Sciencemadness Discussion Board - Isopropyl peroxide ?

Isopropyl peroxide ?

CROpyrO - 21-7-2003 at 07:22

ok . i wanted to make AP but i messed something up. i had 100 ml 6% hydrogen peroxide , 25 ml hydrochloric acid and now the problem- instead of acetone i mixed 75 ml of isopropyl alcohol (CH3CHOHCH3) and for 2 days i find a oily liquid

(it looks equal to MEKP). i did that last year , and now i am going to make it again and test its sensetivity and power . i think that it is has higher velocity then AP . can you please tell me some information about this explosive peroxide and is it posible to make a "dynamite" explosive out of it. if yes - how ???

???

p.s. sorry if i had some mistakes in my english becose im from croatia.

blip - 21-7-2003 at 21:55

I did a search on <a href="http://www.ixquick.com/" target="_blank">ixquick</a> and didn't find anything really. But then I had an idea that possibly some H2O2 could oxidize the isopropanol to acetone:
CH3CHOHCH3 + H2O2 unknown conditions > CH3COCH3 + 2H2O

Be careful!

CROpyrO - 22-7-2003 at 10:19

thanks . will this explosive have the same power when mixed with sodium chlorate or potassium nitrate ?

Mumbles - 22-7-2003 at 10:25

Could it be possible for it to have formed some AP, then dissolved in excess Isopropyl alcohol? I would think that the water would have flushed it out though. According to the msds it does in fact form a peroxide though. I can't really find anymore information about the compound though.

If the peroxide is infact a liquid I suppose you could make "dynamite" the same way you would for any other liquid explosive.

CROpyrO - 22-7-2003 at 10:44

tomorrow i will do some experiments on it . im very interested ... maybe it is more stable then other organic peroxides . i don't know exactly how powerful it is , but i think it has a better velocity then AP . if somebody has some information or ideas about this new explosive peroxide , please post . _______thanks

blip - 22-7-2003 at 12:40

I don't recommend mixing anything with it until you know what it really is. I was just speculating; and organic peroxides cannot be regarded as stable! Safety should be your first priority! Mumbles, where can I find that MSDS?

Mumbles - 22-7-2003 at 16:04

http://www.soest.hawaii.edu/krubin/MSDS/ISOPROPANOL.html

In the Handling and Storage section it states "Small quantities of peroxides can form on prolonged storage. Exposure to light and/or air significantly increases the rate of peroxide formation. If evaporated to a residue, the mixture of peroxides and isopropanol may explode when exposed to heat or shock."

Also, Isopropyl alcohol is listed in several lists of peroxide forming substances.
http://www.missouri.edu/~muehs/Peroxide.htm
http://www.people.memphis.edu/~ehas/perox.htm
http://www.ehs.cornell.edu/lrs/chp/12.peroxides.htm
There are three prime examples. Note in some it is refered to as 2-propanol.

Experimenting without much knowledge of the product can indeed be very harmful. There is very little information that I can find of this substance. Without knowing how sensitive, or stable the product is I wouldn't get within 100 feet of it. Thats just me though. If you do decide to carry out this experiment please use the utmost safety and care. Please report your findings as well.

CROpyrO - 24-7-2003 at 07:35

now the peroxide is started to form , it needs a little longer to form than AP . tomorrow it should be completly formed and then i will to start to test small amounts of it . meanwhile can you tell me information or a site about picric acid . thanks

CROpyrO - 26-7-2003 at 01:14

the peroxide is formed . on 1. picture you can see what it did to a wood stick( i dipped it just that it touched the peroxide ! ) , 2. picture shows you the peroxide ,and the 3. shows you my ammonium nitrate that i'm going to mix it with. i'm still testing the sensetivity.

Image68.bmp - 297kB

CROpyrO - 26-7-2003 at 01:17

picture of the peroxide

Image77.bmp - 297kB

CROpyrO - 26-7-2003 at 01:21

and the 3. picture - ammonium nitrate crystals .

Image83.bmp - 297kB

trinitrotoluene - 26-7-2003 at 12:16

I have heard about the dangers of isopropyl peroxide. I had heard from account that you never distill to dryness. I have heard of some highschool chemistry classes who distilled isopropyl alcohol to dryness and the apparatus exploded due to the formation of peroxides.

two explosives - one procedure ?

shadeT - 8-8-2003 at 06:54

guys , i need your help . here's what i did , i was meaning to make some isopropyl peroxide , i found a solvient . the stuff in it are MEK,isopropyl alcohol and water . so i used it with the standard procedure. i let it stay in the fridge , but for 36 there was still nothing so i lowered the temp to -13 , i let it so for 2 hours , now i have a oily layer on top ( MEKP ? ) and some fine chrystals on the bottom . is it posible that i got MEKP and it didn't freeze but the isopropyl peroxide ( ? ) on the bottom has frozzen ??? now i let it on -3 so that the IP melts in a oily liquid again . it's good that the IP stays on the bottom and the MEKP is on the top so there isn't a problem like mixing them together ( could be dangeraus becose we don't know much about the IP sensetivity ) thanks for any information and help _______!!!

shadeT - 8-8-2003 at 08:37

the isopropyl peroxide in my mixture has molten by now , but it is all over in the liquid . ill try to freeze it again and than ill get the mekp out and than ill let IP to melt and let it slowly come to the bottom.then ill get the liquid out and there will be only IP left . there is more IP than MEKP , maybe becose the solvient contained more isopropyl alcohol . cool thing , when you make IP you get MEKP too , same thing when you make MEKP , you get IP too . the only problem for someone will be finding that kind of solvient . maybe mixing MEK with isopropyl alcohol ... ?? post info :cool:

a123x - 8-8-2003 at 18:20

Have you done any sensitivity tests with the IP to see how sensitive it is compared with MEKP and AP? It sounds like IP might be pretty cool if it isn't ridiculously sensitive(as in like untransportable, more sensitive than AP). Also does the IP happen to have much smell to it?

shadeT - 8-8-2003 at 22:52

no i didn't do sensetivity tests , but i'm meaning today or tommorow , i have them both in my fridge so i just have to separate them . well AP would be probably most sensitive , than IP and than MEKP , but ill do some tests . for now i now that IP is little more flame sensitive as MEKP ... yes IP also smells bad but i think that not the same , well only once i had clear IP so i don't very well remember the smell , i don't belive that IP is toxic like MEKP , i got one drop on the skin and nothing happened , i just washed it fast . well you could make your experimental yields , few ml , to do some tests , i made a little more but i'l try detonation tests too ( IP is fuse sensitive ) . ill post all new info that i find about them . post your info too

a123x - 9-8-2003 at 23:11

I just finished adding catalyst to an IP synth.

-23ml of H2O2, boiled down from 260ml of 3%
30ml of 91% isopropyl alcohol
8ml of 93% H2SO4

Temperature never exceeded 10C on the acid addition. Temperature increases was much less than with AP or MEKP, also no hissing was observed during acid addition the way it is with AP or MEKP using H2SO4. Unlike my AP and MEKP synths nothing has formed by the time the acid all has been added. Since concentration doesn't seem to be too big a factor with IP(original poster got IP with 6%) I assume that it just takes a while to form or maybe requires temperatures below 0C as shadeT observed. It's in my freezer now.

shadeT - 10-8-2003 at 01:49

yes , IP needs much more time to form , 4-7 days . i heard that light speeds up the reaction , so ill try to put some lamp in my fridge . my mixture is also still in the fridge , but the IP didn't form ... ill wait few more days . IP apears as oily bubbles on the bottom as i said , i have some tiny bubbles starting to form , maybe 2 more days now . i hope that the results will be good . ill post info about yield and sensitivity ... (post your info)

a123x - 10-8-2003 at 10:13

After 12 hours nothing as formed, I thought perhaps using sulfuric acid would allow the reaction to procede more rapidly. I'll allow it to sit in the freezer for several days. What were the specifics of your synth shadeT? It would be helpful to know this in trying to get similar results.

shadeT - 10-8-2003 at 11:02

i used 100 ml of h2o2 ( 12% ) , 15 ml sulfuric acid and 80 ml of the isopropyl alcohol+mek mix. i never made IP with just isopropyl alcohol ... so i dont know much about that reaction ... i will try to make it with just isop. alc. as you did . tommorow ill buy 12% h2o2 becose i don't have more , and ill do it with 70% IA , ... about the reaction . you could speed it up by leting it opened in the fridge , it will stink but speed up ( this night ill let it stay opened with a mini lamp ), and as i said light will speed up too . just let your first mixture in the fridge for a few more days , that's a little shity by this explosive , it needs more time than other peroxides , but its worth it . ill experiment tommorow with your synth . ill post information

Haggis - 13-8-2003 at 13:13

Also, I have attempted to prepare this chemical. I used:
190ml of H202 around 9%
20ml HCl-31%
75ml 2-propanol-91%
The reactants were cooled in -5 celcius temperature for an hour to knock the temperature down. The flask was stirred vigorously before placing back down to set. As of 24 hours, no results have formed. I have not had any light present, so that could affect it.
When/if I get any results, I shall post them.

shadeT - 20-8-2003 at 01:54

did somebody had succes making IP ??? i will make some pics of IP and post.

Haggis - 20-8-2003 at 11:29

After the week or so has gone by, no liquid is seen on the bottom of the flask. However, there is a foggy white mist that is heavier than the solution. when the flask is tipped on the side, the fog eventually settles down on the bottom. when the flask is 'rolled' around, tiny bubbles are emitted from the bottom, very slowly rising up. I was thinking that these small bubbles could be HCl coming out of solution, but I have no evidence to back it up, as they are very small and in small quantity.

Madog - 20-8-2003 at 13:34

im thinking that white filmy shit on the bottom there could be a very small amount of acetone peroxide. made from the IPrOH being oxidised to acetone by H2O2(very small amount that is) then tunring to AP. my first atempt at AP was useing 28% HCl with the same ratios used for 75% H2SO4(so it was seveely under catylized) and it had a white film on the bottom like you describe.

just my theory on it.

shadeT - 20-8-2003 at 23:42

well , i have to detonate IP or just throw it away , becose it is realy sensitive and all comounds ( tried to make it more stable ) have the same sensetivity . so a better thing would be making just MEKP . and here a interesting thing , i got also such a foggy thing but only when i used 6% conc h2o2 , with 9% and 12% i didn't see the foogy thing but i just had MEKP on the top ( i'm using the one procedure - two materials method ) ... this is realy strange !

failed IP

The Ed - 1-9-2003 at 14:00

I attempted making some isopropyl peroxide the other day but the results were... odd. I think the fact that I used sodium perborate as the peroxide source might have had something to do with it.

The isopropanol I was using was already 30% water so i just dissolved as much of the oxy-clean ripoff(mixture of sodium carbonate and sodium perborate) in it as i could. I then dripped in enough sulfuric acid to neutralize the sodium carbonate/sodium borate and dripped in a little more to catalyze the reaction. There was indeed an oily layer that formed on the bottom but it was completely inert. It wouldn't burn at all nevermind detonate. I tried using a fuse, failed. I tried a hammer, failed. The top layer of leftover alcohol burned with a slight greenish flame indicating boron compounds dissolved in it.

I'd try this experiment again if I ever got ahold of some 30% H2O2.

shadeT - 2-9-2003 at 02:29

im sorry for you . it seems that you realy have problems with making IP ... i tried with 6% h2o2 and 9% - nothing , than with 12 % - worked fine . ill try to make a nice photo of it and than post. i still have all 20 ml of IP in my basement. it seems that it is storage safe ...

a123x - 21-9-2003 at 13:58

Quote:

Originally posted by Haggis
After the week or so has gone by, no liquid is seen on the bottom of the flask. However, there is a foggy white mist that is heavier than the solution. when the flask is tipped on the side, the fog eventually settles down on the bottom. when the flask is 'rolled' around, tiny bubbles are emitted from the bottom, very slowly rising up. I was thinking that these small bubbles could be HCl coming out of solution, but I have no evidence to back it up, as they are very small and in small quantity.

I too got that white mist when trying to make IP. I suspect that the use of isopropyl alcohol mixed with MEK by shade is why he is having success. I don't understand enough to know what reactions could be taking place but an MSDS for MEK that I was just looking at listed 2-propanol as an incompatibility so it just makes me think that they might react wierdly together to form a peroxide.

flashpoint - 16-12-2003 at 16:01

i may just have to give this a shot...I have some 30% H202 as well as some 30% HCl. Time to figure out a good way to do this...

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No kidding. Now ain't that news shocking enough to waste space here...

[Edited on 17-12-2003 by vulture]

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Sorry

[Edited on 18-12-2003 by flashpoint]

narkar - 18-12-2003 at 00:48

hello. i mixed 8ml h2so4 94% or 96% ,1ml glycerin 99% and 3ml h2o2 50%. reaktion time was 1-4sec. (runaway reaction) but if i poured it into water i saw some white hairs formed

Mumbles - 18-12-2003 at 14:00

Ok, what does that have to do with anything? Expecially related to IPP. It contributed nothing to this conversation at all. Perhaps it (and possibly you) would be best suited elsewhere.

chemoleo - 18-12-2003 at 16:35

true, it's got nothing to do with this thread.
But, hang on for a sec, he used glycerin, H2O2 and H2SO4. Why would you get chrystals there?

Mumbles - 18-12-2003 at 16:56

ummmmm, glycerol sulfate maybe? The sulfuric acid would act as its own catalyst in the reaction I'd image, if thats indeed what happened. Perhaps they formed some sort of condensation product.

What really intrigues me is the "runaway reaction". I have a good portion of money that says it was the Hydrogen Peroxide decomposing. Glycerine is listed as an incompatable with H2O2. Perhaps it was this decomposing. If not, the strongly acid environment surely did. Maybe the crystals were some sort of intermediary in the decomposition of glycerol with sulfuric acid, or an intermediary that reacted with sulfuric acid. I really have no clue, but I think we should maybe discuss this elsewhere so we don't polute the thread anymore.

KABOOOM(pyrojustforfun) - 19-12-2003 at 21:11

the reason glycerine is listed as an incompatable with hydrogen peroxide is that alcohols form quite powerful explosive mixs with it the glycerine mix has especially been known/studied. not just H2O2 mixs with alchols are serious hazard but almost with any fuel
the white hairs should be a polymer. maybe that of acroleine or acrylic acid I'm not sure because H2O2 additionally reacts with the vinyl group ...

unionised - 20-12-2003 at 04:22

Just to add to the complexity of the question, aldehydes form peroxides too.

chemoleo - 20-12-2003 at 18:01

kaboom, that's what came to my mind too. Heating glycerin to very high temperatures produces carcinogenic acrolein, which is also a product when animal fats are dropping on your lovely barbeque coal. That's why burnt meat is unhealthy by the way.
Anyway, I was thinking that maybe the H2SO4 creates acrolein. This could potentially react with the double bond, or, as you say, form polymers, that react then.
Check your U2U pls.

unionised - 21-12-2003 at 05:54

I haven't got any Na2SO4 kicking about so I can't test this, but I know that strong aqueous solutions of salts don't always mix with alcohols. MgSO4 solns don't mix with IPA, (NH4) SO4(aq) doesn't mix with ethanol. Can anyone check on whether the "oily layer" at the bottom of the reaction mixture in the first post in this thread might just be sodium sulphate solution?
I suspect that any organic peroxide product would have ended up in the organic phase (ie the IPA). It may well have beeen in too dilute a solution to make any difference to the flammabillity of the IPA.

MEK as catalyst in alcohol peroxidation?

Polverone - 16-4-2004 at 17:53

From a datasheet on methyl ethyl ketone, appearing in this month's Journal of Chemical Education: "Secondary alcohols containing even traces of methyl ethyl ketone are readily peroxidized and therefore explosively unstable."

I wonder if this has any bearing on shadeT's claim to be able to make isopropyl peroxide, but only when using a MEK/isopropanol mixture.

PainKilla - 30-5-2004 at 09:17

Well, being lazy as usual here is my mostly copied post from APC...

Well I am now conducting research on 2-Propanol Peroxide (Isopropyl Alcohol Peroxide). The procedure I followed was sort of random, but loosely based on the one at MadScience. I have one chilling at room temp, and one chilling in the freezer. I will allow them to form for 5 days after which I will try igniting the mixture formed and see what happens (if nothing else happens) Anyone have insight on possible formations, sensitivity, etc... This was the procedure:

100ml of 70% IPrOH was added to a flask, not chilled but at room temp, (18 degrees or something like that) to that was added 30ish (most likely 35) ml of 20% H2O2 was added to the other flask. The H2O2 was very slightly chilled and because of this the temperature dropped slightly, with no signs of increasing. To this mixture was added 35 ml of 23% HCl acid at room temperature. The temperature rose due to the warmth of the HCl, no other heat change was recorded. Accidentally spilling the mixture in a small flask (around 30ml was spilled) the mix felt oily and peroxidised my finger, and took off some stains of an old key that I had. One mix was placed in fridge and at room temp.

A very useful page was found on organic peroxides. It is VERY useful, and shows some very interesting details on peroxidation of organic compounds.

http://ehs.ucdavis.edu/ftpd/sftynet/sn_23.pdf

I will further provide details on the IP reaction, unless someone tells me its super sensitive.

This is continuation of the experiment...

SUCESSS IS IMMINENT!!!! ... Here is a more scientific report....:

Day 1 (24 Hours since start of synth) Refrigerated Flask: The flask has remained stationary at the coldest freezer temperature, which is probably around -5C. Small crystals are precipating out; there is an estimated .5g so far. It is increasing certainly however because when checked it in the morning the amount of crystals doubled by the second time I checked it. I will now definetly let the reaction continue, the crystals look like almost totally dissolved salt, but they are white.

Day 1 (24 Hours since start of synth) Room Temperature Flask: This I spilled AGAIN in the morning, but crystals are forming there. There is probably .2g-.3g in a 50ml of liquid, I think light accelerates the reaction greatly and I would recommend not placing it in the freezer but rather keeping in indirect light. This reaction seems to be proceeding rather nicely. The crystals are almost exactly the same as the ones in the flask.

EDIT: Forgot to mention that the crystals are at the bottom of the beaker resting all together and not floating around. The beakers were perfectly clean, so it could not be anything not part of the original reaction.
------------------------
Well those are the current observations, anyone have possible ideas on what could have formed? I will start testing soon, probably tomorrow for the small beaker since there is not a lot in there, I don't want a lot not knowing the sensitivity. Someone should try this synthesis too, using the method I posted, the HCl is 23% and H2O2 was around 20-25%. There was no heat change for me so you should have no fear of a runaway. Good Luck, I shall report more soon!

I didn't get a chance to do day 2 since I went to the city. Meanwhile, Mumbles mentioned how the IP could be AP due to the peroxidation of 2-propanol. I was also thinking on this topic in school but came to no definite conclusions. This is real post now...

Day 2-3 (48-72 hours) Room Temp Flask: I didn't feel like having this sit in my room so instead, I tried to filter and wash the crystals. On a coffee filter, I dumped the insanely small crystals and watched all the water drip off. The crystals were still there. I added water slowly and slowly the crystals began to disappear, but not into the solution in the bottom, there was no visibility at all of any signs of crystals. I came to the conclusion that the crystals were possibly water-soluble. I threw stuff at the coffee filter and lit it just incase the crystals were still there, but nothing happened, so the crystals definitely weren't there. I dumped out the rest of the stuff because I had to go.

Day 4 (96 hours) Freezed Flask: Not much change here, except that there are more small crystals and some floating around in the solution. The mixture smells of Isopropanol still, no signs of any acetone at all... Perhaps this is IP?

That is the end of my current results, I will wait up to a week before I filter and do tests on the formed substance.

Isoproplyene peroxide

Dr. BOOM - 20-12-2004 at 01:11

Anyone actually made his material before? VOD?

PainKilla - 20-12-2004 at 08:34

I assume you mean isopropyl peroxide....I have tried it but it did not work, I got about 3 crystals, probably from imputies in the liquid. Even if it is possible, it is not explosive and used rocket fuels or something like that. Or wait, no that IsPOH nitrate..... I dont think this is even possible.

AngelEyes - 20-12-2004 at 08:57

I would have thought:

Isopropyl + H Peroxide + Acid --> Acetone Peroxide (+ Water + remaining acid)

The Isopropyl is first oxidised to Acetone which is then subsequently peroxidised to AP.
There are a few energetic materials (and salts?) that can be made from Isopropyl...just not a peroxide I think.

?

Dr. BOOM - 20-12-2004 at 12:32

organic chem book says that say it can be peroxidized...humm, but I tried it last night and the liquid is still sitting there..slight amount of bubbles but no solid crystals. I wonder if this material needs some warmth? oh well,

SEARCH before you post! Chemoleo.

[Edited on 20-12-2004 by chemoleo]

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Gezzz, sorry Chemoleo.... didn't mean to double post
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I have a warning for all of those who want to make IP.. the crystalization process occurs through its vapours... I found crystals forming ontop of the container lid and they are extremely sensitive to any kind of friction or sudden change in temperature. Damn, I knew it. Be careful guys. ---guess the H202 is converting the Isopropal Alcohol into actone. ...just a guess.

[Edited on 21-12-2004 by Dr. BOOM]