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Author: Subject: PETN synth
dann2
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[*] posted on 25-2-2011 at 16:51


Hello,

Can anyone tell me how to make PETN of the 'high surface area' type that is suitable for use in EBW detonators. This stuff is more sensitive than regular PETN.
I presume it's just a matter of recyrstallizing in some special way?

There is a thread here
https://www.sciencemadness.org/whisper/viewthread.php?tid=81...
which is close to the mark but nothing specific that I can see.

Cheers,
Dann2
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quicksilver
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[*] posted on 26-2-2011 at 09:25


Quote: Originally posted by dann2  
Hello,

Can anyone tell me how to make PETN of the 'high surface area' type that is suitable for use in EBW detonators. This stuff is more sensitive than regular PETN.
I presume it's just a matter of recyrstallizing in some special way?




It's preferred that individuals provide patent reference or documentation rather than specific "how to" agenda. This is both a safety and science based issue. Retyping any synthesis is not only laborious but can omit critical material or side-issues.
Particulate density may have relevancy but most often the lower nitration adulterants make some difference.
From "the horse's mouth" research please see "The Pentaerythritols" (Berlow, Barth, & Snow: 1957) & Urbanski
PETN is PETN & RDX is RDX unless adulterated by lower nitrated products or density issues arise in application.


edit:
Specifically see PEN as related to PETN synthesis.

[Edited on 26-2-2011 by quicksilver]




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nitro-genes
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[*] posted on 26-2-2011 at 09:25


IIRC, Fine needles are most sensitive and used for EBW, make by fast cooling of saturated solution in acetone.

nm(!)-um size irregular shapes can be made by high pressure spraying of a saturated 60 deg. C acetone solution in stirred ice water.

[Edited on 26-2-2011 by nitro-genes]
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dann2
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[*] posted on 11-3-2011 at 16:56



Apologies for the 'cook book' attitude.
From the bowles of the US info. bridge came the following:

HE F0RMULATI0N
A. G. Oabom
DEVELOPMENT DIVISION
JULY - SEPTEMBER 1971
SANL 900-003, 004, 006, 008
Lawrence Livermore Laboratory

The method here gives PETN with a surface area of 5300cm^2 per gram. A micronizer will give 20,000 cm^2 per gram.

The reprecipitation of the control batch into LX-13 PETN was done by conventional crash reprecipitation into water not using-the Micronizer. It is similar to that used by manufacturing except for the batch size and the vessels used. Thirty-six pounds of PETN dissolved in 20 gallons of Acetone (a 15% solution) is added to 280 gallons of violently agitated distilled water at 70F in the 300- gallon kettle. Some stops were required to change the in-line filter. The in-line filter is included immediately before the spray nozzle which is held approximately 6 inches above the violently agitated water. The reprecipitated PETN is filtered in to a cloth lined filter buggy and subsequently dried for 36 hours at 150F after being washed with distilled water.


Dann2
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[*] posted on 7-11-2012 at 22:38


I synthesized my first and second batch of PETN.
Thank you very much Nuke. Your method worked great for me.
Yield look great ... Will know for sure when it dries.
Thanks again Nuke. Will post final results shortly.




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[*] posted on 10-11-2012 at 20:58


Well for some reason ... I couldn't edit.
But reguardless.
I did 3 batches. 10, 20, 20 grams of PE.
End result of re-crystallized PETN was 108 grams.
I did everything like Nuke besides heat the mix to +70*C. Didn't feel comfy doing that .... instead just let the flask sit in hot tap water 40*C.
My nitration didn't start till about 13*-14*C.
I could see the PE floating around when cold. As soon as the nitration begins .... Mixture starts to get cloudy.
After drying I have fine dry powder. Definitely no needles .... Just fine powder.
Don't have a microscope to examine.
Thanks again Nuke.

[Edited on 11-11-2012 by Motherload]




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[*] posted on 11-11-2012 at 03:10


I have also synthesized PETN for the second time now, but the problem I get is the detonation. So far I have used only HMTD, which was successfully produced (the hammer test of small quantities gave out a pretty large bang), but I haven't been able to successfully detonate PETN with it. In the first try I figured the lair of paper between the two was to thick, so the blast was directed upwards, away from PETN. But on the second try, I used the thinnest of toilet paper lairs, but yet again I was only able to set PETN on fire without an explosion (both reagents were in powdered shape).

Was the mixture not compressed enough (I feel kind of uneasy compressing mechanically sensitive explosive such as HMTD) and is there a better way of detonating it? I don't have much experience in detonation but I heard that plastification of PETN and then using a detonator is the best method. Is there a thread about making detonators and plastification anywhere?
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[*] posted on 11-11-2012 at 08:08


Well ... I just made a cap with a .22WMR (.22 Magnum) case and pressed the PETN down with a 7/32 punch.
Then .... only primary I have access to is cartridge primers ... I dismantled 5 large pistol magnum primers and pressed those on one at a time with a wooden dowel.
3 inches of cannon along with a grommet was pushed in the case ... And crimped with my multitool. SOG has a EOD model with a #8 cap crimper.
Test .... Sometime this afternoon.




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[*] posted on 22-11-2012 at 07:09


Cap worked fine .... I did top up the primer/Styphanate with a little BP.
It was shoved inside an old garden tie and it split it after it went off.
I had .4 gm of PETN in it.
Next is to see if that same set up cap will work to detonate some PETN+PIB "C-4".




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[*] posted on 28-11-2012 at 02:37


Can PETN be made as it is told in powerlabs method . Does the PETN made by powelab is of enough pure quality to be used in detonators
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[*] posted on 29-11-2012 at 08:36


How percent pure Pentaerythritol for petn ? %98 Pentaerythritol Is it enough?
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[*] posted on 29-11-2012 at 09:23


Quote: Originally posted by Vikascoder  
Can PETN be made as it is told in powerlabs method . Does the PETN made by powelab is of enough pure quality to be used in detonators


hi

i made PETN this way and have to say, that its pretty powerful and the shape of the crystals after recrystalisation in acetone was like small needles and where much better to compress than PETN made of high concentrated nitric acid (crystals like dry sand) - im not sure if its the Tetra-nitrate of PE or something lower but i would go for it as a detonator...


@gamez34

sure, why not?
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[*] posted on 29-11-2012 at 09:48


@VladimirLem
Thank You :) I'm just researching
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[*] posted on 30-11-2012 at 10:03


@gamez34
All I have is some Korean brand 98% Pentaerythritol.
It seems to work just fine.

Although I found (CCI large pistol magnum primers) lead styp doesn't always detonate PETN. I was using 5 primers per .4 grams of PETN.
Some caps went off and some ... Only the top blew off .... PETN stayed in the bottom casing besides a few sprinkles.
PETN is from the same batch and dry.
Lead Styp is from the same pack of primers.
Do I need to rid the primer composition of fillers and use pure Lead Styp ??
Any suggestions on purification ? Not much available for solubility data.
Or
Is there a threshold quantity .... Minimum amount of primary required to detonate a secondary ?
Again ... Not much info on detonator loadings.
I guess it's not as prevailant of a hobby as ammunition loading :)
Thank you.




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[*] posted on 3-12-2012 at 00:50


Alright .. I took apart some federal gold medal magnum rifle primers.
The priming compound has a green color to it ... There is defiantly some lead azide in the mix.
Anyone know what the green might be ?
I pressed .45 grams of PETN in a case and then put a layer of PETN mixed with primer and then primer.
Hopefully it provides reliable ignition.




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[*] posted on 3-12-2012 at 03:28


Quote: Originally posted by Motherload  
Alright .. I took apart some federal gold medal magnum rifle primers.
The priming compound has a green color to it ... There is defiantly some lead azide in the mix.
Anyone know what the green might be ?
I pressed .45 grams of PETN in a case and then put a layer of PETN mixed with primer and then primer.
Hopefully it provides reliable ignition.

I'm pretty sure the green stuff is a waterproof lacquer with a dye for colour-coding purposes.

I don't know that much about primers (ammunition is hard to find in my country) but Tenney L. Lewis states that PETN can be detonated by 0.01g of lead azide. Eventually you'll make your own primary explosives, right?
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[*] posted on 3-12-2012 at 11:09


@Kallium
I don't think it's a dye as its not a 100% homogenous and crystalline ... I can see whiter clumps which I believe are Pb(N3)2

I will make my own primaries when I get a hot plate stirrer for Christmas from my self..
Then the Hydrazine Sulfate via the MEK ketazine and then the azides.
In the meantime I am just going to use percussion primers. There is no storage concerns with them unlike a 5 gram vial of dry primary.
And I just stay as far away from peroxides. Too damn unpredictable.




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[*] posted on 16-1-2013 at 10:24
PETN Sensitivity


I have purified the fluffy powder PETN with Acetone.
Hot Acetone in a water bath around 55*C with some added urea and NaHCO3.
PETN was added and dissolved. A separate solution in hot water was made with urea and NaHCO3.
Now the hot water solution was trickled into the hot acetone solution via a burette.
~ 3 drops/sec.
Eventually the PETN crystallized out a needles about 1 mm or so long as the mixture turned to a slushie.
The PETN crystals were filtered and washed twice with hot 60*C water.
Then let out to dry for 48 hours near a radiator..

So I put a tiny pinch in some aluminium foil .... Put it on an anvil and give it good wack with a 1 pound hammer..
Nothing !! The foil tears and embeds itself and some powdered PETN into the anvil and the hammer..

Can someone tell me what's wrong here.. Unfortunately there is no videos floating around regarding impact sensitivity of PETN on the tube..




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[*] posted on 16-1-2013 at 12:59


It should definitely detonate between steel
(and make your ears ring if you use a little to much)

[Edited on 16-1-2013 by hiperion42]




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[*] posted on 19-1-2013 at 19:00


I take a small square of Al foil .... And put in half a match head clump of crystals ... Fold it into a quarter .... Finger press it and give it a wack. Nothing happens.
Do I need to use more ? Am I not hitting it hard enough and over estimating PETN's sensitivity ? Or is there something wrong with my product .... Tri-nitrates etc.
Any pointers will be appreciated.




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[*] posted on 23-1-2013 at 18:55



What impurities is paint grade PE liable to contain?
It is not considered pure enough for PETN (military grade ).
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[*] posted on 26-1-2013 at 16:32


On impurities in paint grade PE.

See post of 7 12 10

From this web page:

http://www.vistachemie.com/index.php/most-active-chemicals/5...

There are commercially three grades of pentaerythritol: mono ( 98 percent, with di- and tripentaerythritol impurities), technical (88 percent, with 8 to 10 percent dipentaerythritol, balance tri-) and nitration (99 percent, with di- and tripentaerythritol impurities).




Attached file gives a table showing % of impurities in a companys PE.

What are 'formals'?

Useful paper here is anyone can get it.

http://onlinelibrary.wiley.com/doi/10.1002/jctb.5030320404/a...

Patent for PE purification
http://www.freepatentsonline.com/2358697.html

Attachment: pentaerythritol_20081124[1].pdf (547kB)
This file has been downloaded 1214 times



[Edited on 27-1-2013 by jock88]
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[*] posted on 26-1-2013 at 20:09


Well according to the last link for a brochure ... The only difference between "nitration grade" and "mono grade" is particle size.
Other properties seem identical.
Others on this board have used the same PE from the same Korean supplier which is 98% and seem to have no trouble.
I believe I am overestimating the sensitivity of PETN. Given the physical properties and the amount of washings with hot water .... It shouldn't contain lower nitrates.
I am going to try a slightly larger pellet and a harder swing.
Thanks for the input though.
I'll post more info.




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[*] posted on 4-3-2013 at 05:28


Hi guys, I am new to this forum and this is my first post. I tried preparing PETN with successful experience in small scale preparation of NC,NG,NS,HMTD,TATP and nitrourea. I used 35.2ml 58% HNO3 + 40ml 89%H2SO4 cooled it to -15C. I started adding 10g PE(98% Loba Chem) very slowly keeping temp at 5C. at about 10C NO2 starts evolving,I controlled it with salt Ice mix and very fast steering with blowing air into flask.It took abt an hour to add 10gm PE but then also the mixture seems to start evolving NO2 if temp is going above 12C. I had about 2kg of ice which all finished and in about 3hrs time the whole mixture came to 22C and started evolving NO2 again. I didn't dare to heat the mixture at 45C for 20 mins as it was evolving NO2 and seems unstable. I dropped whole mixture in 10C cold 500ml water. I started filtering the diluted solution (the NO2 was still evolving very slowly from filter paper. I washed the product 3 times with normal water (500ml) every time I found milky filtrate. I next washed with 400 ml 5% sodium carbonate solution. The solution was cloudy. I left the PETN and 5% Na2CO3 solution for 6hr in refrigerator to settle. even after 6hr the mixture didn't completely settle. It has white ppt and milky solution above. I decided to filter the solution filtrate was turbid which I thrown in sink and washed the solid ppt with water and let it dry. I will recrystallize it with acetone later today.

Please can I get some help in understanding why I got runaway nitration even at 15C and why mixture become unstable even after consuming 2kg ice and 3hr of time.
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[*] posted on 4-3-2013 at 06:52


ONLIASHISH: I'm no expert at PETN synthesis but I can venture a guess. What type of Sulfuric Acid are you using? If it is the drain cleaner type (I assumed you were by the 89%), impurities such as metals could be reacting negatively with your Nitric Acid to cause the evolution of NO2 gases and excess heat. After all, NA is notorious for attacking metals.

I have some experience in the metal plating business and Nitric Acid (~35%) is often to use to strip surfaces of a plated metal. For instance, a Titanium heater that had been used in Nickel plating needed to be stripped back down to the Titanium. I placed it in a 35% NA solution for several hours to strip the Ni plating layer. Ti forms a tough Oxide layer so I was not worried about it being destroyed by the acid.

Anyway, oxidation/nitration of the Ni generated NO2 gas and heat. Not to mention a puke green color that is characteristic of Nickel Nitrate. So what I'm throwing out there is that perhaps metal impurities in your nitration bath are causing your problem. Try using higher grade H2SO4 and see what happens.
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