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DennyDevHE77 - 30-11-2023 at 20:42

The oddities of plastic explosives. Recently I made plastic (on PETN) on polybutylene once again. 90\10. If earlier this composition was like a very steep dough with high density (1.6 g/ml), now the plastic explosive turned out to be very easily compressible, at the same time it crumbles easily and has low density (1.3). I have not seen this before, even 95/5 compounds were easy to crumble but hard to compress.

The fractional composition is very different, from manually ground into flour, and the smallest crystals obtained by rapid infusion of hot acetone into water, to quite distinguishable crystals.

So far, my only assumption is that most of the PETN is just too fine and a coarse fraction should be added, but I could be wrong.

Has anyone ever encountered anything like this? When the plastic looks like kinetic sand?

greenlight - 1-12-2023 at 06:09

How have you stored the polyisobutylene? Away from heat, moisture and direct sunlight?
The only thing I can think of at the moment considering the PETN has been prepared the same way is that the PIB has somehow gone bad.

Laboratory of Liptakov - 1-12-2023 at 08:05

Denny.....I think you made a mistake when mixing the PIB : Oil ratio. Because PIB is usually added as a 10% solution of PIB in gasoline. But the oil is added as a 100% solution. A very common mistake is that someone mixes 1 part PIB and 1 part oil. In that case, the effect you described will occur. Flowing lump......:cool:

DennyDevHE77 - 1-12-2023 at 09:28

I use mouse glue as a source of polymers. Its composition is polybutylene - 80.83% , polyisobutylene - 9.60% , cyclosan - 9.57%. What the latter is, is not clear, perhaps they are low molecular weight polymers, or a trade name for a crosslinker.... But I think it is just low molecular weight polymers to give the finished product (glue), more liquid consistency. Or maybe it's really some kind of oil with sebacic/phthalic acid esters. As far as I understand, production of low molecular weight polymers is not economically feasible, it is much cheaper to dilute high molecular weight ones. The result will be the same.

I don't use gasoline, as I mix it with my hands, like kneading dough, and then roll it out with a rolling pin. And I don't use oil, because I think that would make it really snotty.

Right now, to illustrate my words with a photo, I decided to make a small sample of plastic. But I took an old tube of glue. And this time, the same PETN came out with a normal plastic explosive. Much harder, requiring a strong hand pressure for molding. I measured the density, it came out 1.56.

Apparently, I got a defect. And the new mouse glue is apparently too liquid.

In any case, I now have to either check the glue after purchase, or try to heat it so that all the volatile from it evaporated ....

I still want to put a second coarse fraction of crystals into the plastic. But the problem is that the crystals in it are 0.25-0.5mm. I'm afraid that such large crystals can trivially not detonate.....

[Edited on 1-12-2023 by DennyDevHE77]

MineMan - 3-12-2023 at 23:41

Quote: Originally posted by DennyDevHE77  
I use mouse glue as a source of polymers. Its composition is polybutylene - 80.83% , polyisobutylene - 9.60% , cyclosan - 9.57%. What the latter is, is not clear, perhaps they are low molecular weight polymers, or a trade name for a crosslinker.... But I think it is just low molecular weight polymers to give the finished product (glue), more liquid consistency. Or maybe it's really some kind of oil with sebacic/phthalic acid esters. As far as I understand, production of low molecular weight polymers is not economically feasible, it is much cheaper to dilute high molecular weight ones. The result will be the same.

I don't use gasoline, as I mix it with my hands, like kneading dough, and then roll it out with a rolling pin. And I don't use oil, because I think that would make it really snotty.

Right now, to illustrate my words with a photo, I decided to make a small sample of plastic. But I took an old tube of glue. And this time, the same PETN came out with a normal plastic explosive. Much harder, requiring a strong hand pressure for molding. I measured the density, it came out 1.56.

Apparently, I got a defect. And the new mouse glue is apparently too liquid.

In any case, I now have to either check the glue after purchase, or try to heat it so that all the volatile from it evaporated ....

I still want to put a second coarse fraction of crystals into the plastic. But the problem is that the crystals in it are 0.25-0.5mm. I'm afraid that such large crystals can trivially not detonate.....

[Edited on 1-12-2023 by DennyDevHE77]


I don’t know.

dettoo456 - 6-12-2023 at 11:37

If the material is acting like kinetic sand you probably have too low viscosity/too much liquid-like material instead of rubbery solids in your mix. Also, dropping the particle size will probably help to make your PBX more malleable as it’ll increase the surface area on which the binder (PIB rubber) can adhere to. High MW PIB can be hard to find, especially in consumer products and the rat glue probably isn’t even high enough MW. One source of PIB that I found might work is the glue/adhesive tape on steel drum (like 40 or 55 gal) lids. It’s used to hold the rubber gasket/seal to the lid. If you pull the gasket off you should be able to see it.

C4 used to use EXXON Vistanex which has a really high MW - even higher than any BASF PIB. The PBX mainly relies on high MW rubber loadings with mineral oil (or some low viscosity PIB) and DOS to give malleability.

dettoo456 - 11-12-2023 at 11:36

Quote: Originally posted by dettoo456  
If the material is acting like kinetic sand you probably have too low viscosity/too much liquid-like material instead of rubbery solids in your mix. Also, dropping the particle size will probably help to make your PBX more malleable as it’ll increase the surface area on which the binder (PIB rubber) can adhere to. High MW PIB can be hard to find, especially in consumer products and the rat glue probably isn’t even high enough MW. One source of PIB that I found might work is the glue/adhesive tape on steel drum (like 40 or 55 gal) lids. It’s used to hold the rubber gasket/seal to the lid. If you pull the gasket off you should be able to see it.

C4 used to use EXXON Vistanex which has a really high MW - even higher than any BASF PIB. The PBX mainly relies on high MW rubber loadings with mineral oil (or some low viscosity PIB) and DOS to give malleability.


Pardon my earlier post, the adhesive used to hold gaskets in 55gal drums is actually likely Styrene-butadiene. The styrene-butadiene itself can still be used in PBXs though, it just needs a suitable solvent.

MineMan - 12-12-2023 at 01:04

I thought silicone worked well? Wesson smith used it

dettoo456 - 12-12-2023 at 13:10

I believe Wesson smith used HTPB and/or lithium grease in his formulations but he may have mentioned silicone before. Silicone can be used but it will cure and you’ll be left with a rubbery puck instead of a plastic material. Also, the issue with lithium grease is that it doesn’t have any tack/binding ability, only plasticizing ability.

Styrene, HTPB, PIB, Viton, and even something like asphalt are the only real choices for a good PBX since they provide both plasticizing and binding ability on their own (high MW polymers need an oil though - to lower viscosity).

DennyDevHE77 - 1-1-2024 at 07:21

Do you think it is possible to grind PETN in a coffee grinder as follows. Mix PETN and, for example, sugar in a ratio of 20 to 80. We grind it in several steps (as the mixture gets noticeably warm when grinding for a long time), and then just dissolve it in hot water, all the sugar goes into the water, and the PETN is filtered out.

Do you think such a mixture can detonate at all?

If anyone has played with PETN like this before, please write back (you survived, right?).

dettoo456 - 1-1-2024 at 11:30

Don’t blend any explosive in a coffee grinder. Insensitive oxidizers and fuels (kept separate of course) can be ground; i.e. KNO3 or Al. If anything, a slurry of PETN in water may be run in a ball mill at low speeds but definitely not a coffee grinder. PETN may release oxygen and other nitrogen oxides at higher temperatures when being physically broken down, these can oxidize the reducing sugar and potentially cause a deflagration or detonation. Not to mention, if the seal between the cutting blade and the inside of the grinder isn’t tight enough, some powder may fall in and make direct contact with the grinder’s motor and internal circuit, potentially causing a fire, and/or a detonation from DDT.

PETN crashed out via the anti-solvent method (Acetone or alcohol into water) should yield plenty small enough crystals. If that doesn’t work, try to buy a TLC sprayer and spray a solution of PETN onto a cooled sheet of something like PTFE, then carefully scrape off the dried powder.

Plenty of methods to yield small particle EMs exist, but the mechanophysical methods are usually the least safe.

[Edited on 1-1-2024 by dettoo456]

Laboratory of Liptakov - 2-1-2024 at 01:38

dettoo has truth....Methode acetone or alcohol / water provide plenty small crystals itself (agglomerates) . Maybe you can use stainless sieve 1x1 mm. For bigger parts. In water bath you can PETN slowly crushed thru sieve under water level.....:cool:

DennyDevHE77 - 5-1-2024 at 05:07

Thanks for your previous replies, I still don't think petn would explode at a 20 to 80 ratio, but the fact that it could start decomposing doesn't make me happy, because that's a loss of yield.

But here the following question has arisen, how to make up optimal ratios of nitric acid (57%) and phosphorus pentaoxide for distillation? It would seem that it is not easier, just take the molar ratios of the reaction. But this way is obviously not optimal, because during distillation pyro and meta phosphoric acids will be formed, which pull water even stronger than sulfuric acid, so in the end the amount of phosphorus pentaoxide can probably be significantly reduced. But I have no idea how to calculate that.

dettoo456 - 5-1-2024 at 15:30

P2O5 will dehydrate HNO3 all the way to N2O5, which isn’t even needed for PETN or any other aliphatic nitrate ester. You can use either WFNA or NH4NO3/H2SO4 for PETN and you won’t need to waste P2O5.

Metaphosphoric acid (obtained from aggressively heating H3PO4 at around 500C until white fumes are emitted and a gel is left over) can dehydrate H2SO4 to SO3/H2SO4 but I haven’t seen the same reaction demonstrated with HNO3 -> N2O5/HNO3. You can try to do this, but IMO it’s a waste if you have access to nitrate salts, H2SO4, and/or 69% HNO3. The Metaphosphoric acid dehydration pathway is only useful if you have already high concentration mineral acids and need close-to-anhydrous acids; which most people don’t. Plus, if you can get P2O5 for cheap, you’d likely be able to find NH4NO3 as well, and that’s much more useful in EM synthesis.

DennyDevHE77 - 6-1-2024 at 01:09

Well, I have access to NH4NO3, but I use it most often as a component of mixed explosives. Sulfuric acid is relatively cheap to me, but it is sold sub-accountably. Phosphorus pentaoxide, like nitric acid (58-70%) is sold absolutely freely, although P2O5 is three times more expensive than sulfuric acid. Of course, if I could get tens of liters of sulfuric acid, I would not ask myself this question, but I can only get tens of kilograms of phosphorus pentaoxide, and sulfuric acid is more limited for me.

Yes, P2O5 dehydrates nitric acid to N2O5, but only anhydrous, if it is an azeotrope (68%) then water will be removed first, either directly or the resulting N2O5 will react with water.

DennyDevHE77 - 8-1-2024 at 11:55

Guys, could someone please point me to the critical diameters of cast ETN, TNT, and picric acid? I found only for TNT, and that, in different sources it is indicated from 25 to 40 mm.

OneEyedPyro - 13-1-2024 at 07:44

Quote: Originally posted by DennyDevHE77  
Guys, could someone please point me to the critical diameters of cast ETN, TNT, and picric acid? I found only for TNT, and that, in different sources it is indicated from 25 to 40 mm.


ETN is 8 to 10mm depending on who you ask. I can't really say about TNP but given its higher power and sensitivity I'd guess lower than TNT. I remember seeing a diagram where pressed picric acid was used as a booster in impact fuse assemblies for small mortars by some country back in WWII (France maybe?). In any case, the diagram showed the booster portion being relatively small in diameter, maybe 20mm.

DennyDevHE77 - 28-1-2024 at 20:19

Quote: Originally posted by OneEyedPyro  
ETN is 8 to 10mm


I'm a little surprised. pentolite (50% PETN, 50% TNT) has a critical diameter of 6.7 mm. On the other hand, pentolite is not homogeneous in its consistency, so maybe this has an effect.

Sir_Gawain - 29-1-2024 at 16:32

Small irregularities such as bubbles and cracks greatly increase the sensitivity of an explosive. Also, my EBW detonators have a 6.4 mm ID with pure ETN, and they definitely go high order.

OneEyedPyro - 30-1-2024 at 14:22

Quote: Originally posted by Sir_Gawain  
Small irregularities such as bubbles and cracks greatly increase the sensitivity of an explosive. Also, my EBW detonators have a 6.4 mm ID with pure ETN, and they definitely go high order.


I've made little caps with pressed ETN and SADS in those stirring straws you get with coffee or at a bar with mixed drinks. They're maybe what, 2.5mm inner diameter? Too small for a standard visco fuse to fit inside.
I still got a full detonation every time, but I only made several. Had I tried dozens I'm sure some would have failed. Had the straw been 20 meters long instead of 2cm long the detonation would have certainly fizzled out before reaching the end.

ManyInterests - 12-3-2024 at 14:01

I have a question about storing liquid explosives such as nitroglycerine, ethylene glycol dinitrate, propylene glycol dinitrate, and diethylene glycol dinitrate.

Is it safe to store such material in PET bottles? The same bottles that water and soda is stored in? I plan on makying DEGDN since it is safer to handle than NG and also even less volatile (from Urbanski's books), but is hygroscopic, so drying it and storing it to stop any moisture absorption will mean I will need to stop it in a semi-open bottle in another container. Does it need glass or will any plastic suffice?

dettoo456 - 12-3-2024 at 14:51

I definitely wouldn’t store in glass, simply due to the risk of shrapnel in a DDT situation (though rare). If you dissolve it in something like DCM though, glass might be alright as long as you vent it every once in a while.

If you store pure, HDPE should work. It is pretty much the standard for storing dry EMs and would likely be fine with liquids. I couldn’t find much info relating to storing EGDN, but, on page 7 of the attached doc, the author mentions potential issues of HDPE relating to interactions of nitrate esters w/plasticizers.

https://apps.dtic.mil/sti/tr/pdf/AD0778207.pdf

I’d test at small scale before storing anything >1g, just in case.

ManyInterests - 12-3-2024 at 20:24

I never intend to store anything but pure. But if storage is an issue, then I will make as needed.

underground - 27-3-2024 at 10:19

Does Calcium Cyanate (CaOH and Urea reaction) and Hydrazine Sulphate produce semicarbazide ?

[Edited on 28-3-2024 by underground]

Nemo_Tenetur - 2-4-2024 at 06:57

Anyone here with carbodihydrazide synthesis experience? I require a larger quantity as precursor for different energetic materials and I don´t want to buy it because I´m a cheapskate. Fisher scientific sell it for 450 Euro per 500 gram, that´s a ripp off.

There are different routes, phosgene as precursor is out of question. Cyanuric acid and Propylene carbonate are mentioned in patents as better yielding and purer product than urea, but the latter is unbeatable cheap (about 100 euro / 50 euro per kilo versus less than 2 euro per kilo for fertilizer grade).

The yield ist not decisive for me, but the purity (or more precise, the ease of purification) of the final product. The available information is pretty sparse about purity and purification with respect to the different routes. So input and comments about the different routes are welcome. I have enough glassware, fume hood, two stage vacuum pump etc. and 80% hydrazine hydrate in stock.

dettoo456 - 2-4-2024 at 07:25

The propylene carbonate route may yield propyl carbazate impurities, so an excess of N2H4 and long rxn time would be required. But I’d say that’d be easiest method. Dry Hydrazine Sulfate & NaOH can be refluxed in n-propanol or isopropanol to extract the Hydrazine, then that propanol solution can be decanted and refluxed with propylene carbonate while distilling off the excess solvent. I haven’t heard of the cyanuric acid route though.

I also know a Russian supplier who has carbohydrazide for 2400₽/kg, but I don’t know how sanctions are where you live, and their payment provider isn’t very secure. I’ve had to cancel a debit card due to fraud payments after a purchase from them in the past, even though my order arrived fine to me in the US - it was Red P that cleared customs too :D . I’ll send the info via U2U if you’re interested.

Nemo_Tenetur - 2-4-2024 at 09:22

Thank you for fast reply and information. There are plenty sanctions here in the EU and try to import something from Russia at present time is like asking for trouble, at least will raise a big red flag.

Additionaly, there are so much overhead costs and paperwork associated with such a transaction that I´ll avoid it whenever possible. About 20 years ago I´ve bought an exotic amine from TCI in Japan. I´ve paid additional 550 Euro for air freight, tax, hazmat fee, ATLAS fee etc.

underground - 2-4-2024 at 13:13

Quote: Originally posted by Nemo_Tenetur  
Anyone here with carbodihydrazide synthesis experience? I require a larger quantity as precursor for different energetic materials and I don´t want to buy it because I´m a cheapskate.


What do you have into your mind. You can buy it from ali for a relative good price

Nemo_Tenetur - 4-4-2024 at 14:05

I have no experience with ali (baba or express?) and I´m not sure if such a parcel with white powder (hazmat) will raise a red flag at the EU border. Do they ship in compliance with dangerous goods regulations?

Trashcanman - 4-4-2024 at 15:09

Quote: Originally posted by Nemo_Tenetur  
I have no experience with ali (baba or express?) and I´m not sure if such a parcel with white powder (hazmat) will raise a red flag at the EU border. Do they ship in compliance with dangerous goods regulations?


A few years ago I bought 3 americium ionization chambers from aliexpress.
Those things have radiation warnings on them and I think those packages were opened after crossing the EU border because the packages looked as if someone cut them open and sealed them again. I don't know what will happen if some overmotivated customs officer opens a parcel with white powder that was sent from china xD.

But that's just my two cents :)

Yorty2040 - 15-4-2024 at 17:47

What adhesives resist 95% NM/5% Ethylenediamine PLX?

dettoo456 - 15-4-2024 at 20:14

What do you mean by adhesives? Are you trying to gelatinize PLX with a polymer? If so, that might cause some issues since NM could simply dissolve a wide range of polymers and ethylenediamine is a fairly aggressive base that could attack esters & olefins.

Yorty2040 - 15-4-2024 at 21:16

I might need to glue the blasting cap in place, and need a glue that can withstand contact with PLX. If there is no such glue, I'll need to get creative with solder, which will present its own issues.

dettoo456 - 16-4-2024 at 11:25

Sorry, I don’t think there’d be a clear answer to that query.

You’ll probably just need to test on a small scale to figure out the best glue or somehow mount a fitting with plastic screws to hold a detonator in place.

dettoo456 - 16-4-2024 at 11:28

This inert version of a binary mix (https://inertproducts.com/product/texpak-binary-explosive-se...) uses a custom molded case to partially surround the detonator.

So you might be able to just tape your cap directly to the bottle of PLX and achieve full detonation.

Yorty2040 - 29-4-2024 at 17:37

Has anyone done any work on the nitration of hydantoin? The dinitramine looks like it might make an interesting energetic.

There are papers about the use of 5,5-dimethyl dinitrohydantoin as a nitration agent for arenes, but the synthesis involves the use of triflic anhydride, which is a bit pricey.

I reckon that the nitrate salt of hydantoin, plus acetic anhydride, ammonium nitrate, and fuming nitric acid, might form the dinitramine, but I can't find any references for the dinitration of unsubstituted hydantoin.

dettoo456 - 30-4-2024 at 07:47

Mononitration at the 1 position likely wouldn’t be too difficult but the dinitration would definitely prove harder due to how bulky those carbonyls are. And the product (either mono or dinitramine) probably wouldn’t be too stable. Nitrourea compounds and related nitroamides are not known for their fantastic hydrolytic stability; they tend to hydrolyze very quickly even at rt and in neutral conditions. Plus, pure hydantoin isn’t very commercially available. BCDMH is, but it’s still expensive on its own. And Ac2O is hard to get as well.

A better use for hydantoin could be through di-oxidation (if possible) and subsequent oxidation to just the dinitroimidazolidine. But hydroxylamine is expensive too.

Yorty2040 - 30-4-2024 at 13:36

I think hydantoin can be made from glycine hydrochloride and potassium cyanate, via the Urech hydantoin synthesis. But if the product of the dinitration hydrolyzes rapidly in water that would be a problem. Do you think MeCl2 could extract the product from the nitration mixture?

dettoo456 - 1-5-2024 at 17:20

DCM will dissolve nitric acid very readily, though I don’t know how soluble the hydantoin is in DCM either. And it’s not that it might hydrolyze in a water solution, but likely in trace amounts of water and/or acid. It doesn’t seem like a very good EM candidate from a price, stability, or ease of manufacturing perspective.


dettoo456 - 9-5-2024 at 07:13

Although there doesn’t seem to be much info on it, the detonation velocity (from the few sources I’ve seen) of TEGDN is around 2000m/s. This seems extremely low considering that EGDN is 6600m/s and DEGDN shouldn’t be much lower than that.

Does anyone know why TEGDN is apparently so weak? Apart from its low OB%, it doesn’t make sense to me.

https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8154001/

clearly_not_atara - 9-5-2024 at 10:08

Extending the oxyethylene chain not only decreases the oxygen balance but also the density.

dettoo456 - 15-5-2024 at 07:39

Has anyone noticed some papers describing odd synthesis methods for EMs? The paper linked below describes using a 1:1 molar ratio of AN to Erythritol in an excess of H2SO4 to prepare ETN, but there should be at least a 4:1 ratio of AN to Erythritol, to properly convert all of the AN to HNO3 in-situ and all hydroxyl groups to nitrates, correct?

[Edited on 15-5-2024 by dettoo456]

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[Edited on 15-5-2024 by dettoo456]

Yorty2040 - 17-5-2024 at 09:05

Anybody have a good synthesis of 2-imidazolidinone? The wiki says ethylene glycol and urea, but it doesn't say how it's done. Is it as simple as mixing them and boiling off the water, or is an acidic or basic catalyst required?

Most of the literature is for the ethylenediamine+ethyl carbonate procedure, which is less accessible to the amateur.

EF2000 - 17-5-2024 at 09:30

Quote: Originally posted by Yorty2040  
Anybody have a good synthesis of 2-imidazolidinone? The wiki says ethylene glycol and urea, but it doesn't say how it's done. Is it as simple as mixing them and boiling off the water, or is an acidic or basic catalyst required?

Most of the literature is for the ethylenediamine+ethyl carbonate procedure, which is less accessible to the amateur.

2-imidazolidinone is also called 1,3-ethyleneurea, right? So, it appear that this article is what you are looking for: Ethyleneurea. II. Syntheses From Ethylene Glycol or Ethanolamine and Urea (or Carbon Dioxide and Ammonia) by Carl E. Schweitzer.

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Yorty2040 - 17-5-2024 at 18:03

Thank you! Unfortunately that synth looks like a PITA with the high pressures and temperatures, but it's still a good find.

BTW, is ammonium hydroxide basic enough to deprotonate ethylenedinitramine and form a salt, or will only alkaline metals do? I can't find a good literature value for EDNA's pKa in water or I'd answer myself.

[Edited on 18-5-2024 by Yorty2040]

Yorty2040 - 20-5-2024 at 08:47

Does anyone have any knowledge of nickel (bis-ethylenedinitramine) diperchlorate?

dettoo456 - 20-5-2024 at 09:00

Didn’t read it fully, but this may help:



[Edited on 20-5-2024 by dettoo456]

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Yorty2040 - 20-5-2024 at 11:42

So it seems a bis compound isn't possible with nickel, at least via simple methods.

Yorty2040 - 24-5-2024 at 17:40

Does anyone have any information on melamine diperchlorate? Solubility, handling, decomposition temp, sensitivity, shelf life, etc?

Precipitates - 24-5-2024 at 20:43

Quote: Originally posted by Yorty2040  
Does anyone have any information on melamine diperchlorate? Solubility, handling, decomposition temp, sensitivity, shelf life, etc?


I could only really find this article on Melamine Diperchlorate Hydrate.

I assume reasonable solubility, not ridiculously sensitive and relatively stable.

[Edited on 25-5-2024 by Precipitates]

dettoo456 - 28-5-2024 at 08:08

Has anyone carried out a destructive nitration procedure on a ketone before? I couldn’t find much information on them; it seems Russian chemists were messing around with the principles and kinetics in the mid 90s, but those journal entries are very hard to find, let alone translate.

As far as I can tell, it’s basically the same conditions as for the preparation of Nitroform from Acetone (or from the dehydration of IPA and subsequent nitration). Carbonyls, mainly ketones but apparently carboxylic acids as well, undergo decarboxylative nitration to yield the trinitromethyl or dinitromethyl derivative at the alpha position relative to the carbonyl.

This polynitromethyl product though, can be generated by the action of WFNA/H2SO4 with the ketone at 0C, and Hexanitroethane can even be prepared like this in up to a 75% yield from the terminal-trinitro ketone (authors reported using trinitropentanone, though I believe this was a mistake, and trinitrobutanone might have been used instead).

https://www.researchgate.net/publication/250556009_ChemInfor...

This abstract does not provide much insight as to the conditions (molar equivalent, addition rate, extraction), and I couldn’t find the article in the Russian Org Chem journal.

In short, is it plausible that this reaction could be applied to something like MEK, to yield 1,1,1-trinitroethane?

Yorty2040 - 14-6-2024 at 17:44

So methazonic acid (2-nitroacetaldoxime) can be produced by the base-catalyzed self-condensation of nitromethane, followed by acid workup.

Is there any info on using sodium perborate + glacial AcOH to convert it to 1,2-dinitroethane? The procedure should work, but the devil (and yield) is in the details of the procedure and subsequent workup.

dettoo456 - 14-6-2024 at 20:14

I’m assuming you’re referencing this paper (linked below) for the oxidation with perborate. As you mentioned though, the preparation will suffer in yields with the scope being so wide (small chain aldoxime already with a nitro substitutient compared to mainly aryl ketoximes reported being used).

A more sketchy method to yield 1,1,2-TRInitroethane could be the ponzio reaction; NO2 or N2O4 in ether or a suitable polar nonprotic at low temperature).

Or, some other, cleaner oxidizer like oxone or H2O2. Though, in any case, including the Perborate/GAA method, oxidation of the aldehyde to carboxylic acid and oxime to carbonyl is probably the reason for such low reported yields.

[Edited on 15-6-2024 by dettoo456]

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Yorty2040 - 17-6-2024 at 16:22

What's the technical, physicochemical explanation for why complexing the oxoacid salt of a nitrogenous base with a transition metal typically increases sensitivity compared to the uncomplexated salt?

[Edited on 18-6-2024 by Yorty2040]

dettoo456 - 23-6-2024 at 13:44

The acidity of the acid itself may contribute to instability (the free H+). Or, since the main decomposition pathway of energetics is based on BDEs (bond disassociation energies) of different groups and bonds on a molecule, if the oxoacid has a lower BDE than other groups in the complex (ionic bonds between the metal and anion), it could kickstart a decomposition process. C, O, and N intermediates may also simply be easier for a group like ClO4-, NO3-, etc to oxidize than the metal itself too. OB% factors in to this as well, along with perhaps higher densities of the materials due to packing of the nitrogenous oxoacids in the complex’s lattice; such higher densities can affect sensitivity too.

Fluorite - 30-6-2024 at 05:24

Can hexamine undergo hydrolysis with sodium hydroxide to form sodium formate, ammonia and methanol?

dettoo456 - 3-7-2024 at 17:56

It’d likely form ammonia (or more likely urea) and formaldehyde (the formaldehyde quickly decomposing to formate), in a reverse reaction to the manner in which hexamine itself is prepared.

A controlled hydrolysis may yield (mono, di, or tri)methylamine.

I doubt the conditions would be anywhere close to reducing enough to reduce formaldehyde or formate to methanol.

[Edited on 4-7-2024 by dettoo456]

solo - 4-7-2024 at 16:03

..how to mono aminate 1,5-Dibromopentane....solo


dettoo456 - 16-7-2024 at 17:16

Explosion welding/cladding is usually carried out on thin metal sheeting (no greater than 1” or 25mm) with minimal explosive used per sq in (<50g in most cases, and low power EMs like ANFO at that).

Would there be any way to feasibly weld 2” (50mm) or thicker mild steel with much larger quantities of explosive or higher VoD explosives?

As the size of the EM charge itself is increased, I’d assume a kicker charge design might be able to increase the total energy transferred to the witness plate from the flyer plate. But as the EM performance rises, and brisance along with it, I’d be worried about the flyer plate just being shattered or shock hardening to the point that it’d be too brittle to weld to the witness.

For context, I have lot of thick steel bar scrap and am too cheap to buy an anvil.

UndermineBriarEverglade - 30-7-2024 at 11:01

Do I need to purify monkfruit sweetener for use in ETN? I'm not able to buy pure erythritol online or find it locally. I have Lankato brand, ingredients erythritol and "monk fruit extract" (mogrosides). They don't publish an exact percent, but their website says that monkfruit is 200x as sweet as sugar and erythritol is 70% as sweet. For the mix to match sugar, this would imply 99.6% erythritol. 1.5g of crud per pound of sweetener.

If I want to avoid nitrating mogroside V, how do I get it out? Can't find solubility figures for it.

[Edited on 2024-7-30 by UndermineBriarEverglade]

Laboratory of Liptakov - 30-7-2024 at 21:53

If I were faced with the same question, I would do the nitration of 2g Lankato as is. The behavior and returns of ETNs are very well known. I would determine the usability of Lankato based on the differences in the behavior of the final product. Yes or no....:cool:.....Only my opinion, not more.

dettoo456 - 1-8-2024 at 11:42

Most food grade erythritol is pure enough for direct nitration. If the ingredients are just “Erythritol” then you’ll be fine. The small impurities are likely silica dust or some other agent to prevent clumping and/or hygroscopicity.

UndermineBriarEverglade - 1-8-2024 at 12:59

LL, I am considering it. I would like to store the ETN and I'm nervous about impurities causing deterioration. Easier to test immediate sensitivity characteristics. dettoo, the second ingredient is "monk fruit extract". Unfortunately I can't find food grade erythritol in my region and I'm not able to purchase it online.

Now that I think of it, one more simple question. ETN becomes much more sensitive over the melting point, so you must be extremely careful when meltcasting. When recrystallizing ETN, so putting it in solution but it's below 61C, do I need to take the same level of precaution?

dettoo456 - 2-8-2024 at 08:23

ETN in solution (Acetone, IPA, and/or EtOH) at the solvents’ bp can be dangerous if spilled on a hot surface - which is why a water bath is recommended. Though it isn’t nearly as sensitive to shock, friction, etc. as the pure melted ETN.

Monk fruit extract in and of itself shouldn’t present any problems in nitration. It is primarily erythritol stereoisomers with small impurities of other polyols, so no real concern is warranted IMO.

UndermineBriarEverglade - 4-8-2024 at 20:40

Nitrated 9g of "Lankato". Unfortunately I got <35% yield (ETN is still damp). More simple questions:


Sir_Gawain - 4-8-2024 at 21:31

Quote: Originally posted by UndermineBriarEverglade  
Do US hardware stores carry methanol anymore? Are there options besides small HEET bottles?

Methanol can be distilled from windshield wiper fluid. Usually the lower the temperature rating, the more methanol. Also, most “denatured alcohol” is about 50/50 ethanol/methanol which can easily be separated by distillation.

Laboratory of Liptakov - 4-8-2024 at 22:35

If you have yield 5g final pure dry ETN (from recrystallization proces), is it pretty good yield. If you used method H2SO4 + KNO3 + 9g Lankato......:cool:
With pure reagents HNO3 / H2SO4 is yield usually 18g from pure 9g E.

charley1957 - 5-8-2024 at 03:26

I just ordered methanol from Amazon. I’m using it as a solvent for the extraction of a plant alkaloid. It came in 1L plastic containers. I think I got 8 of them. Price wasn’t too bad IIRC.

greenlight - 7-8-2024 at 08:10