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VTchem
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PETN synth
A lot of your posts refer to PETN. In my trolling of the web I have come across some information about it but I seem to have missed the memo on how to
synthesize it.
If this belongs in another thread let me know. I searched PETN and I only found tangential references to it and no threads about making it. If there
is a really simple explanation elsewhere just point me in the right direction, if not, then would some one care to post a fairly comprehensive
procedure (many of you seem to be very familiar with the stuff). Anyway, thanks to all of you, I have finally found people who think like I do. I was
always blowing things up (or attempting to) as a kid, and now I am embarking on a career in chemistry and am glad to find like minded people!
Go Hokies! \"If it goes \'BOOM\' I like it!\" -Me
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Pulverulescent
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Have a look in Davis' COPAE in the site-library.
It's the best place to start.
PETN is a very powerful explosive, as you probably already know!
I'm an obsessive blower-things-upper, too!
Oh, and you're welcome aboard!
P
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Pulverulescent
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Actually, I should have described myself as someone with a strong interest in energetic materials!
'Sounds marginally better!
P
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VTchem
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Thanks, I had started reading that but had not gotten through all 490 pages yet. Is there anything that I should note in particular about this
process? Has anyone done this (the procedure given by Davis) and is Pentaerythrite readily available to an individual or will I have to make it from
formaldehyde and acetaldehyde?
And thanks for the welcome, can't wait to contribute.
In today's world sounding PC is sometimes more important than being PC! And yes, I too am an "unpaid energetic materials researcher" etc.
[Edited on 25-4-2008 by VTchem]
Go Hokies! \"If it goes \'BOOM\' I like it!\" -Me
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vulture
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First of all, don't double post but use the edit function.
Secondly, we frown upon recipe exchange here. Get your own creative chemistry going, think of something new, but don't go down the beaten path with
how much X with Y to get "insert explosive".
[Edited on 25-4-2008 by vulture]
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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VTchem
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OK will do, thanks for being understanding.
Go Hokies! \"If it goes \'BOOM\' I like it!\" -Me
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-jeffB
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Welcome aboard, and go Hokie, but not the way I did my freshman year:
If you're going to make flare compositions (much less primaries), don't do it in Lee Hall.
If you do, don't use chlorate and sulfur.
If you do, don't set off a little bit of it, then tuck all the rest away in the back of your dresser.
If you do, don't rearrange your room and move your dresser against the radiator.
If you do, don't expect to get off with probation as I did. Those were gentler times.
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octave
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Dang I didn't know people here lived near me! Pentaerythritol isn't readily available for purchase for any average Joe as it has no other use than for
the synthesis of this explosive and for Some type of resin process if i recall correctly.
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VTchem
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Wow how much damage did that inflict JeffB? That sounds like the kind of RA nightmare passed done to scare the incoming freshmen! Thanks for the
warning, however I live on upper quad and there have already been explosions here occasionally since the days of prohibition. I was planning on doing
some chemical exploration when I got home and I don't think I would ever try to synthesize something so frowned upon here at school unless I had a
really good reason.....but I could probably come up with one if I thought hard enough.
Anyway, the only reason I asked about a recipe is because I don't want to lose a hand or worse, you know I have a very limited supply of body parts! I
will however try my own synth but just make sure I start small. If this needs to be Detritus-ed, go ahead and do that sorry for the annoying thread. I
have been reading on here for sometime now but only recently decided to join the conversation, so please excuse any minor mistakes, this is the first
forum that I felt was good enough to join, the rest usually degenerate into mindless banter and mudslinging and I get more that enough of that with
the elections the way they are!
Go Hokies! \"If it goes \'BOOM\' I like it!\" -Me
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Sickman
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VTchem,
Check out this link for the best step by step synthesis for PETN that I have seen for a lab scale synthesis.
Very good PETN synthesis courtesy of Rosco Bodine
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Pulverulescent
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PETN is fairly difficult, all things considered, VTchem!
Have you thought about cyclonite (RDX)!
Its synth is somewhat easier, more forgiving, and raw material (hexamine) easier to get.
It uses the same quality HN03 but yields are smaller (minor detail?).
It's slightly more powerful and somewhat less sensitive than PETN!
P
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Pulverulescent
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http://www.svenskakemi.nu/lagerkemikalier.html
This Swedish pyro-supplier lists pentaerythritol on its chem-page.
'Some other interesting stuff, too; all in Swedish, though!
P
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-jeffB
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| Quote: | Originally posted by VTchem
Wow how much damage did that inflict JeffB? That sounds like the kind of RA nightmare passed done to scare the incoming freshmen! Thanks for the
warning, however I live on upper quad and there have already been explosions here occasionally since the days of prohibition. I was planning on doing
some chemical exploration when I got home and I don't think I would ever try to synthesize something so frowned upon here at school unless I had a
really good reason.....but I could probably come up with one if I thought hard enough. |
I don't think there's a reason good enough today. You'd make the national news, and you'd probably go away for a very long time. All I had was a
fire -- in addition to respecting my body parts, I never liked loud noises -- and I was still really, really lucky not to face charges. That kind of
luck is no longer available.
If I hadn't been so busy with computers -- which, unlike chemical reactions, offer "undo" commands and restoration from backups -- I would've pursued
an undergrad research opportunity with someone in the chem department. I don't have any specific recommendations; this was all close to thirty years
ago, and I don't know if any of the profs I talked to are still there. They actually had a fluorine lab at that time, but it looks like that's gone
now. Take a look at the departmental Web site, see what research the different faculty members are doing, and pick a few areas that seem interesting.
After you've gotten a year or two of classes under your belt, you should be able to get involved with a project that's doing real research; you might
even be able to get a publication or two.
| Quote: | | Anyway, the only reason I asked about a recipe is because I don't want to lose a hand or worse, you know I have a very limited supply of body parts! I
will however try my own synth but just make sure I start small. If this needs to be Detritus-ed, go ahead and do that sorry for the annoying thread. I
have been reading on here for sometime now but only recently decided to join the conversation, so please excuse any minor mistakes, this is the first
forum that I felt was good enough to join, the rest usually degenerate into mindless banter and mudslinging and I get more that enough of that with
the elections the way they are! |
The only thing I can say is, DO NOT try ANYTHING like this in a dorm, and be very, very cautious about trying it in an apartment. Others here may
have different perspectives, but as far as I'm concerned, group housing is no place for even mildly hazardous materials. (And, let's be honest, are
you really interested in materials that AREN'T hazardous?  )
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VTchem
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I would never do it in the dorms, I agree that group housing + hazardous materials = very bad situation. Thanks for the synths guys, I was trying to
decide what I wanted to work up and I came to PETN because so many people compare what they made to it, and it seems to be some kind of standard. RDX
also had piqued my interest but I thought that seemed more exotic but if you say its not top bad I might try that too, Pulverulescent. Its only a few
days now until I leave campus and all of my equipment/materials are at home so currently I am doing all the research I can into the backgrounds of all
of these compounds.
What compound would you guys say is stable, safe and easy to make (yield and power are secondary for now). I need to walk before I run. I have
experience with things like LN2 and HCCH + O2 stuff but this will be my first nitration. I was also thinking about peroxidation but that seems so much
more dangerous from what I what have read, correct me if I am wrong but organic peroxides tend to be really rich and rather unstable.
Go Hokies! \"If it goes \'BOOM\' I like it!\" -Me
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-jeffB
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| Quote: | Originally posted by VTchem
What compound would you guys say is stable, safe and easy to make (yield and power are secondary for now). I need to walk before I run. I have
experience with things like LN2 and HCCH + O2 stuff but this will be my first nitration. |
This isn't my main field of interest, but I'd guess the best starting point (safe/stable/easy) would be nitrocellulose. I managed to get a runaway
with even that by nitrating toilet tissue (too porous and absorbent), but the only untoward result was copious NOx and steam. I usually started with
cotton cloth or cotton wads, rinsed with water and bicarbonate, and then dissolved in acetone. I never tried to get it to detonate, and doubt that it
would, but my better efforts deflagrated quickly and cleanly.
Then again, I blew up my dresser, so I'm not the best source of advice. 
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Pulverulescent
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Hexamine was the first compound I nitrated, and I did it in the kitchen-sink.
The reaction-vessel was cooled by running water (~20*C) and the acid was yellowish.
It would have been safer to decolourise the acid first, though, by blowing dry air through it.
One compound I'd be very wary of is nitro.
I made it once but never again; I don't quite trust it, anymore!
P
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VTchem
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Thanks guys, NG looked interesting at first despite its obvious hazards and a lot of people here seem to have made it or tried, but then when I read
that it is even more sensitive when impure, I decided to look elsewhere...but maybe someday.
[Edited on 26-4-2008 by VTchem]
Go Hokies! \"If it goes \'BOOM\' I like it!\" -Me
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chemoleo
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Back on TOPIC please guys.
Quicksilver has made PETN with HNO3 less than 100%, I think he posted it in the trinitrotoluene thread:
| Quote: |
***********
for PETN synth
***********
Verified efficient method of preparing PETN from diluted HNO3
use
32,7 ml of 70% HNO3 (75% excess)
18,9 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------
or
34,0 ml of 65% HNO3 (66% excess)
24,8 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------
or
34,8 ml of 58% HNO3 (48% excess)
36,3 ml of 96% H2SO4
10,0 g of Pentaerythrite
Let me say this; it does need to be monitored to a get degree. Temp must not exceed 15-20C or else it may run and spew NOx.
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There's some question about whether these are full tetranitrates or mixtures, but crystallisation appears to occur well, suggesting the purity of the
final product is high.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Microtek
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I downloaded an excel sheet from roguesci which contained an adaptation of the triangular nitration graphs in Urbanski. You could enter amounts and
purity of acids and then it would calculate the change in concentration as the nitration ran. The results was then displayed as an overlay on the
triangular graph. This allowed you to see if the process stayed within the PETN production zone or if it strayed into domains where the lower nitrates
were produced.
Playing with this tool lets you determine an optimum acid composition depending on your individual supply situation.
I also found that with well purified and highly concentrated nitric (99%) you should get almost quantitative yield with only 2.5 ml acid per gram of
PE. I tested it with nitric acid that titrated as 99.5 % concentration and got a 97% yield (assuming only the tetranitrate was produced).
I don't have the document anymore, but I think it was called petn2.xls
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Pulverulescent
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| Quote: | Originally posted by Microtek
I tested it with nitric acid that titrated as 99.5 % concentration and got a 97% yield (assuming only the tetranitrate was produced).
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I have no experience of PETN yet, but I just assumed lower nitrates would be removed by repeated washings.
And 99.5% HN03 Microtek, that's practically anhydrous---how did you get that high a concentration?
P
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hokk
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The downside with that shop is that you have to make a minimum order of 1500SEK (161 Euro, 255$ excluding
VAT).
This polish guy also has it tough (among other things), http://www.keten.org.pl/odczynniki.html
| Quote: | Originally posted by chemoleo
Quicksilver has made PETN with HNO3 less than 100%, I think he posted it in the trinitrotoluene thread:
....
There's some question about whether these are full tetranitrates or mixtures, but crystallisation appears to occur well, suggesting the purity of the
final product is high. |
Don't know how pure it is (any tips for testing this?), but the synth in the middle
gives a one hell of a energetic compound.
[Edited on 27-4-2008 by hokk]
[Edited on 27-4-2008 by hokk]
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Microtek
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| Quote: |
And 99.5% HN03 Microtek, that's practically anhydrous---how did you get that high a concentration?
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Note that I only said that it titrated as 99.5%....
Anyway I made it as follows:
50 ml HNO3, 62% conc. was added to 50 ml H2SO4, 96% in a distillation setup. The mix was distilled at atmospheric pressure without boiling to reduce
decomposition.
The first 30 ml was collected and the remaining acids were heated to 200 C to reconcentrate the sulfuric acid.
Then, after cooling down, the 30 ml distilled nitric (which had been determined to be about 85% conc by gravimetric measurement - this was an estimate
since there was some dissolved NOx ) was added.
The mix was distilled as before, but even slower. I collected about 20 ml of very pale yellow acid. This acid was then heated to 50 C and dried air
was bubbled through until it was completely colourless. It was stoppered up and cooled to 20 C, at which point a sample was removed for titration.
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Pulverulescent
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Thanks for that, Microtek.
So slow below-boiling distillation does work.
I imagine it's very slow, but if the temp was constant (~90*C?) it could presumably run for many hours unattended, giving higher than usual
concentration of acid.
It's quite interesting!
P
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Microtek
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Yes, I let it run in my shed unattended, I just check on it now and again. I think that a batch like that takes maybe three hours. I use a glass
kettle placed on a portable electric stove and a water cooled condensor (cooling water recirculated by a small bilge pump). The temperature fluctuates
between maybe 90 and 110 C since the thermostat is not so accurate. I wrap the top of the kettle in Al foil to provide a little insulation, so the
temp of the acids doesn't have to be higher to compensate for heat loss before the vapour gets to the condensor.
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DJF90
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3 hours for 20ml of acid  thats long... its a good job it can be left
unattended... but at the end of the day the collected acid is surely worth it. I assume that using a larger RB flask than necessary would aid in the
distillation as it would provide the acid with more surface area and hence can evaporate/vaporise more readily? Can I ask what you titrated the acid
with? NaOH solution would seem reasonable, but at what concentration? And how large was the sample of acid to be titrated? Your results are truely
outstanding though microtek
[Edited on 27-4-2008 by DJF90]
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