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The Ed
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failed IP
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.
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shadeT
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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 ...
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a123x
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| 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.
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flashpoint
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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...
-----------------------------
No kidding. Now ain't that news shocking enough to waste space here...
[Edited on 17-12-2003 by vulture]
-----------------------------
Sorry 
[Edited on 18-12-2003 by flashpoint]
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narkar
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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
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Mumbles
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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.
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chemoleo
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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?
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Mumbles
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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.
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KABOOOM(pyrojustforfun)
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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 H<sub>2</sub>O<sub>2</sub> mixs with alchols are serious hazard but almost with
any fuel
the white hairs should be a polymer. <i>maybe</i> that of acroleine or acrylic acid I'm not sure because
H<sub>2</sub>O<sub>2</sub> additionally reacts with the vinyl group ...
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unionised
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Just to add to the complexity of the question, aldehydes form peroxides too.
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chemoleo
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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.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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unionised
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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.
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Polverone
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MEK as catalyst in alcohol peroxidation?
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.
PGP Key and corresponding e-mail address
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PainKilla
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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.
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Dr. BOOM
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Isoproplyene peroxide
Anyone actually made his material before? VOD?
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PainKilla
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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.
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AngelEyes
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I would have thought:
Isopropyl + H Peroxide + Acid --> Acetone Peroxide (+ Water + remaining acid)
The Isopropyl is first oxidised to Acetone which is then subsequently <i>per</i>oxidised to AP.
There are a few energetic materials (and salts?) that can be made from Isopropyl...just not a peroxide I think.
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Dr. BOOM
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?
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]
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