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MineMan
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DIAMINOURONIUM (DI)NITRATE
I am really excited to find this tonight, I hope everyone else will be too. It’s VOD and Vdet is equivalent to RDX, however, it is less sensitive
and seems to be very easily prepared.
Diaminourea is nitrated at RT with 30%NA. That’s pretty much it... if 2 moles of NA is used the dinitrate is formed. The only downside of the
dinitrate is it decomposes at 115C, a problem for industry but not for us...
The Dinitrate has a OB of 10 percent... I have not calculated the VOD of the mononitrate...
This looks very promising! Diaminourea seems to sell for about $15/kg in bulk. If anyone can find a US supplier I can investigate.
Love to hear your thoughts.
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Fulmen
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Interesting.
This has some basic info:
https://onlinelibrary.wiley.com/doi/pdf/10.1002/prep.2011000...
(scihubbed for convenience)
Attachment: fischer2011.pdf (344kB)
This file has been downloaded 716 times
We're not banging rocks together here. We know how to put a man back together.
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underground
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Well, i can not seen anywhere anyone selling diaminourea that cheap
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Boffis
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Diaminourea is known as carbohydrazide (as mono-aminourea = semicarbazide) and it has been discussed severasl time before on SM (UTFSE). If you have
access to hydrazine hydrate or are prepared to make it from hydrazine salts the preparation is simple. Simply treat either urea or dimethylcarbonate
with slightly more than 2x its molar equivalence of hydrazine hydrate, the later requires that this is done in two stages. There is also a patent that
describes the preparation from cyanuric acid and hydrazine hydrate. I have several paper on this compound.
Check out http://www.sciencemadness.org/talk/viewthread.php?tid=1128&a...
The last post by Rosco Bodine has a few link to useful papers. The patent is US 3258485 (cyanuric acid + HH)
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MineMan
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but has the nitrate been discussed here...
Can anyone calculate the performance of the perchlorate salt?
Both the perchlorate salt and the mononitrate have yields of 97 percent. I say sorry to the critics. Because yields which are in the high 90s, and
only a need for dilute acid once the precursor is had... this looks like the best high performance EM comparable to RDX for us... and the sensitivity
is very favorable... it contains less energy then RDX, I don’t know why as the molecule looks more favorable. But the volume of gas is impressive.
The dinitrate is a waste of time
[Edited on 5-6-2019 by MineMan]
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underground
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Have you ever consider melamine dinitrate ?
http://edoc.ub.uni-muenchen.de/12420/1/goebel_michael.pdf
https://patentimages.storage.googleapis.com/29/78/69/1bab837...
[Edited on 7-6-2019 by underground]
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MineMan
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Underground. I don’t see the advantage. The Detonation pressure is close to TNT.... I think it’s a good molecule, especially for very high
tempatures, stable enough for space... but with those specialty applications money is not an issue and higher performance EMs can be used....
The diaminourea on the other hand has a very real potential to replace RDX in many applications, it’s safer, and obtains the same Dp... the only
downside is the heat of explosion,but rest assured 15 percent Al powder can take care of that... and it will be out performing RDX in shape charge and
propellant applications... while only needing dilute nitric acid... THATS HUGE. I am surprised at the lack of excitement....
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twelti
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So, I found carbohydrazide on eBay for around $2/g, so not the cheapest (coincidentally the same vendor selling aminoguanidine bicarbonate and several
other interesting chems). Still, no WFNA needed, so that would offset some of the cost/effort required for RDX. Are you going to try it?
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Fulmen
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The lack of excitement is due to cost and availability. $15/kg doesn't sound bad, but that's in bulk. 1kg would probably cost closer to $1000. Even
1/10 of that would negate any benefit from simple nitration.
We're not banging rocks together here. We know how to put a man back together.
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MineMan
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Quote: Originally posted by twelti  | | So, I found carbohydrazide on eBay for around $2/g, so not the cheapest (coincidentally the same vendor selling aminoguanidine bicarbonate and several
other interesting chems). Still, no WFNA needed, so that would offset some of the cost/effort required for RDX. Are you going to try it?
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I want to give it a go when I am done from my travels. I would like some advice from those more wise then me about recrystallization and
measurements.... I can report back of course... or if you don’t hear from me you can assume it’s so amazing I am taking the secrets to my gave.
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twelti
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I found it for $20 / kg, min order 1 kg, on Alibaba. Not sure I trust that the min order is really 1 kg, but that is what it says.
[Edited on 7-6-2019 by twelti]
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Microtek
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In my experience you can probably trust the minimum order quantity, but the price per kg will likely be much higher.
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Fulmen
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yeah, that's probably the bulk price.
We're not banging rocks together here. We know how to put a man back together.
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twelti
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Right enough. I did get a quote for $100 for one kg. That's not too bad assuming you can use that much.
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underground
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It sounds cool. From where you got it from alibaba? Let us know how it does work after you got it.
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twelti
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Chemfine
No.1 Product information:
cas:497-18-7 carbohydrazide 99% boiler water treatment chemicals
Model no. carbohydrazide
Unit price
USD 100.0 /Kilogram/Kilograms
Order quantity
1.0
Product details
Place of Origin:CN;JIA Type yestuff Intermediates Type harmaceutical Intermediates Type:Syntheses Material Intermediates CAS No.:CAS
NO.497-18-7 Other Names:1,3-diaminourea MF:CH6N4O EINECS No.:207-837-2 Purity:99.0%min Brand Name:ChemFine Application:watertreat chemicals
Appearance:White Crystalline Powder Product name:Carbohydrazide 99% Appearance:White needle crystal powder Purity:99.9%min PH:7.2-9.7
Keywords:Carbohydrazide 99% Packing:25kg/bag HS Code:2928000090 Sample:Availiable
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MineMan
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That quote is too high unless it includes shipping.... they will likely charge 25-100 dollars for shipping. Most likely in the 80 range. Give it a
try. I plan too.
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underground
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I also just buy 2kg for 120 USD from Alibaba (including shipping). The transaction was very smooth with very good service. 1kg was for USD70 while
USD120 for 2kgs and USD640 for 25kgs because there is big discount on shipping cost for quantity above 20kgs. If anyone wants any details just send
me a PM
[Edited on 11-6-2019 by underground]
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twelti
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| Quote: Originally posted by underground | I also just buy 2kg for 120 USD from Alibaba (including shipping). The transaction was very smooth with very good service. 1kg was for USD70 while
USD120 for 2kgs and USD640 for 25kgs because there is big discount on shipping cost for quantity above 20kgs. If anyone wants any details just send
me a PM
[Edited on 11-6-2019 by underground] |
That is a bit better than the quote I got, who is your vendor?
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underground
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You have PM
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underground
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According to Fulmen's PDF, it may be a bit tricky to crystallize it out.
"Both nitrate salts, especially the monodeprotonated salt 2, cause major problems during their isolation since both remain as colourless liquids after
the water has been evaporated. 3 crystallizes after the liquid has been taken up in methanol and slowly been evaporated again, whereas 2 solidified
after the liquid was taken up in methanol and chilled to -20C for several days. Scratching the flask with a glass rod after the mixture was allowed to
come to room temperature resulted in the crystallization of the product. "
"Diaminourea (0.90 g, 10 mmol) is dissolved in nitric acid (2 M, 5 mL, 10 mmol) at room temperature. The solvent is removed from the clear solution
resulting in a colourless oil. Recrystallization from ethanol/water yields 2 as colourless solid (after long standing). Alternatively the compound was
crystallized after storage at -20C under methanol for several days and scratching the flask with a glass rod after the mixture was allowed to come to
room temperature. Yield: 1.48 g, 9.7 mmol, 97%."
It is said that the bis-perchlorate salt could not be isolated due to its high hygroscopicity, and the dinitrate forms a monohydrate so i believe the
the mononitrate it should be quite hygroscopic too, but it is still quite interesting.
[Edited on 11-6-2019 by underground]
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twelti
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| Quote: Originally posted by underground | According to Fulmen's PDF, it may be a bit tricky to crystallize it out.
"Both nitrate salts, especially the monodeprotonated salt 2, cause major problems during their isolation since both remain as colourless liquids after
the water has been evaporated. 3 crystallizes after the liquid has been taken up in methanol and slowly been evaporated again, whereas 2 solidified
after the liquid was taken up in methanol and chilled to -20C for several days. Scratching the flask with a glass rod after the mixture was allowed to
come to room temperature resulted in the crystallization of the product. "
"Diaminourea (0.90 g, 10 mmol) is dissolved in nitric acid (2 M, 5 mL, 10 mmol) at room temperature. The solvent is removed from the clear solution
resulting in a colourless oil. Recrystallization from ethanol/water yields 2 as colourless solid (after long standing). Alternatively the compound was
crystallized after storage at -20C under methanol for several days and scratching the flask with a glass rod after the mixture was allowed to come to
room temperature. Yield: 1.48 g, 9.7 mmol, 97%."
It is said that the bis-perchlorate salt could not be isolated due to its high hygroscopicity, and the dinitrate forms a monohydrate so i believe the
the mononitrate it should be quite hygroscopic too, but it is still quite interesting.
[Edited on 11-6-2019 by underground] |
The freezing method should be doable, right? Once you have some crystals of diaminouronium dinitrate, maybe you could use them to seed the chilled
liquid.
My question is, since this is less sensitive than RDX, and RDX is already not that sensitive, would it be hard to initiate?
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Tsjerk
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| Quote: Originally posted by twelti |
The freezing method should be doable, right? Once you have some crystals of diaminouronium dinitrate, maybe you could use them to seed the chilled
liquid.
My question is, since this is less sensitive than RDX, and RDX is already not that sensitive, would it be hard to initiate?
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You could also use a seed crystal with a comparable structure, or use a piece of dust.
Initiation could be done with some lead azide or something.
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MineMan
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| Quote: Originally posted by underground | According to Fulmen's PDF, it may be a bit tricky to crystallize it out.
"Both nitrate salts, especially the monodeprotonated salt 2, cause major problems during their isolation since both remain as colourless liquids after
the water has been evaporated. 3 crystallizes after the liquid has been taken up in methanol and slowly been evaporated again, whereas 2 solidified
after the liquid was taken up in methanol and chilled to -20C for several days. Scratching the flask with a glass rod after the mixture was allowed to
come to room temperature resulted in the crystallization of the product. "
"Diaminourea (0.90 g, 10 mmol) is dissolved in nitric acid (2 M, 5 mL, 10 mmol) at room temperature. The solvent is removed from the clear solution
resulting in a colourless oil. Recrystallization from ethanol/water yields 2 as colourless solid (after long standing). Alternatively the compound was
crystallized after storage at -20C under methanol for several days and scratching the flask with a glass rod after the mixture was allowed to come to
room temperature. Yield: 1.48 g, 9.7 mmol, 97%."
It is said that the bis-perchlorate salt could not be isolated due to its high hygroscopicity, and the dinitrate forms a monohydrate so i believe the
the mononitrate it should be quite hygroscopic too, but it is still quite interesting.
[Edited on 11-6-2019 by underground] |
I believe the mononitrate is the only worthwhile salt. The dinitrate has far to low energy of explosion.
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underground
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The dinitrate does not worth cause it forms a mono-hydrate. I have seen some other compounds with the same properties from NileRed. When a solution is
super saturated sometimes it does not crystallize out. Scratching the container by pressing the crystals it will crystallize out. Also by dropping a
single crystal it will crystallize out too. I don't think so we will have any issues. Also he used vacuum to drive off the water. I guess he did not
dry the compound completely with vacuum cause he was afraid for decomposition. As long as i do not have any vacuum distillation set up, i will just
use some cacl into a desiccator bad to drive all the water off. It may take a while but i believe it will remove all the water completely to dryness.
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