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Hey Buddy
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Quote: Originally posted by KNEWKID  | Orange crystal fraction soluble in pure nitromethane white powder insoluble in NM. Large mass of NTNT crude about 1/2 to 3/4 lb when dry.
Note: first extraction in NM cool yielded yellow crystals. 2nd extraction heated to 100F NM product turned orange...possible secondary rxn.
Will upload Raman spectra of each material later
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great work. --oh boy, Im going to have to bust out the NM.
What are the chances the white is NTNT, the yellow is linear, and the yellow changes color reacting with NM at temp, and the melt is funny on m.p.
because the melt is a eutectic mix and the ratios are changing on the times the melt seems finicky? lol
The white looks very similar to the mysterious "m1".
If there are two materials, I think that means they are co-crystallizing from acetone.
it keeps getting stranger and stranger
[Edited on 25-11-2022 by Hey Buddy]
[Edited on 25-11-2022 by Hey Buddy]
[Edited on 25-11-2022 by Hey Buddy]
[Edited on 25-11-2022 by Hey Buddy]
Okay Ive got a NM separation at room temp evaporating now. I dont think my insoluble fraction looks as white as knewkid's. My fraction looks a little
neon still, whiter than how it went into the NM, but it seems more yellow still than the pics he posted.-- I used H2SO4 derived NTNT and didnt use any
heat, just mag stirred in NM for 10m then gravity filter. --Knewkid, I have to ask if you are yielding half pounds, have you found a high yield method
to get that much sample? or are you just doing big ol batches? I'm not getting half pounds.
I really wonder if this multi-material phenomenon is an analogue the hexamine behavior in RDX/HMX or TMTN/DNPT? I suppose it could simply be some
linear nitrosamines. If knew kid can come through with some raman it will save a lot of head scratching for my scalp. Hopefully someone can interpret
his numbers because Im only fluent in top raman.
[Edited on 25-11-2022 by Hey Buddy]
[Edited on 25-11-2022 by Hey Buddy]
lol, what if he just uploaded a raman spec and it turned out to be NaCl. jk
[Edited on 25-11-2022 by Hey Buddy]
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MineMan
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Knew kid, what procedure did you use and what was your yield… you might be able to give us a good density with that quantity
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KNEWKID
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NTNT synthesis
180g NQ, 680cc 32% HCL, 220g Hexamine 500g NaNO2.
Mix 180g NQ and HEX in 5 Liter beaker add HCL slight exotherm dissolves after 10 minutes. Pour into 5 gal poly bucket add 8 lbs ice. Solution is
slightly transparent. Mix 500 g NaNO2 with 600cc water. Add 1/2 mix stir vigorously with foaming with ppt forming. Let settle some and add rest of
NaNO2 solution with mixing. let stand and stir. Evolution of formaldehyde gas. Stir to degas solution. Let stand over night and filter through 100
micron large pp bucket filter. Even 1 day later giving off formaldehyde gas.
Letting air dry for few days
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Hey Buddy
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Post NM separation, still waiting on soluble fraction (evaporating the NM). insoluble white fraction does not melt. It decomposes somewhere in
neighborhood of 170 C.
In that case, an extracted component not melting and dec. at much higher temp, I propose a hypothesis: eutectic mix making low temp melt @75 C. Crude
material precipitate from reaction is a cocrystal of two different materials with different properties, together creating a eutectic. Recrystallizing
from acetone is then again co-crystallizing a different higher density plate morph. That could be possible because acetone can dissolve both polar and
non polar but NM is more polar.
This would make sense because it could explain the trouble in density sampling and in melt temp. It could also explain small differences between H2SO4
and HCl rendering. One acid could form more of comp a, another more heavily b. The various ratios would create a melt curve, probably traditional
eutectic V curve, changing depending on the ratio.
That would be an interesting case if true because I have not heard of this phenomenon at all let alone in an energetic material. To automatically
generate a low temp proportional eutectic melt from a simple reaction, that then gives confusions like what is found here. Of course that's all hunch,
I suppose it could be something else.
I do not believe the white material from NM extraction is the same material found earlier as "M1". The open flame burning of "NM extracted white" is
much more gentle than burning of M1. M1 also seems more "powdery" in consistency.
I think next logical step is, 1) hope knewkid can show us the boomfax 2) Begin examining this as a eutectic and that is basically the same steps as
already planned, ie. material compatibility and understanding the melt. The main difference caused by this new information is that now performance
testing is even more critical because additional work could be a waste of time if this material is not high performance and if it is not the target
material "NTNT". Now the possibilities for identity of the materials are: 1) NTNT is not present, two other materials are formed, these are a eutectic
system 2) it could be that one material is NTNT and the other is not, and therefore because all testing thus far has erroneously assumed one material,
all of that testing and character is actually attributable to the eutectic system and is not a property of the target molecule "NTNT" (if it is in
fact even present).
The interest in the material is based on the likelihood of it being 1) meltable and 2) high energy.
It has to be ascertained what the performance of the eutectic system is, if it is anywhere as high performance as other triazines. At this point I
have to eat any performance theory and the yield data, OB and valence calculations because if there is a eutectic system it changes all the rules and
none of that could possibly apply. It could still be high performance and a simple melt cast eutectic system that is simple and convenient to prepare,
but none of the known comparable triazine data could help in identifying it, so if it's not a triazine it's all mystery from here. It does hammer det,
burn energetically, melt at the right temp, is high density and is easy to produce. The only thing thats really changed is the material's identity.
I suppose the another exhaustive avenue would be a nitrosation in acetic acid which might produce yet again another variant, similar to RDX/HMX or
TMTN/DNPT.
Wild.
--please correct anything im overlooking or simply unaware of
[Edited on 26-11-2022 by Hey Buddy]
-knewkid just goes big or goes home
[Edited on 26-11-2022 by Hey Buddy]
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underground
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Welll, can someone give a try on 2-nitrimino-5-nitrohexahydro-1,3,5-triazine? Also wondering about reacting aminoguanidine instead of NQ and nitrating
it since Zrdx is unstable. So most likely the Zrdx but with an amino group instead of a nitro group would be much more stable.
A lot of energetics can be made from amino/nitro guanidine and hexamine which all of those are still unexplored.
[Edited on 26-11-2022 by underground]
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Hey Buddy
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Soluble fraction dries as yellow powder. Is melting at ~75 C. It is most likely containing the nitroso groups because of its yellow color.
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MineMan
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Updates?
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Hey Buddy
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Ive got sample loaded for testing but Im searching for a good primary t ogo with, So far it looks like cmc lead azide/ptfe. As I search the labyrinth
unfolds from one room to the next. Trying to get a handle on AGu perchlorates and see what they hold but AGu preparation is a bit more annoying than
hydrazine so I might just go with azide. Wherever I arrive will be used for testing this failed-NTNT substance. I havent been as interested in it
since learning about glycine perchlorate melting properties. I will compare both at some point.
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MineMan
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But you said this outperforms HMX. Glycine perchlorate does not.
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Hey Buddy
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I said, *If the molecule is correct*, it should out perform RDX, possibly HMX. The density seems to support that but now that it's learned that it is
two unidentified molecules, it's a wild card, probably not a triazine so the comparative chemical makeup cant be relied on to predict its performance.
GlyClO4 performance is really still unknown generally, but if it is >8000m/s it is close to PETN/RDX and can melt just over 100 C. So to compare
the two meltable explosives, "NTNT" requires H2SO4/HCl/GuNO3/Hexamine for 30-40% probable yield versus GlyClO4 requires Glycine/NH4ClO4 at near
quantitative yield requiring no acid. That is why my interest shifted to GlyClO4. Both need to be tested on firing. I think the mysterious NTNT will
still do okay, but I'm not as excited now that I know it could be a linear nitrosamine.
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MineMan
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Oh. I see 
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