Sciencemadness Discussion Board

PETN synth

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dann2 - 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

quicksilver - 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]

nitro-genes - 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]

dann2 - 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

Motherload - 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.

Motherload - 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]

Neitz - 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?

Motherload - 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.

Motherload - 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".

Vikascoder - 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

Peroksit - 29-11-2012 at 08:36

How percent pure Pentaerythritol for petn ? %98 Pentaerythritol Is it enough?

VladimirLem - 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?

Peroksit - 29-11-2012 at 09:48

@VladimirLem
Thank You :) I'm just researching

Motherload - 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.

Motherload - 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.

Kalium - 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?

Motherload - 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.

PETN Sensitivity

Motherload - 16-1-2013 at 10:24

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..

hiperion42 - 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]

Motherload - 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.

jock88 - 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 ).

jock88 - 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 1425 times



[Edited on 27-1-2013 by jock88]

Motherload - 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.

ONLIASHISH - 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.

10digits - 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.

Motherload - 4-3-2013 at 11:27

If you start adding PE at a temp that's too low .... The PE builds up and not nitrated to PETN. So when the temp rises to the nitration temp .... All the surplus PE wants to get nitrated at the same time causing hot spots and spikes which is probably what results in runaway signs.

PETN Synth

ONLIASHISH - 4-3-2013 at 23:43

Hi Motherload, Thank you for your help,I guessed the same reason as you have mentioned. I did lot of search found I should have done nitration at 15C to 20C very slowly. I have recrystallize impure PETN with acetone at 50C and then filtered after adding water yield is 12g(instead of 22.1g). Learnt something from mistake ;)

PETN Synth

ONLIASHISH - 4-3-2013 at 23:51

Hi 10digit,Thank you for your help. I had pure acids without any other impurities other than water. I had done other synthesis(Nitroglycerine,nitro urea, GC etc) with same acids . The reason given by Mother load is more accurate for my case.

Question about PETN synthesis

Hellbat - 11-1-2016 at 05:30

Hi, I have found a synthesis description for PETN that uses 65% nitric acid instead of fuming nitric acid: http://www.powerlabs.org/chemlabs/petn.htm
But on many other pages I've read that nitrating PE with the mixed acid method mostly yields Pentaerythritoltrinitrate (PETRIN). It seems to be soluble in acetone just as well, so the purification by recrystalization would not remove it. Maybe, this guy actually made the trinitrate without knowing? It's a strong explosive as well.

I've actually found a german synthesis description for PETRIN which was nearly the same procedure as on the website I linked.

hissingnoise - 11-1-2016 at 05:45

Quote:
Maybe, this guy actually made the trinitrate without knowing?

I have the feeling that when Sam Barros 'makes something' he knows exactly what it is he's made!


Hellbat - 11-1-2016 at 07:02

But does anyone have accurate information about that? According to german wikipedia, if PE is nitrated with mixed acid, mostly the trinitrate is formed...
So, either wikipedia or Sam Barros must be wrong.

Bert - 11-1-2016 at 07:09

Why don't you do an experiment and verify if Wikipedia is wrong, and report back.

-------

The method and ratios work. I have tried the version of this originally posted by "Boomer" that Sam apparently either directly copied or used the same information (from Thadeus Urbanski Vol. IV) to derive. Should give 90% + yields with care and the correct grade of pentaerythritol.


Quote:

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
------------------------


Nitration:
1. Cool nitration mixture during mixing of acids, thus minimalize even minimal decomposition of HNO3. Nitration mixture must be cooled before nitration process to temperature of 10°C.
2. While stiring, add pentaerythritee in small portions (1-2g) to nitration mixture, always after previous batch is dissolved. Nitration mixture gradually thicken as PETN forming in solution.
3. Constantly monitor reaction temperature and maintain it in 10-15°C range. Interval of adding pentaerytritol conform to reaction temperature, must not rise over 15°C, leave beaker in cold water.
4. Stir with mixture for next 5 minutes after all pentaerythrite is added and dissolved. Mixture is now thick, but stirring is going well. During nitration process must not be developed any brown fumes of NOx!
5. Now put beaker with mixture into water bath and maintain temperature at 50°C, continuously stir with mixture. During 20 minutes at this temperature, all of possible sulfoesters come into PETN for maximal yield of nitration.
6. While maintaining mixture at higher temperature, mixture must be monitored for developing of NOx fumes. Only light brown colour can be in shrouded beaker. Raised development of NOx pointing to higher temperatures used (even during previous nitration) or insufficient chmemicals purity and further heating may end up in uncontrolled reaction and oxidation of formed PETN. In this case it is better to do not heat at all and end just after nitration (if brown fumes apperas during nitration), the yield will be lower. In case of accidentally runaway reaction during heating, immedialtely pour mixture into cold water, don't try stop reaction by cooling beaker, it will not help.
7. When heating after 20 minutes pass off, pour reaction mixture into cold water and follow standart procedure of filtration, neutralization and purifying of PETN.

Yield was 22,1g of PETN from 10g of pentaerythrite, ~95% of theoretical yield (with 65% HNO3 used).

This procedure is result of my research of most effective method preparing PETN from diluted HNO3. Acid ratios are precisely calculated on data from PETN nitration graph published by T. Urbanski in his book vol. IV. Generaly said, PETN is forming to maximum 30% of water portion in nitration mixture. But, when also H2SO4 is contained in nitration mixture, minimum ammount of water must be keep, or oxidation with small yields occur. With this acid ratios 20% of H2O is minimum. So, this nitration mixture has 20% of water on nitration start and 30% at the end, area for most effective nitration, but again only with this ratios. For other acid ratios must be all recalculated. Excess of HNO3 is used to controll ammount of reaction water. Only ammount of nitration mixture can be extended for lower mixture thickness, but it lower utilization of acids and overall efficiency. But it isn't necessary.

I hope there is no major mistakes in my translation to english ;-)


I am going to merge your thread with an existing PETN thread-

http://www.sciencemadness.org/talk/viewthread.php?tid=10413&...

And you might want to look at the alternative method posted by Rosco Bodine:

http://www.sciencemadness.org/talk/viewthread.php?tid=6151#p...

[Edited on 11-1-2016 by Bert]

NeonPulse - 11-1-2016 at 15:22

I'll too vouch for roscoes method. It is the best synthesis I've tried. No problem in producing high yielding high quality PETN that is easily neutralised and Recrystallized. No heating needed and no Dangerous fuming. You do need High strength clear fuming nitric though. But the trouble is worth it. The end product does seem superior to mixed acid PETN

gnitseretni - 13-1-2016 at 20:25

I don't think the trouble is worth it. Only if you're specifically after PETN for some reason. Otherwise, just go the mixed acids route (assuming that's the easier route for you). You won't notice the difference between a 7k or 7.5k velocity explosive.

I precool my acids and I add my PE while the acids are still below freezin, and I add it pretty fast. It does tend to heat up pretty fast after a certain point but as long as you are prepared and have plenty of ice available you'll be fine.

Microtek - 14-1-2016 at 05:02

The superiority of the product has more to do with stability than with performance, I think. It is very difficult to remove the last traces of sulfuric acid from the product, and this makes it unstable, particularly at elevated temperatures.

Etanol - 18-7-2023 at 10:26

Quote: Originally posted by Bert  

The method and ratios work. I have tried the version of this originally posted by "Boomer" that Sam apparently either directly copied or used the same information (from Thadeus Urbanski Vol. IV) to derive. Should give 90% + yields with care and the correct grade of pentaerythritol.

It seems the diagram in the 4th volume is a lie. 90% PETN output is also formed in mixtures with a small water content in which, according to the diagram, it should not form.

Laboratory of Liptakov - 11-1-2024 at 01:34

Since recently there have been ambiguities regarding the synthesis of PETN, I am attaching a repeatedly proven method of preparation in graphic form to the relevant thread....:cool:





P1.png - 721kB P2.png - 888kB P3.png - 819kB

P4.png - 825kB

DennyDevHE77 - 11-1-2024 at 02:29

Has anyone tested the product above on a chromatograph? How does it match PETN obtained with pure 98% nitric acid?

Laboratory of Liptakov - 11-1-2024 at 03:47

Using 98% HNO3 can cause more trouble than good. But that's just my guess. Using 98% HNO3 has not been tested in this process. Chromatography was not used for measurement PETN from graphic guide process. But the result is stable and quality PETN. Repeatedly. 20g PE can be added to 65% HNO3 at once. Without dramatic increase of temperature. PE is completely soluble in HNO3 65% by picture.

DennyDevHE77 - 11-1-2024 at 05:58

That's not the point. When using a mixture of nitric and sulfuric acid, it also partially converts pentaerythritol into mixed sulfoesters. When heated to 50-60C, nitric acid will convert these esters to PETN. But some esters (I think pentaerythritol dinitrate-disulfate) are still not completely converted to PETN.

I used to (and still do sometimes) boil PETNs in 1% baking soda solution to remove them. But this resulted in 5-10% yield loss, later an ethanol member advised me to "cook" PETN in 85-90C soda solution, without boiling, and it seemed to work.

That's the upside of nitrating 90-99% nitric acid. PETN is obtained with a slightly higher yield (up to 98%), and most importantly it is formed immediately pure. All that is needed afterwards is to remove the acid in acetone, and that's all.

ManyInterests - 15-1-2024 at 15:59

I am making some ammonium nitrate since I managed to find a place that sells ammonium carbonate for relatively cheap and am turning some calcium nitrate into it, I was planning on testing it to make some ETN. While reviewing my notes and the forums, I came accross this thread on SM that linked to this video https://www.bitchute.com/video/XrjpCnYs7fVL/

He mentioned in the video that he used the same method to make PETN out of ammonium nitrate. It was something that I was looking for as well. Obviously in the video he doesn't show the purification and recrystalization (but I already know how to do that), and I do have strong reservations about him simply dumping the whole amount of erythritol into the nitrating mixture, but if it is as good as he says it is (and I will add the stuff slowly) I am thinking of following those steps.

Except instead of letting the whole thing be at -18C, I'll start at a warmer temperature for PETN. I remember the problems I had with my first synthesis where my yield was extremely low.

DennyDevHE77 - 15-1-2024 at 20:55

The nitration reaction of ETN (at least when ammonium nitrate is used), proceeds much more calmly than the nitration of PETN. I have many times added tens of grams of erythritol to the nitrating mixture at once, when cooling with cold water, moreover, periodic lowering of the beaker with nitrating mixture into ice water was enough for effective cooling during the whole nitration (usually 2 hours). Besides, with ETN there is no difference between +5°C, +10°C, +25°C. And even above +30°C it is hard to lose control, the mixture starts to bubble a bit, at which point you can stir it vigorously and cool it down.

PETN is quite different. Its nitration is much more active and the temperature can rise much higher. Usually when loading 100g of pentaerythritol it should be added 1-2 grams at a time, preferably each new portion should be added after adding and dissolving the previous one and stabilizing the temperature. Ah yes, in sulfur-nitrogen mixture PE dissolves much slower than erythritol. PETN when nitrated with 90-97% acid alone is normally nitrated both at 0°C and at +20°C. When nitrating with sulfuric acid you need to keep temperatures between +8°C and +15°C. If the temperature is lower, you get PETRIN (heavy oil, I got it at +3°C), if it is higher, you get badly exploding, yellow PETN (I posted it here once). However, PETRIN is removed by holding at +30°C after adding all the PE.

To summarize, if you're nitrating ETN, just throw in tablespoons of erythritol into the nitro mixture, stir lazily, and occasionally watch that it's not above 25°C. You can just keep a glass of nitro mixture in a bowl of cold water. It's with nitrate! If with nitric acid, the reaction is more active, but still easily controlled.

With PETN, however, strictly watch the temperature. Ice cubes with water will give you +11 to +14. Then soak at +30, then soak for 20 min at +50°C.

Since it is winter, you can use 3 weight parts of snow and 1 weight part of ice, this will give you about -20. Then pentaerythritol can be added in tens of grams, but again, pentaerythritol takes a long time to dissolve, so after adding all the pentaerythritol, allow a soak of 10 min, stirring it before moving on to the next steps.

ManyInterests - 16-1-2024 at 03:35

Quote: Originally posted by DennyDevHE77  
The nitration reaction of ETN (at least when ammonium nitrate is used), proceeds much more calmly than the nitration of PETN. I have many times added tens of grams of erythritol to the nitrating mixture at once, when cooling with cold water, moreover, periodic lowering of the beaker with nitrating mixture into ice water was enough for effective cooling during the whole nitration (usually 2 hours). Besides, with ETN there is no difference between +5°C, +10°C, +25°C. And even above +30°C it is hard to lose control, the mixture starts to bubble a bit, at which point you can stir it vigorously and cool it down.

PETN is quite different. Its nitration is much more active and the temperature can rise much higher. Usually when loading 100g of pentaerythritol it should be added 1-2 grams at a time, preferably each new portion should be added after adding and dissolving the previous one and stabilizing the temperature. Ah yes, in sulfur-nitrogen mixture PE dissolves much slower than erythritol. PETN when nitrated with 90-97% acid alone is normally nitrated both at 0°C and at +20°C. When nitrating with sulfuric acid you need to keep temperatures between +8°C and +15°C. If the temperature is lower, you get PETRIN (heavy oil, I got it at +3°C), if it is higher, you get badly exploding, yellow PETN (I posted it here once). However, PETRIN is removed by holding at +30°C after adding all the PE.

To summarize, if you're nitrating ETN, just throw in tablespoons of erythritol into the nitro mixture, stir lazily, and occasionally watch that it's not above 25°C. You can just keep a glass of nitro mixture in a bowl of cold water. It's with nitrate! If with nitric acid, the reaction is more active, but still easily controlled.

With PETN, however, strictly watch the temperature. Ice cubes with water will give you +11 to +14. Then soak at +30, then soak for 20 min at +50°C.

Since it is winter, you can use 3 weight parts of snow and 1 weight part of ice, this will give you about -20. Then pentaerythritol can be added in tens of grams, but again, pentaerythritol takes a long time to dissolve, so after adding all the pentaerythritol, allow a soak of 10 min, stirring it before moving on to the next steps.


I suspected that PETN would be hotter than ETN. ETN synthesis is quite mild.

But I am assuming that this nitrate salt method will work and hopefully get good yields. I am getting a little fatigued of basic reagent synthesis.

Ok, so start at -20C for PETN, but it will need a heating step to allow to turn everything into quality PETN and and such. I think we thought we needed to start at a hotter temperature? I don't got much time now, so I will leave this thought for now...

[Edited on 16-1-2024 by ManyInterests]

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