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Sir_Gawain
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1. I’ve done this reaction before, although with ammonium nitrate instead of potassium nitrate. It’s not very exothermic and is pretty straight
forward and safe. I didn’t get a very high yield though.
2. Urea nitrate can be detonated on its own, but I would suggest mixing with ammonium nitrate to make an oxygen balanced explosive. I’ve tested this
mixture, and it’s cap sensitive and fairly powerful.
3. While nitrourea is said to be more powerful, I’ve heard it has poor stability. Nitroguanidine is more powerful and stable.
4. I don’t know.
5. I successfully detonated a charge of AN/UN with a diameter of 1cm.
6. Urea nitrate is very insensitive, don’t know about nitrourea.
If you’re trying to make shaped charges, pure urea nitrate is not a good choice. It has a low detonation velocity. A mixture of urea nitrate and ETN
could work. You wouldn’t have to make nearly as much ETN.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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UndermineBriarEverglade
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Unfortunately I can't buy AN or high-% ammonia. I could produce AN from KNO3 but I'd first need to buy condensing equipment for ammonia. Path to NQ is
long from where I am.
Mixing is a good idea but I think it'd take too much ETN. I calculated
ETN 302.1 g/mol
C4H6N4O12→(4 CO2 + 3 H2O + N2 + 3/2 O2) 3 oxygen provided per mol
urea nitrate 123.06 g/mol
CH5N3O4→CO2 + N2 + 1/2 N2 + 2 H2O + H) 1/2 oxygen needed per mol
nitrourea 105.05324 g/mol
H2NC(O)NH(NO2) → (H2O + CO2 + N2 + 1/2 N + H) 1/2 oxygen needed per mol
nitroguanidine 104.068 g/mol
(CH4N4O2 → CO2 + 2N2 + 2 H2[O]) 2 oxygen needed per mol
So for an oxygen-balanced 100g charge:
29g ETN + 71g urea nitrate
32.4 ETN + 67.6g nitrourea
66g ETN + 34g NQ
If my math is right a 2kg charge with ETN/UN would be 580g of ETN. Although the mix would be safe to handle I don't want to manufacture such
quantities of ETN. If UN must be mixed I'd rather use a cheap oxidizer. Don't want to waste my KNO3 but I wonder what calcium sulfate would do?
I think strong confinement might be able to make working shaped charges from low VOD explosive.
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Sir_Gawain
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ETN only produces 1 oxygen per mole, not 3.
(C4H6N4O12 > 4CO2 + 3H2O + 2N2 + 1/2O2)
I highly doubt adding any calcium sulfate to an explosive composition would increase performance - it’s far too unreactive. Even if it did manage to
take part in the detonation reaction, the solid byproducts would dampen the energy significantly.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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UndermineBriarEverglade
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Equation contaminated by atmospheric O2!  In that case the situation is even
bleaker, 2 moles urea nitrate per 1 mole ETN to be oxygen balanced.
I grabbed off a list of pyrotechnic oxidizers, looking for easy-to-obtain chemicals. Tichapondwa 2015 uses it to replace barium sulfate in
slow-burning delay compositions, which is about the opposite of an explosion. I guess a more reactive oxidizer is in order. I may need to find a
fertilizer source of KNO3, stump remover is pricey.
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dettoo456
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NQ is far and away the best option for mixing with ETN, as it’s very powerful on its own, insensitive, and very stable. The only issue is obtaining
the right crystal morphology to select for small particle size and rounded crystal shape. Even so, UN is just too weak and finnicky IMO.
If you’re not comfortable answering, don’t feel you need to, but are you in the US? If so, pyrochemsource still offers GN cheaply (a cheaper
alternative than making your own if you’re doing small scale work). Then, just dehydrate with conc H2SO4, regenerate the spent acid, and then repeat
the process.
Also, a shaped charge with a cone angle <90ish degrees WILL require a high performing EM with uniform density and initiation to perform correctly.
If you are considering using ETN mixes instead of pure ETN, I’d recommend just looking at EFPs - easier to produce, much more forgiving in use with
weaker EMs, and performs on-par with amateur made shaped charges.
To give some ideas on how to optimize performance based on different materials and charge designs: https://apps.dtic.mil/sti/pdfs/ADA419413.pdf
[Edited on 22-8-2024 by dettoo456]
[Edited on 22-8-2024 by dettoo456]
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UndermineBriarEverglade
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Thanks dettoo, I'll do more research into EFPs. Curious what determines the amount of "curve" of the parabolic? liners I see in videos.
(NH2)2CO + KNO3 + HCl -> CH5N3O4 + KCl
So what about using this KCl byproduct with bleach to make potassium chlorate, to mix with UN? (Maybe not NU, highly reactive with S traces from
dehydration.) It would be oxygen balanced at 14:86 ratio. Wonder if it would be too sensitive.
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UndermineBriarEverglade
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Think I'm not going to do potassium chlorate, probably too sensitive. Potassium perchlorate possibly, but it's additional trouble to make. KCl from UN
reaction is better off poured down the drain, it's easier to buy food-grade KCl. I might just mix ETN and UN for EFPs so that I can get on with it.
I tried melt-casting a 10g cylinder of ETN but it's full of bubbles. Obviously I don't want to knock liquid ETN around to get the bubbles out. Has
anybody made a vacuum chamber for melt-casting?
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dettoo456
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I believe the vacuum casting has been brought up before but I can’t remember what was discussed regarding design or implementation.
In any case, you’d need plastic to avoid shrapnel (just in case). I’d say those glass dessicators could work too, but they have really thick glass
which would act as a strong thermal mass, and whenever melt casting, you’ll want your heating vessel to be able to dissipate heat quickly in case of
a thermal runaway.
On top of that, you might run into issues using water as a heating fluid with its higher vapor pressure. A light oil could be better.
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Bender84
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Is dry PETN prone to static charge accumulation due to e.g. triboelectric effect? Is it a standard practice to wash it with an anti-static agent
before drying? I'm asking this in the context of detonating cords production process. Thanks in advance.
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UndermineBriarEverglade
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Urea nitrate
Made some urea nitrate. When stored at room temp it gave off acid fumes and seemed permanently damp. I thought it was supposed to be storage stable
and non-hygroscopic. How do you guys dry and recrystallize it?
I pressed 20g of crystals into a 16mm tall / 36mm wide plastic cylinder (approx 1.3 g/cm3 after cap intrusion) and attempted to detonate
from above with a 400mg ETN cap. Incomplete or no detonation occurred. The sides and lid of the cylinder were destroyed but the bottom face was
practically unharmed and some clumps of urea nitrate remained on it. What happened?
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Sir_Gawain
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Did you wash it with alcohol?
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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UndermineBriarEverglade
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No. I was fooled by the wiki which has the wrong value for ethanol solubility. With pure and dry product, would it have detonated in that arrangement?
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Sir_Gawain
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Urea nitrate isn’t very sensitive, but I would expect it to detonate under those conditions. Maybe try adding a sensitizer, like ETN.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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UndermineBriarEverglade
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Thanks. I'll probably repeat the experiment with better UN.
One more set of questions. I'm thinking about giving up on UN and its derivatives and using ETN as primary charges. I see that you can make a PBX with
styrofoam+acetone, and that ETN can be melt-cast with nitrocellulose.
Instead of melting, could I dissolve ETN and NC in acetone and then let the mix dry? Seems safer than molten ETN, enough do it
under vacuum to remove bubbles.
What are the properties of ETN+NC? Is it more or less sensitive than ETN?
How about polystyrene mixes?
I've also got DBSP. Dangerously sensitive over pure NC lacquer?
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underground
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ATO (aminotriazolone)
Will carbohydrazine and formic acid form aminotriazolone (ATO) just like semicarbazide with formic acid form triazolone ? I am not a chemist so i am
not really sure
Edit: From this paper ATO is made from carbohydrazide and triethyl orthoformate
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The ATO used in this work was prepared as follows. Appropriate quantities of triethyl orthoformate (20 ml) and carbohydrazide (25 g) in aqueous
solution were put into a reaction bulb and stirred at 60–85 °C for 3 h. The water and the by-product ethanol were distilled off and the white
precipitate was collected by filtration. The precipitate was washed thoroughly with ethanol and vacuum dried.
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Triethyl orthoformate from wiki
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Triethyl orthoformate is an organic compound with the formula HC(OC2H5)3. This colorless volatile liquid, the ortho ester of formic acid, is
commercially available.
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So my question is if just formic acid can be used instead of Triethyl orthoformate, just like the triazolone synthesis.
[Edited on 25-9-2024 by underground]
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dettoo456
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I believe the terminal amines would be more reactive and the end product would either be a pseudo-polymeric, nitrogenous chain of carbohydrazide with
methyl linkages, or just 1,2,4,5-tetrazine-3-one. The tetrazine though, is most often prepared with a much stronger formylating agent like Diphosgene
or CDI.
So I can’t give a specific answer, but I don’t think the triazole’s formation would be very likely.
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underground
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Quote: Originally posted by dettoo456  | I believe the terminal amines would be more reactive and the end product would either be a pseudo-polymeric, nitrogenous chain of carbohydrazide with
methyl linkages, or just 1,2,4,5-tetrazine-3-one. The tetrazine though, is most often prepared with a much stronger formylating agent like Diphosgene
or CDI.
So I can’t give a specific answer, but I don’t think the triazole’s formation would be very likely.
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According to the attached file, carbohydrazide cyclocondensate with aldehydes to form tetrazine
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Firstly, thiocarbohydrazide (1) was prepared as shown in
equation (1) and Scheme (1)[18] in good yield (76 %)
[15]. This compound gave three special absorption bands
in FT-IR spectra at 3306, (3274 and 3203) and 1282 cm-1
refered to three functional groups NH2, NH and C=S
respectively in addition to the N-N functional group at
1489 cm-1 and C-N functional group at 1384 cm-1. While
in U.V spectra it gave two types of electronic transition
represented by n→π* and π→π* at (355 & 272 nm
)respectively [19].Thiocarbohydrazide (1) used as a
good precursor to form symmetrical tatrazine represented
by compounds 6-aryl1,2,4,5-tetrahydro tetrazine-3-thione
compounds (2-6) through cyclocondensation reaction with
substituted benzaldehyde in acidic media , and these compounds
were isolated in good yield (Table I). The reaction started
by the formation of schiff base through the action of the
electron pair of primary amino group in
thiocarbohydrazide on the carbonyl group in substituted
benzaldehyde followed by proton transfer which lead to
the intracyclization reaction between the second primary
amino group and schiff base to obtained compounds (2-6)
as shown in (Scheme 2) [11].
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CHZ will first react with C=O bond of the formic acid (1:1) to form
H2N-NH-C-NH-N=C-OH
_______II ______I___
_______O ______H___
Then, if the OH group will react with NH2, tetrazine will be form.
If the OH group react with the NH group then ATO will be formed.
Now with excess of formic acid,i believe a polymeric mess may accure
Attachment: Dr.ShaymaaK.Younis.pdf (727kB)
This file has been downloaded 14 times
[Edited on 25-9-2024 by underground]
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underground
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Ok after searching a bit, the amine group like to react with the C=O group forming C=NH + H20 while amides like to reach with the C-OH group forming
C-NH2. A good example is semicarbazide and formic acid. The amine react with the C=O group and the amide with the C-OH group closing the ring. So most
likely CHZ and formic acid (1:2) will form this
So if i am correct, it will somehow close the ring with oxalic acid forming this
Interestingly, CHZ and parabanic acid may form an analoge to glycoluril.
[Edited on 27-9-2024 by underground]
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