Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1    3  ..  8
Author: Subject: DIAMINOURONIUM (DI)NITRATE
MineMan
International Hazard
*****




Posts: 1002
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 4-6-2019 at 22:13
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.

View user's profile View All Posts By User
Fulmen
International Hazard
*****




Posts: 1710
Registered: 24-9-2005
Member Is Offline

Mood: Bored

[*] posted on 5-6-2019 at 00:39


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 696 times




We're not banging rocks together here. We know how to put a man back together.
View user's profile View All Posts By User
underground
National Hazard
****




Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline


[*] posted on 5-6-2019 at 05:50


Well, i can not seen anywhere anyone selling diaminourea that cheap
View user's profile View All Posts By User
Boffis
International Hazard
*****




Posts: 1858
Registered: 1-5-2011
Member Is Offline

Mood: No Mood

[*] posted on 5-6-2019 at 08:08


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)
View user's profile View All Posts By User
MineMan
International Hazard
*****




Posts: 1002
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 5-6-2019 at 15:35


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]
View user's profile View All Posts By User
underground
National Hazard
****




Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline


[*] posted on 6-6-2019 at 11:53


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]
View user's profile View All Posts By User
MineMan
International Hazard
*****




Posts: 1002
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 6-6-2019 at 19:47


Quote: Originally posted by underground  
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]


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....
View user's profile View All Posts By User
twelti
Hazard to Others
***




Posts: 217
Registered: 20-2-2019
Member Is Offline


[*] posted on 6-6-2019 at 20:58


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?
View user's profile View All Posts By User
Fulmen
International Hazard
*****




Posts: 1710
Registered: 24-9-2005
Member Is Offline

Mood: Bored

[*] posted on 6-6-2019 at 23:48


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.
View user's profile View All Posts By User
MineMan
International Hazard
*****




Posts: 1002
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 7-6-2019 at 00:48


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?


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.
View user's profile View All Posts By User
twelti
Hazard to Others
***




Posts: 217
Registered: 20-2-2019
Member Is Offline


[*] posted on 7-6-2019 at 01:59


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]
View user's profile View All Posts By User
Microtek
National Hazard
****




Posts: 850
Registered: 23-9-2002
Member Is Offline

Mood: No Mood

[*] posted on 7-6-2019 at 05:39


In my experience you can probably trust the minimum order quantity, but the price per kg will likely be much higher.
View user's profile View All Posts By User
Fulmen
International Hazard
*****




Posts: 1710
Registered: 24-9-2005
Member Is Offline

Mood: Bored

[*] posted on 7-6-2019 at 12:42


yeah, that's probably the bulk price.



We're not banging rocks together here. We know how to put a man back together.
View user's profile View All Posts By User
twelti
Hazard to Others
***




Posts: 217
Registered: 20-2-2019
Member Is Offline


[*] posted on 10-6-2019 at 09:04


Right enough. I did get a quote for $100 for one kg. That's not too bad assuming you can use that much.
View user's profile View All Posts By User
underground
National Hazard
****




Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline


[*] posted on 10-6-2019 at 11:03


It sounds cool. From where you got it from alibaba? Let us know how it does work after you got it.
View user's profile View All Posts By User
twelti
Hazard to Others
***




Posts: 217
Registered: 20-2-2019
Member Is Offline


[*] posted on 10-6-2019 at 11:31


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:Dyestuff Intermediates Type:Pharmaceutical 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
View user's profile View All Posts By User
MineMan
International Hazard
*****




Posts: 1002
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 10-6-2019 at 19:35


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.
View user's profile View All Posts By User
underground
National Hazard
****




Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline


[*] posted on 11-6-2019 at 02:22


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]
View user's profile View All Posts By User
twelti
Hazard to Others
***




Posts: 217
Registered: 20-2-2019
Member Is Offline


[*] posted on 11-6-2019 at 07:57


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?
View user's profile View All Posts By User
underground
National Hazard
****




Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline


[*] posted on 11-6-2019 at 11:18


You have PM
View user's profile View All Posts By User
underground
National Hazard
****




Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline


[*] posted on 11-6-2019 at 14:36


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]
View user's profile View All Posts By User
twelti
Hazard to Others
***




Posts: 217
Registered: 20-2-2019
Member Is Offline


[*] posted on 13-6-2019 at 09:21


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?

View user's profile View All Posts By User
Tsjerk
International Hazard
*****




Posts: 3030
Registered: 20-4-2005
Location: Netherlands
Member Is Offline

Mood: Mood

[*] posted on 13-6-2019 at 09:24


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?



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.
View user's profile View All Posts By User
MineMan
International Hazard
*****




Posts: 1002
Registered: 29-3-2015
Member Is Offline

Mood: No Mood

[*] posted on 13-6-2019 at 23:17


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.
View user's profile View All Posts By User
underground
National Hazard
****




Posts: 702
Registered: 10-10-2013
Location: Europe
Member Is Offline


[*] posted on 13-6-2019 at 23:28


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.
View user's profile View All Posts By User
 Pages:  1    3  ..  8

  Go To Top