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Author: Subject: Methyl Ethyl Ketone Peroxide
Rosco Bodine
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[*] posted on 24-1-2016 at 12:34


Quote: Originally posted by Rosco Bodine  
Quote:
Originally posted by Zinc
I have heard that MEKP and a solution of AP in MEKP do not need to be neutralized and that in fact residual acidity makes them more stable. Is that true? I have 65 grams of 50:50 MEKP/AP sitting in a measuring cylinder so I would like to know what is the safer thing to do before storage.


I have a half liter of the 50/50 separated straight from
synthesis , unwashed , no neutralization , put into storage
in a cool and dark location , and showing zero decomposition after several years . No change whatsoever is evident .


Recently I disposed of the original 50/50 MEKP/AP sample which had been stored for almost 13 years and the material showed no sign of decomposition whatever. What to make of others reported different observations about the stability and sensitivity I don't know, except to attribute differences to unknown impurities or unidentified byproducts. My original sample was still absolutely water clear and unchanged after more than a decade of storage underground.

The material was first described here
http://www.sciencemadness.org/talk/viewthread.php?tid=470&am...

A time capsule storage experiment :D

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[*] posted on 18-5-2016 at 11:10


Hello all these are my observations making MEKP/AP

This is the first time I have made explosives. I really wondered if what you people were saying was true and since it would only cost less that $30 i went for it.

I followed Mr Roscoes method.
I made 3 batches as to use all the chemicals.
First batch was not end product as described. It did have 2 layers but the bottom layer was hundreds of tiny bubbles that varied in size. I believe I made a mistake letting the peroxide/ MEK/Acetone get warmish and chems were not measured perfectly but by eye.
2nd batch I used my mums glass measuring cup to get accurate measurements I did not allow Peroxide/MEK/Acetone to rise in temp. The reaction did not start until the 4th acid addition 15 minutes later reaction was complete I believe as even though I left jar for 24 hours there was no increase in yield. The 2 layers were clearly visible this time but the top layer fairly clear and bottom layer was cloudy. Where I made a mistake was adding the acid whenever I felt like it not every 15 minutes.
3rd batch I was took extra care to follow procedure to the letter and to my amazement it has worked like clockwork.
2 layers formed top layer was cloudy and bottom layer crystal clear like water and what a yield. bottom layer was at least 80% of the jar.
Thank you all very much I am looking forward to impressing my brothers with some real detonations much cooler than the dull soda stream or chlorine booms they make.


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[*] posted on 23-5-2016 at 05:13


You made MEKP with grammar like that using the chemicals BY EYE? Are you insane? You must have some kind of death wish, or you are a kewl. If I were to bet, I'd go for the latter. You need to get off this forum.
I'm starting with energetics at the moment: I'm 14 as well. I'm starting with a simple perchlorate mix! Either change your attitude or get off the forum. This isn't a YouTube comments section: you will learn the hard way that stupid people get very bad press very quickly. I found that out the hard way.

[Edited on 23-5-2016 by glymes]
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[*] posted on 23-5-2016 at 06:26


Quote: Originally posted by ill behaviour  
Hello all these are my observations making MEKP/AP

This is the first time I have made explosives. I really wondered if what you people were saying was true and since it would only cost less that $30 i went for it.

I followed Mr Roscoes method.
I made 3 batches as to use all the chemicals.
First batch was not end product as described. It did have 2 layers but the bottom layer was hundreds of tiny bubbles that varied in size. I believe I made a mistake letting the peroxide/ MEK/Acetone get warmish and chems were not measured perfectly but by eye.
2nd batch I used my mums glass measuring cup to get accurate measurements I did not allow Peroxide/MEK/Acetone to rise in temp. The reaction did not start until the 4th acid addition 15 minutes later reaction was complete I believe as even though I left jar for 24 hours there was no increase in yield. The 2 layers were clearly visible this time but the top layer fairly clear and bottom layer was cloudy. Where I made a mistake was adding the acid whenever I felt like it not every 15 minutes.
3rd batch I was took extra care to follow procedure to the letter and to my amazement it has worked like clockwork.
2 layers formed top layer was cloudy and bottom layer crystal clear like water and what a yield. bottom layer was at least 80% of the jar.
Thank you all very much I am looking forward to impressing my brothers with some real detonations much cooler than the dull soda stream or chlorine booms they make.



Beware of the jar...if it is glass...with a sensitive compound like MEKP or CTAP, it is like a grenade generating lethal shrapnels in case it detonates.

Note that I had a police lab report of a wet CTAP sample exploding into the police lab fridge...
It was from the investigation of a bottle found in a lake in Brussels, the environmental bureau (IBGE-BIM) had found ducks and fishes dead and a sample was sent to the lab I was working for to evaluate the potential cause...
We did a lot of conventionnal tests but the client had noticed that aceton bottle looked alike the bottle found in the bottom of the lake.
The bottle had fumed when he opened it (I told him it was not very wise to do so if he did'nt know what's in it)
I said that aceton is not toxic enought to kill ducks and fishes especially in a lake that would dilute the aceton a lot.
We found that pH was quite acidic and that it contained a lot of chloride.
I then hypothesised that aceton + H2O2 + HCl may have formed CTAP and that a kewl bomber was testing it/blasting it into the lake...the client was sceptical...until next day when he explained me that the police lab fridge had exploded during the night!

CONCLUSION:
ORGANIC PEROXYDES ARE NOT FOR FUN...they look stable and that you can handle it...but it can explode without reason even when wet, cold and undisturbed!




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[*] posted on 23-5-2016 at 06:31


Quote: Originally posted by glymes  
You made MEKP with grammar like that using the chemicals BY EYE? Are you insane? You must have some kind of death wish, or you are a kewl. If I were to bet, I'd go for the latter. You need to get off this forum.
I'm starting with energetics at the moment: I'm 14 as well. I'm starting with a simple perchlorate mix! Either change your attitude or get off the forum. This isn't a YouTube comments section: you will learn the hard way that stupid people get very bad press very quickly. I found that out the hard way.

[Edited on 23-5-2016 by glymes]

You are not wel placed to give advices to others...better keep such comments for yourself.

It is not real organic chemistry that needs much control...it is like cooking so BY EYE is OK, but you need to keep the temperature low and avoid to do it in large quantities....what is tempting because of the easyness of making... Without cooling you may gas yourself by a big lachrymatory smog of boiling chloroaceton, Cl2 and aceton what is by the way very inflamable and explosive (risk of FAE).
So you can easily make, if you don't take care 100g or more of it what is equivalent to 80g TNT --> one or two dynamite sticks....
Thus enough to blow your body and kitchen/house appart.
The substance is also very unpredictable and may detonate on its own (even when wet, in the cold and undisturbed) as proven by my true experienced story in last post!

[Edited on 23-5-2016 by PHILOU Zrealone]




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[*] posted on 23-5-2016 at 06:54


I know that I'm not in the position to do safety talks... But when someone makes organic peroxides FOR THEIR OWN FAMILY I'm obviously going to forcefully make my point.
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[*] posted on 23-5-2016 at 19:54


Very sorry if I offended any of you good people.
I appreciate the concern for me and my families safety.
I conducted my experiment outside and away from the house.
I live semi rural so my danger to others was a minimum.
I disposed of the first 2 batches by dumping them in a 1 foot hole in the ground.
The good stuff was soaked into toilet paper and exploded safely and without incident except to say it was loudest thing I have ever heard and my brothers said it shook the windows and set my mums car alarm off. They asked was it was I said match heads.
They didn't believe me but I decided not to tell them because if
they had a accident I would feel I was to blame. Later today my plan is to put a charge into a rabbit burrow BTW this is a huge complex of connected tunnels with multiple entry holes/exit holes and around 30 foot by 30 foot area.

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[*] posted on 24-5-2016 at 07:05


Ok. Fair enough.
I'm going to try 7:3 NH4ClO4:MEKP to see whether the MEKP has enough heat of formation for enough time to elevate the perchlorate to its detonation temperature.
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[*] posted on 26-5-2016 at 01:51


Quote: Originally posted by glymes  
Ok. Fair enough.
I'm going to try 7:3 NH4ClO4:MEKP to see whether the MEKP has enough heat of formation for enough time to elevate the perchlorate to its detonation temperature.

As such "Heat of formation" has little interest to increase the temperature of NH4ClO4 to detonation...The only interesting parameter here is: has MEKP enough kick (detonation strenght) to initiate NH4ClO4 to detonate.

Heat of formation (from the elements) is only interesting if it is positive (endothermic) because then, when the molecule is burned (exploded/detonated) the heat of formation of its decomposition products (from the elements) what is negative (exothermic) adds to the heat of formation of the initial molecule.

This comes from Hess law of thermodynamic:
No matter the way you go from the réactants to the products, the energy of reaction is simply the difference between the energy of the products - the energy of the reactants.
So nothing is against a passing by the elements as an intermediary point wich is a good reference since H°f (enthalpy standart of formation of compounds from the elements) is used for the purpose to get a reference scale/point of energy for energies of reactions....

I already gave you a warning about "playing" with organic peroxydes...may explode with no reason even when wet and in the cold undisturbed...
Friction sensitivity with mineral cristals like NH4ClO4 must be avoided and contact with metals like Fe, Cu, ... also.

[Edited on 26-5-2016 by PHILOU Zrealone]




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[*] posted on 26-5-2016 at 02:44
advice


Glymes, if you have NH4ClO4, you can prepare TACP and copper hexamine perchlorate for pretty power detonator.
It is much more safety, than madness mix with organic peroxide. No-compatability with metals is usually problem for normal use on fields conditions. Next words, if you have AP, you can prepare almost anything from family of energetic materials. KClO4, NaClO4, HClO4 and more. However estimate, that my advice are almost unneccessary.....LL....:cool:
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[*] posted on 28-5-2016 at 11:24


Upon heating, would NH4ClO4 decompose into NH3 and HClO4, or otherwise unspecified?
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[*] posted on 29-5-2016 at 06:03


Quote: Originally posted by glymes  
Upon heating, would NH4ClO4 decompose into NH3 and HClO4, or otherwise unspecified?

No!
Into N2, HCl, Cl2, H2O and O2.




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[*] posted on 26-8-2016 at 14:57


Quote: Originally posted by madscientist  
If the temperature of the reaction is kept low, I suppose HCl could be used.

As for adding the H<sub>2</sub>SO<sub>4</sub>, I suggest diluting it prior to adding it to the solution prepared by mixing MEK with hydrogen peroxide.

I have only ever used HCl for making MEKP and it worked just the same. More must be used compared to H2SO4 of course, but it seemed that the temperature never really went up much.
I did have a question: Do you know if freezing MEKP would reduce the sensitivity? Thanks for a reply.




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[*] posted on 27-8-2016 at 04:57


"More must be used compared to H2SO4 of course"
--> WRONG!
HCl is a more than 1000 times a stronger acid than H2SO4...so despite it can only reach 35% by weight (HCl gas dissolution into water) it will always protonate much than H2SO4...except when very dilluted where the two acidities tends to nearly equal.




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[*] posted on 27-8-2016 at 07:49


The first proton of H2SO4 is a stronger acid than HCl (see Ref. 1):

HOSO2O---H, pKa= -10

Cl---H, pKa= -7

Compared to HNO3:

O2NO---H, pKa= -1.5

Reference:

[1] Marye Anne Fox, & James K. Whitesell. Organic Chemistry, 3rd edition, Jones and Bartlett Publishers ,2004, p. 295

[Edited on 27-8-2016 by Dany]
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[*] posted on 27-8-2016 at 08:26


Quote: Originally posted by Camroc37  
Quote: Originally posted by madscientist  
If the temperature of the reaction is kept low, I suppose HCl could be used.

As for adding the H<sub>2</sub>SO<sub>4</sub>, I suggest diluting it prior to adding it to the solution prepared by mixing MEK with hydrogen peroxide.

I have only ever used HCl for making MEKP and it worked just the same. More must be used compared to H2SO4 of course, but it seemed that the temperature never really went up much.
I did have a question: Do you know if freezing MEKP would reduce the sensitivity? Thanks for a reply.


Freezing MEKP would be a bad idea, IDK its melting point but usually crystals are more impact sensitive than liquid explosives.
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[*] posted on 27-8-2016 at 10:09


when I made a few Ml of it I washed in distilled salted water then absorbed into clean dry wood dust, then allowed to sit for several weeks to test stability, then it was fired on the spot so it needn't been handled.

It behaved well, but the synth was very care fully don with good clean chemicals and all procedures where care fully followed. Even then I did not trust it! Peroxide in of its self under goes decomp in the fridge with no light exposure!!!!!

Put simply you are playing a serious game of chance messing with them, make a few Ml to experience but then stay far far away for your own sake and the sake of relatives that may end up IDing your body

It was entertaining to make and fire but no where enough to endure the risks!
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[*] posted on 27-8-2016 at 12:03


Quote: Originally posted by Dany  
The first proton of H2SO4 is a stronger acid than HCl (see Ref. 1):

HOSO2O---H, pKa= -10

Cl---H, pKa= -7

Compared to HNO3:

O2NO---H, pKa= -1.5

Reference:

[1] Marye Anne Fox, & James K. Whitesell. Organic Chemistry, 3rd edition, Jones and Bartlett Publishers ,2004, p. 295

[Edited on 27-8-2016 by Dany]

pKa1 of H2SO4 is usually refered into pKa tables into the range -3 (at least into water) while that of HCl is 6.3 in the same context...
Maybe since the reference is for Organic chemistry the pKa is into another solvent than H2O...often DMSO is used into pKa tables also.




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[*] posted on 29-8-2016 at 02:09


Quote: Originally posted by PHILOU Zrealone  
Quote: Originally posted by Dany  
The first proton of H2SO4 is a stronger acid than HCl (see Ref. 1):

HOSO2O---H, pKa= -10

Cl---H, pKa= -7

Compared to HNO3:

O2NO---H, pKa= -1.5

Reference:

[1] Marye Anne Fox, & James K. Whitesell. Organic Chemistry, 3rd edition, Jones and Bartlett Publishers ,2004, p. 295

[Edited on 27-8-2016 by Dany]

pKa1 of H2SO4 is usually refered into pKa tables into the range -3 (at least into water) while that of HCl is 6.3 in the same context...
Maybe since the reference is for Organic chemistry the pKa is into another solvent than H2O...often DMSO is used into pKa tables also.

Edit: Frogot the "-" sign for HCl that is -6.3 of pKa




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[*] posted on 16-1-2019 at 16:02


I read somewhere in this thread that MEKP is not compatible with metals. Do metallic compounds catalyze decomposition of organic peroxides (the way some metallic compounds do with hydrogen peroxide) or is MEKP simply corrosive to metals due to traces of acid in it from catalyzing the reaction. Would MEKP be okay in metal (e.g. brass) if it where neutralized first?

Also, 497 claimed to have had success sensitizing smokeless powder by soaking it in MEKP : https://www.sciencemadness.org/whisper/viewthread.php?tid=20... Would anyone happen to know if Methyl Ethyl Ketone Peroxide degrades smokeless powder/NC/NG? would it become unstable or lose its power if left mixed for an hour? what about a day or a week? I know this is an old thread and a beginner question, but I couldn't find anything (on SM or otherwise) about the compatibility of organic peroxides with nitrate esters.




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[*] posted on 17-1-2019 at 00:04


MEKP is commonly used as a hardener for epoxy resins, I think going through some material safety data sheets (MSDS) will provide most of the answers you are looking for.
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[*] posted on 24-1-2019 at 15:08


Thanks. I looked at some, and found out some more information. According to www.illawarrasurf.com/msds/mekp.pdf the peroxide hardener is incompatible with "strong acids, strong alkalis, reducing agents"

For Crompton Hi Point 90, (www.tapplastics.com/uploads/pdf/MSDS_TAP_MEKPC.pdf) it says "avoid contamination with any foreign substance" and "Incompatible materials Strong acids, Reducing agents, accelerators. Promoters. Other reactive chemicals."

Easy composites MSDS (https://www.easycomposites.co.uk/downloads/MSDS/EC-MSDS-MEKP...) "Do not mix with accelerators, reducing agents, strong alkalis, andheavy metal compounds..." The product must never be stored together with accelerators such as driers, heavy metal compounds etc. Avoid contact with rust..." Use clean equipment an tools of inert material such as stainless steel, polyethylene, polypropylene, glass."

"Incompatible materials such as acids, strong bases, tert amines, friedel-crafts catalysts, heavy metals, cobalt accelerators or other peroxice accelerators or promoters, rust, brass, galvanized steel, acetone, reducing or oxidizing agents, grinding dust, and dirt."

Arkema: https://www.arkema.com/export/shared/.content/media/download... "keep away from incompatible materials such as: Strong oxidizing agents, powerful reducers, acids, bases, amines, transition metal salts, sulfur compounds, rust, ash, dusts (risk of self-accelerating exothermic decomposition)..."

Norox MEKP-925 www.advanced-plastics.com/Docs/MSDS/M29_141218%20SDS.pdf "keep/store away from clothing,/strong acids, bases, heavy metal salts and other reducing substances/combustible materials..." "keep away from strong acids, bases, heavy metals, salts, reduing agents and accelerators. Contaminants (e.g. rust, dust, ash). Combustible materials, Risk of decomposition. Dimethylaniline, Cobalt Napthenate and other promoters, accelerators, reducing agents, or any hot material."

http://www.tuffstuff.co.uk/application/files/7914/4957/5131/... "keep away from reducing agents, e.g. amines, acids, alkali, heavy metal compounds (e.g. accelerators, dryers, metal soaps)." "Violent reactions may be expected with acid, alkali, heavy metals and reducing agents. Avoid contact with rust."

"Use only stainless steel 31.6. PVC, Polythene or glass-lined equipment"

Regarding smokeless powder, I could only find http://ceemjournal.org/upload/pdf/ceem-15-055.pdf "A case of severe corrosive gastritis and liver necrosis caused by ingestion of methyl ethyl ketone peroxide" by Jung Oh Chang et. al This is mainly about an emergency medical case in which someone accidentally drank MEKP resin hardener (stored in an unlabled water bottle) and died. However, it does say that "It is used as a general industrial solvent in the manufacturing of nitrocellulose coating, vinyl film, and smokeless powder."

However, I get this feeling that when talking about "a general industrial solvent" they might be confusing MEKP with un peroxided methyl ethyl ketone.

Some of the material safety data sheets did not mention metals, or only mentioned their compounds. But since some cautioned against transition metals in general (as opposed to just their salts), and one mentioned brass specifically, I think the safest assumption (to the extent that making and storing organic peroxide compounds can be called safe) would be to consider MEKP incompatible with brass.

Whether it is compatible with smokeless powder, however, remains unclear to me.

[Edited on 25-1-2019 by C6(NO2)5CH2CH(CH3)N(NO2)2]




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[*] posted on 25-1-2019 at 05:44


My opinion is, Leave the think for mixing MEKP + nitrocompounds. Exist a lot better compounds for examination, for beginners.....:cool:



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