very dangerous product the result.

And as the years have flown by I have become increasingly attached to my extremitys so I personally wouldnt try peroxide labs any longer although I eagerly read others 'adventures' .Regards

[Edited on 19-11-2009 by grndpndr]

gnitseretni - 19-11-2009 at 07:20

At what concentration does H2O2 leave a stain on your skin? 35% H2O2 leaves a stain. Perhaps after you froze 3% H2O2 a couple of times, put a drop of it on your finger to see if it'll leave a stain.. if so, use it and report your yeild; If not, freeze it until it does leave a stain.

Dunno - might work, no?

grndpndr - 19-11-2009 at 17:20

Id prefer to not use my skin as a sort of litmus paper.The 60% or thereabouts Ive heard possible by freezing probably wouldnt be to healthy for living tissue.In the past Ive frozen a known quantity measured what remained and subtracted a bit for loss.Probably close enough though Im sure theres a method to accurately measure %.

gnitseretni - 19-11-2009 at 20:11

Oh well, just a thought

Microtek - 29-11-2009 at 03:46

Just do a redox titration of the concentrated peroxide using a suitable indicator.
One possibility would be to use a solution of KMnO4 (of known concentration) to oxidize the peroxide. If the reaction is acidified with sulfuric acid, the permanganate ion goes quantitatively to Mn(II) which is colourless. So the endpoint is indicated by the persistence of the purple colour.

If you want decent precision, you will have to prepare the KMnO4 soln carefully, as there is always some MnO2 in the KMnO4 you buy (no matter the grade). If you intend to do the titration immediately, you can just standardize the soln on sodium oxalate with reasonable results, but you won't be able to use the soln the next day.

Zinc - 15-11-2010 at 12:06

Sorry to bring up an old thread, but I belive this is the best one for the question I have.

Hww stable is the 50:50 MEKP/AP mix in mildly basic conditions?

I ask because I have some AN that is slightly basic (I belive due to MgO contamination), so I am wondering how safe is it to mix it with the MEKP/AP. I know that in the short run (an hour or two of contact nothing happens, at least nothing observable) But what about 24-48 hours?

Bot0nist - 7-3-2011 at 07:58

Has anyone experimented with MEKP on C6H7(NO2

3O5. I did a search <a href="http://www.sciencemadness.org/talk/search.php?token=&srchtxt=mekp+nitrocellulose&srchfield=body&srchuname=&f[]=all&srchfrom= 0&filter_distinct=yes&searchsubmit=Search">here</a> and <a href="http://www.sciencemadness.org/talk/search.php?token=&srchtxt=gun+cotton+MEKP&srchfield=body&srchuname=&f[]=all&srchfrom=0&am p;filter_distinct=yes&searchsubmit=Search">here</a> but found nothing.

I tried it yesterday, but the MEKP was still a little "wet" with mek and it melted the cellulose nitrate. After letting the mekp dry a bit it seemed to withstand it without going all gooey. I would love to experiment more, but I get very nervous when making mekp and restrict myself to about 3- 5 ml in those little HDPE test tubes, so I haven't been able to run a good control series to compare to. I have 5ml drying now and will try to get around to doing some comparisons tonight.

My mekp was made with 15% H202, 95% H2SO4, and pure mek with the proportions adjusted for concentrations.

The cellulose nitrate was double nitrated in a H2S04 + NH4NO3 using 55ml to 31g and 5 grams of cellulose. 3 hour nitrations with agitation each time.

grndpndr - 8-3-2011 at 03:38

eagerly awaiting results of your experiments-would particularly like to hear of your perception or actual results on test plates etc.

Off topic, it was asked but not answered a few pages back
concerning a chlorate as an oxidizer for MEKP.Specifically sodium chlorate as the oxidizer was the question but Id like to hear if there were any contraindications to using k chlorate,ammonium perchlorate etc.Theoretically of course.

trezza - 8-3-2011 at 06:56

I've experimented with MEKP before.
-------------------------------------------------------------------
Synthesis of Methyl Ethyl Ketone Peroxide using HCl
-------------------------------------------------------------------

Chemicals used:

38mL 30% Hydrogen Peroxide
25mL 100% Methyl Ethyl Ketone Peroxide (PVC Primer solution)
15mL 30% Hydrochloric acid
5-10% Sodium Hydrogen Carbonate solution

Everything was chilled in the freezer and an ice water bath was prepared before I started the reaction.

The H2O2 and MEK were mixed in a 250ml beaker and placed in the ice bath, then over a period of 10 minutes the HCl was added dropwise to the solution, the temperature was watched closely and kept below 5 degrees C.

Once all of the acid was added I moved the beaker to the refrigerator still in the ice water bath for 18 hours.

When the beaker was removed there was an oily layer layer on the bottom and a thin oily layer on top of the solution.

200mL of Sodium bicarbonate solution was placed in a 1L beaker and the MEKP solution was poured into that, there was some frothing and fizzing, I stirred it for 10 minutes until the MEKP layer had been broken up a few times and the fizzing stopped. I collected the MEKP in a syringe and left it in a large beaker to dry.

Final Yield was about around 10mL.

---------------------------------------------------------------------
Testing: Methyl Ethyl Ketone Peroxide/Potassium Nitrate
---------------------------------------------------------------------
I have seen TATP/AN combinations used to detonate ANFO
I had also heard of potassium nitrate and TATP mixtures giving semi successful results so I decided to try MEKP/PN

I wanted to find a good ratio so I decided to Balance the oxygen, I used this equation.

X represents the number of Carbon atoms, Y represents the number of Hydrogen atoms, Z represents the number of Oxygen atoms. M represents the number of metal oxide molecules which can be made from 1 molecule of each compound.

Here I made a graph which shows the balance of oxygen for several energetic compounds...

From that I can tell that a perfect ratio of ammonium nitrate to nitromethane (NM) would be 66:33 which sounds correct as people seem to use mixtures ranging between 25:75 and 50:50
My working out is attached in a .txt file below.

Now to business. I used a ratio of 1mL:4.5g of MEKP to Potassium Nitrate which gave a consistency similar to damp sand, this was placed in a cardboard tube and 1g of HMTD was used to detonate it. There was quite a loud bang, it was more like a thud, similar to what I would expect from an ANFO detonation, it certainly seemed more powerful than 1g of HMTD on its own so I could gather the MEKP detonated. Afterwards I checked for any sign of the Potassium nitrate on the ground but I couldn't find anything, I'm fairly sure the MEKP/PN detonated completely.

[Edited on 8-3-2011 by trezza]

Attachment: oxygen balances.txt (2kB)
This file has been downloaded 1008 times

Bot0nist - 8-3-2011 at 08:36

I will have those test results as soon as I can figure out a good way to quantify the deflagrations, as I would hate to just present you all with just my perceptions.

My first thought was to use a poster that had one inch black increments in a + pattern. I mounted the cotton on a wire so that it was suspended in the center of the plus. I then thought I could use my camera to determine the size of the resulting fireball, like on mythbusters. That failed because my camera cant handle the extreme light and just goes all white at the moment of initiation. :mad:

My next idea was to place the 'charges' on a piece of foil that rests on top of my digital scale. I planed on taring it out, and then measuring the sudden increase in pressure on the scale. This also failed, as the spikes happened to fast for the scale to accurately measure them. :mad:

I can't really think of a good way to quantify the deflagrations using the tools I have, so I will re-due the tests and post some pictures/short videos of the deflagrations, along with my personal observations. That isn't the most scientific approach, but I am at a loss.

I'll synthesis a few more millimeters tonight and I will try to have some meaningful results up by the weekend.

Chordate - 8-3-2011 at 13:02

Back in the 1500s, when star forts were in vogue, a lot of effort went into zeroing cannons within fortifications, such that if one of these forts was assaulted the artilleryman would know at exactly what angle to align their cannons in order to hit an attacking force at important ranges relative to the surrounding fortifications.

The problem then became variable gun-powder quality, the way they tested this was to place a cannonball of known weight in an iron cup next to a metered pole, then ignite a measured amount of gunpowder underneath it and see how high the ball went. Its crude, but it would be do-able. Calculating the amount of energy released accurately wouldn't be trivial, but if you had a reference sample of known qualities you could calibrate that scale and then work from there.

Bot0nist - 8-3-2011 at 13:26

Thank you chordate, I will keep that in mind when I am tring to rig something up. I am a bit scared to try and 'throw' anything with the MEKP. I wonder if the brisance of the compound would cause a problem.

Also, I saw some tests using iron plates to test the power of blasts. It seemed to work pretty well, but I would like to avoid any detonations if possible. I know a small amount of MEKP will detonate if soaked into something or confined, but I have only initiated amounts that resulted in a large deflagration, even when soaked into cellulose nitrate. I suppose I could slightly scale up my tests to get a DDT since I am already set up for the possibility of a full order detonation occurring, just for safety's sake. (Mounted camera, Plexiglas shield, and a remote initiation system.)

[Edited on 8-3-2011 by Bot0nist]

Bert - 9-3-2011 at 18:28

Google the terms "ballistics pendulum" and "ballistics mortar". These were more commonly used for HE than the eprouvette, and you won't need a range to chase cannon balls down. The US Bureau of mines in particular was fond of the ballistics mortar-

Bot0nist - 13-3-2011 at 09:01

Got a few observations for anyone who is interested.

Methyl Ethyl Ketone Peroxide on Cellulose Nitrate.

0.3 grams of C6H7(NO2

3O5 and 0.5ml of M.E.K.P. are the amounts used in all tests.

All amounts were lightly confined in aluminum foil tubes measuring approximately 1 inch long and 2cm in diameter, with four layers of foil going around.

'Charges' were placed on a 1/4inch thick disk of balsa wood about 8 inches in circumference and initiated by a butane pen torch that is attached to a pull arm with a 20ft piece of string.

For some basic controls I first filled two identical tubes with only 0.3 grams of cellulose nitrate and twisted the ends shut (using welders gloves and a face shield of coarse, overkill, i know.) Both of these tests proceeded about how you would expect. As soon as the flame touched the foil packet, a five or six inch flame popped open one of the ends of the tube and erupted outwards.

Next I dripped 0.5ml of M.E.K.P. into one of the foil packets with no cotton at all. This took slightly longer to ignite than the cellulose, but still probably less than a second from when the flame touched the foil, a satisfying pop was heard with a tall column of orange fire, and a clean hole was punched upwards through the foil. Still no damage to balsa wood disks.

Next up I filled 3 foil tubes with 0.5ml of M.E.K.P. on 0.3 grams of regular cotton, and the three last tubes with 0.5ml M.E.K.P. on my double nitrated C6H7(NO2

3O5. First the 3 tubes with regular cotton were initiated one at a time in the same manner as above. All three preformed similarly. A loud band that left only the twisted ends of the foil intact. All three also slightly damaged the balsa wood disks, causing a small slit and several splinters pointing downwards. (A different disk was used for each test.)

Lastly, The foil packets with cellulose nitrate and M.E.K.P were initiated in the same manner. Based on my observations, these last tests definitely had something the others did not. No flame what so ever was observed and it was extremely sharp and loud sounding. All three tests resulted in the foil tubes being reduced to pieces no larger that coarse salt, including the end pieces. A well defined hole was punched in all tree of the wood disks about 5 inches long and 3 inches wide. The second of these tests actually split the wooden disk into 3 pieces and some splinters. I was wearing foam insert ear plugs during all these tests and my ears are still ringing loudly, several hours later. Especially my right one.

This was my first experience with HE detonations and I have to say it was exhilarating, but also terrifying. I have no doubt that those little foil packets, especially the last three, would have maimed me had they been near my person. These tests were done with the material very lightly confined, There was amply room inside the foil packets and no attempt was made to compress the material in any way. Even though they were loosely filled they were much louder that a suitable sized KClO4/Al flash charge and had a different, sharper sound to it. I believe that these would have the necessary brisance to initiate a secondary, even without being compressed.

See a couple posts back for information on the M.E.K.P. and cellulose nitrate synthesis I used for my tests.

[Edited on 13-3-2011 by Bot0nist]

crazywantabies - 23-3-2011 at 15:32

Thank you for the excellent details of MEK peroxide making from scratch. I have been making about "everything" from scratch for 26 years. I love ANGLES & arts. ....therefore, anyone know if this MEK peroxide hardens CASTIN' CRAFT* liquid plastic CLEAR CASTING RESIN?(*copywright CASTIN' CRAFT). I am also going to pray, if I may, for good ol Madscientist one or two times. THANKS AGAIN, Mad..

I speak in lieu of part time for appreciation for all things, slow bumper sticker for love on highways,

, and THE BOX, future consciousness "sin" detection unit for no illusions psychic war, not bloody war- 8 years ive been saying such.

Bot0nist - 23-3-2011 at 17:09

What?

I am sure gelatin can be made by mixing cellulose nitrate with as little acetone as possible to get it to gel up, then mixing said thick lacquer with desired proportion of M.E.K.P. I'm not sure that it could be made cast-able easily, though it can be soaked into many solids. A lot of people seem to prefer nitrate salts as a media.

[Edited on 24-3-2011 by Bot0nist]

grndpndr - 1-5-2011 at 14:47

Quote: Originally posted by Bot0nist

What?

I am sure gelatin can be made by mixing cellulose nitrate with as little acetone as possible to get it to gel up, then mixing said thick lacquer with desired proportion of M.E.K.P. I'm not sure that it could be made cast-able easily, though it can be soaked into many solids. A lot of people seem to prefer nitrate salts as a media.

[Edited on 24-3-2011 by Bot0nist]

I made a similar suggestion to the above(recieving a great deal of grief/ridicule in the process) but using commercial SP/DBSP in lieu of the cellulose nitrate mentioned above.Glad to hear someone tried it.

[Edited on 1-5-2011 by grndpndr]

TheMessenger - 16-5-2012 at 18:34

When you mix MEKP with TCAP 50:50, or even 30:70 you end up with a slushy... The TCAP never fully dissolves into the MEKP.

Is it possible that MEKP/TCAP is actually something different than MEKP + TCAP? Or is it just that when they are synthesized together the MEKP prevents the formation of TCAP crystals...

detonator - 1-9-2012 at 01:31

The MEKP toxicity is not small.

124563 - 25-6-2013 at 20:01

Quote: Originally posted by zeppelin69

The same as those for AP. At twelve percent peroxide, I would use about 2.2 times the volume of MEK so lets say you had 100ml MEK, I would use 220ml 12%H2O2, and of course the catalyst is personal preference, but I would use probably 15ml HCL.

if i screw this up srry first post but i agree with your findings it seems the key mix is equal parts of peroxide to mek if the peroxide is 35% so if you use 3% you want to use at least 10 times more peroxide

killswitch - 25-6-2013 at 20:16

Is MEKP miscible in nitroglycerin, or does it form layers?

Adas - 26-6-2013 at 05:52

Quote: Originally posted by killswitch

Is MEKP miscible in nitroglycerin, or does it form layers?

It should be miscible.

killswitch - 26-6-2013 at 06:14

Quote: Originally posted by Adas

Quote: Originally posted by killswitch

Is MEKP miscible in nitroglycerin, or does it form layers?

It should be miscible.

Goddammit.

Pyrotrons - 6-11-2013 at 03:25

Hi All,

The very first post of this thread gives a procedure for procuring MEKP. Since that thread, I have read numerous times of the following:

1). The addition of concentrated H2SO4 to the MEK/H2O2 solution gives substantial hissing/sputtering noises as it enters solution. I have also noticed that there is discoloration of the droplet when it makes contact. This wasn't mentioned in the original procedure, and it worries me.

2). Coprecipitation of MEKP with Acetone Peroxide yields a substantially better explosive, in terms of initiating effectiveness, while preserving the sensitivity and stability characteristics of MEKP.

3). Coprecipitating AP+MEKP removes the necessity to A). Dry and B). Deacidify, the product. I noticed that in the original procedure, that when the NaHCO3 solution (of unspecified concentration) is added, strong bubbling and boiling occurs within the primary explosive itself. I find this terrifying, and would love to omit that.

In light of these items, I have modified the original procedure to accommodate these changes. I am not a chemist, and I am not aware of all of the variables that can be present in such syntheses. Red-lining, burning, or soaking of the following procedure in MEKP are welcomed.

THIS IS AN UN-TESTED EXPERIMENTAL PROCEDURE
*******************************************

Coprecipitation of Methyl Ethyl Ketone Peroxide and Acetone Peroxide

CHEMICALS NEEDED:

-40mL 27.5% H2O2 solution
-12.5mL Methyl Ethyl Ketone, CH3COCH2CH3
-12.5mL Acetone
-5mL 98% sulfuric acid
-8mL distilled water

NOTE: It is critical that temperatures remain within recommended limits between the beginning of step 4 and the end of step 5. Only after the solution in Step 6 has spent 24 hours between -15C and 5C can the temperature be allowed to rise back to room temperature.

1) In a 100mL beaker, combine 12.5mL of MEK with 12.5mL of Acetone and stir for 30 seconds. In an ice bath, reduce the temperature of this solution to between -10 and 5 degrees Celsius; the lower end of this range is preferable.

2) Place 40mL of 27.5% H2O2 solution in a 100mL beaker. In an ice bath, reduce the temperature of this solution to between -10 and 5 degrees Celcius; the lower end is preferable.

3) Place 8mL of distilled water into a small beaker. Slowly add 5mL of 98% sulfuric acid to the beaker containing the 8mL of distilled water. The temperature of this solution is unimportant, however, better temperature control of the other solutions may be had by cooling this in an ice bath as well.

4) Wait for the temperature of all solutions to stabilize within the recommended temperature range, then pour the beaker of the MEK/Acetone solution into the beaker of the Hydrogen Peroxide solution. Stir for 30 seconds while maintaining the recommended temperature range.

5) Slowly, drop-by-drop, add 13mL (all) of the previously diluted sulfuric acid solution, taking care to keep temperatures within the recommended temperature range, into the beaker containing the MEK/Acetone. If the temperature rises above 5 degrees Celcius, stop adding the sulfuric acid solution immediately.

6) After all of the sulfuric acid has been added, place in a freezer for 24 hours. It is critical to maintain a temperature between -15 and 5 Degrees Celsius during the entirety of this time period. (What is the loss of yield if you only wait 8 hours? 12 hours?)

7) After 24 hours in the freezer, the solution can be allowed to warm back to room temperature.

8) LAYER DESCRIPTION - The original procedure used the words "thick" and "thin". This is confusing as this can refer to both viscosity and size (height) of the layer, so re-word that.

9) Extraction via syringe - definitely important. Decanting results in loss of yield, as the product sticks to the bottom. Don't ask how I figured that out.

10) YIELD was never mentioned in original procedure.

11) STORAGE - "Don't store in polyhydrocarbon plastics"- was the only specification for the MEKP primary??? Edit: I found one MSDS for commercial MEKP (resin hardener) that was distributed in polyethylene containers. LDPE, HDPE, UHMW...or doesn't matter?

12). Some indication of what quality can be expected - Drop test, decomposition temp, plate dent, etc.

END OF UN-TESTED EXPERIMENTAL PROCEDURE
*************************************

[Edited on 6-11-2013 by Pyrotrons]

underground - 6-11-2013 at 05:38

I have a stupid question, but i am going to ask

When you are going to mix a liquid with a solid material, the density is going to be the maximum of both materials or not ?

Pickardjr - 6-11-2013 at 06:34

mekp is used in the marine industry in fiberglass repair/building, Ive seen it catch on fire from a rag that was used to wipe it up.

woelen - 6-11-2013 at 06:49

Quote: Originally posted by underground

I have a stupid question, but i am going to ask

When you are going to mix a liquid with a solid material, the density is going to be the maximum of both materials or not ?

No, on average, the density will be somewhere between that of the two. If mixing is more than simply mechanical mixing, such as dissolving the solid in the liquid, then in general you cannot say very much about the density of the resulting liquid. In theory, it even could be that the density of the solution is larger than the density of any of the starting materials. Such a situation could occur if the liquid consists of large molecules with a lot of 'limbs' such that no compact arrangement in space is possible. If the solid consists of small molecules, then these small molecules might fill up gaps in space, which cannot be occupied by the large molecules and then the density of the solution is larger than the density of the solvent. If the solvent in this case is the one with the larger density (e.g. because it consists of heavy elements), then the resulting solution is more dense than any of the starting material.

underground - 6-11-2013 at 07:04

I was thinking of mixing some ETN with NM to achieve good density, but it looks melting and casting ETN is a one way road for max density...

What about if you are going to mix it with a liquid fuel with high density, like glucose

[Edited on 6-11-2013 by underground]

Pyrotrons - 6-11-2013 at 12:58

Respectfully (underground), this thread is about MEKP.

Pyrotrons - 8-11-2013 at 17:57

The synthesis directly above (Coprecipitation of Methyl Ethyl Ketone Peroxide and Acetone Peroxide) was performed. Notes are as follows, most important to least:

- After all constituents were added to the reaction beaker, and the beaker was placed into the freezer, the liquid in the center of the beaker (warmest point) slowly crept UPWARDS, exceeding 9 Deg. C until it was caught and corrected with stirring. This is unacceptable temperature rise and will be corrected in a new procedure. I will report the original procedure (above) to the mods, as I believe it to be unsafe.

- Swirling the reaction beaker to mix the contents, instead of stirring it with a physical rod, will be recommended in the new procedure.

- It was observed that after reacting for 12 hours, the MEKP/AP was floating on top as a nearly crystal clear layer of liquid, inside the 100mL beaker. Beneath the MEKP/AP surface layer in much larger quantity, was a cloudy white layer. Due to the optical qualities of the floating surface layer of MEKP/AP, I would assume that it is of high purity, and anhydrous. 10g of this material was slowly and carefully extracted from the top of the cloudy layer with an eyedropper, however, 4g of the crystal clear MEKP/AP remained, as it was nearly impossible to remove via the eyedropper without contaminating it with the cloudy layer underneath. The new procedure accommodates extraction better, by letting the reaction sit while cooling overnight in a minimum-size graduated cylinder, where the clear MEKP/AP sitting on top is much easier to extract in full, without contamination.

To summarize this: After performing the procedure detailed above, ANY method, other than direct extraction of the MEKP/AP from the top, seems to result in cloudy whitish (contaminated) MEKP/AP.

- As others have found, diluting the H2SO4 before addition to the reaction beaker fixed the unnerving hissing noises.

- Yield of above procedure: 14g (14mL), after only waiting 12 hours in the freezer, at -10 Deg. C. No solids were ever observed. The product was an absolutely crystal-clear liquid, similar in viscosity to corn syrup.

The new procedure in the works should result in better temperature control, easier extraction of the MEKP/AP solution, and a high purity product.

(edited for grammar)

[Edited on 9-11-2013 by Pyrotrons]

Pard - 21-12-2013 at 05:23

What actually is the projected yield for the synthesis on the first page? Is there a formula for projecting it based on the amount H202 or MEK perhaps?

franklyn - 13-9-2014 at 18:12

Axt has not been seen here since geocities closed down in 2009
http://www.sciencemadness.org/talk/member.php?action=viewpro...

http://www.sciencemadness.org/talk/viewthread.php?tid=20&...
The video from his post is still available
http://www.youtube.com/watch?v=vYpoQ3VrjVE

"A misconception of the structure of MEKP is prevalent in chemical reference literature , assigning the cyclic dimer as the structure for MEKP when it has been shown conclusively that the main components of the commonly produced industrial MEKP are monomer and dimer and that the cyclic dimer is not present." From => www.osha.gov/dts/sltc/methods/organic/org077/org077.html

For energetic purposes it must be noted that the monomer has the highest oxygen balance while the cyclic dimer has the lowest.

C4H10O4 , Monomer

__________________
MEKP Dimer.gif - 7kB

C8H18O6 , Linear Dimer

C8H16O4 , Cyclic Dimer

http://www.sciencemadness.org/talk/viewthread.php?tid=20&...
http://www.sciencemadness.org/talk/viewthread.php?tid=20&...
http://www.sciencemadness.org/talk/viewthread.php?tid=20&...

@ Rosco Bodine
Can you proffer an opinion on whether MEKP can serve to phlegmatize HMTD ?
In the same way you propose for solvation of solid organic peroxide TATP.

.

[Edited on 14-9-2014 by franklyn]

test MEKP

Laboratory of Liptakov - 14-12-2014 at 11:33

I just study MEKP a thread here: http: //www.sciencemadness.org/talk/viewthread.php? Tid = 20 & pag ... (from Axt)
Here I see a single clear or conclusive tests. (and youtube) Question: The container was always 60 g EM? It is not clearly explained. Thus for me. I use everything on auto compiler. Thank you for your reply .... :cool:

...LL

eng_lami - 22-3-2015 at 03:53

hello

please i need your help

i want to make a test to check the effective of MEKP before using it in industry

thnx

NitratedKittens - 13-4-2015 at 02:43

Do you know any other things you could make MEKP Dynamite out of

KesterDraconis - 15-6-2015 at 20:40

So I've synthesized some MEKP lately. I used the procedure outlined on the first page of this thread. However, I've found myself unable to get it to detonate reliably. While I did put some wrapped in aluminum foil over a candle flame and got a loud bang from it, I've not been able to detonate any of it with a fuse or even R-candy burned around it (when it is wrapped in foil). It just deflagarates quickly in a sudden flame, sometimes just slightly popping the foil cover, but with nothing near the bang that follows its detonation.

So basically, the question I've come to ask is if there is some trick to this, or better way to get it to detonate reliably? I like the fact that its relatively stable, and therefore not as likely to take my fingers off, however I also don't like the idea of using this as a primary only for my charge to not detonate (and then I have to find some way to safely dispose of it).

Pages: 1 2 3 4