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lalalympo
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[*] posted on 11-1-2017 at 02:00
Drying urea nitrate


I made urea nitrate yesterday. I dissolved some pure urea (no urine) in water and added nitric acid with a pipette. I calculated the amount of urea and nitric acid needed to produce 10 grams of urea nitrate. I kept adding the nitric acid until I could observe no more reaction. The amount of acid I used was right around the 6 grams I needed for (theoretical) full nitration of the urea. I poured a lot of the water of and transferred the slurry to a shallow glass dish. I added acetone to the dish. If I looked very closely I could see some reactions, presumably remaining nitric acid reacting with the acetone. I left the slurry to dry in the glass dish. It's been more than 24 hours now, I had a fan blowing over it (no warm air, just airflow) to help it dry. It's still a slurry! I could also distinguish a nitric acid smell from the slurry. Should I add more acetone to react with nitric acid, do I need to heat the slurry to accelerate the drying process?

Any help is appreciated.
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simply RED
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[*] posted on 11-1-2017 at 06:21


Do not add acetone, dry well in the filter, and it will be fine...



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PHILOU Zrealone
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[*] posted on 11-1-2017 at 10:16


1°) Urea nitrate is moderately stable salt...it very fast looses its HNO3 by hydrolysis because urea is not very basic.
2°) Aceton is uncompatible with HNO3...when HNO3 is concentrated enough (>40%) ...the mixing induce very fast a runnaway reaction yielding NxOy and oxydation products. NxOy oxydises aceton to methyl-glyoxal mono-oxime and further weird decay products.
3°) If a large exces and concentrated HNO3 is used aceton provides nitroform (trinitromethane) and acetic acid owing to enol form of aceton CH3-C(-OH)=CH2 and first addition of HONO2 to the double link; thus passing from CH3-CO-CH2-NO2, to CH3-CO-CH(NO2)2, CH3-CO-C(NO2)3 and finally to CH3-CO2H and HC(NO2)3; thus a bit what happens for chloroform synthesis from aceton but in highly concentrated acid instead of basic one (chloroform happens in presence of basic media and Cl2 or hypochlorite)

Because of 1°) and 2°) it is not wise to use aceton to dry urea nitrate.
Better use methanol, ethanol and finally ether or simply dry air...




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lalalympo
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[*] posted on 11-1-2017 at 12:33


As a little update I added more acetone, twice. After the second addition the Nitric acid/nitric oxide smell wasn't present anymore. I transferred the product to a HDPE container. I'm gonna try to blow it up in a few days. Any suggestions on how to detonate it? Getting a blasting cap where I live will be a pain if it's even possible at all. With a hammer and anvil maybe?


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[*] posted on 11-1-2017 at 12:41


Quote: Originally posted by PHILOU Zrealone  
1°) Urea nitrate is moderately stable salt...it very fast looses its HNO3 by hydrolysis because urea is not very basic.
2°) Aceton is uncompatible with HNO3...when HNO3 is concentrated enough (>40%) ...the mixing induce very fast a runnaway reaction yielding NxOy and oxydation products. NxOy oxydises aceton to methyl-glyoxal mono-oxime and further weird decay products.
3°) If a large exces and concentrated HNO3 is used aceton provides nitroform (trinitromethane) and acetic acid owing to enol form of aceton CH3-C(-OH)=CH2 and first addition of HONO2 to the double link; thus passing from CH3-CO-CH2-NO2, to CH3-CO-CH(NO2)2, CH3-CO-C(NO2)3 and finally to CH3-CO2H and HC(NO2)3; thus a bit what happens for chloroform synthesis from aceton but in highly concentrated acid instead of basic one (chloroform happens in presence of basic media and Cl2 or hypochlorite)

Because of 1°) and 2°) it is not wise to use aceton to dry urea nitrate.
Better use methanol, ethanol and finally ether or simply dry air...


So I used acetone. I didn't observe any NO2 evolving after the acetone addition. I thought small amount of excess HNO3 (I estimate it's less than a gram) would react with the acetone to make relatively harmless formic acid and acetic acid. Note: I diluted the reaction mixture with distilled water before pouring it off and adding acetone.

The side products you're talking about, I can't find much info on them. Are they dangerous? If so I might have to get rid of this stuff.

For a future synthesis I will use methanol to dry it as suggested. But my primary concern now is finding out whether I've been handling a very poisonous substance today.
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[*] posted on 11-1-2017 at 12:53


Okay so I looked up some info and damn. I left a bare piece of steel (not stainless) in the drying pan to test the dryness without touching the product itself. Some yellow crystals formed close to the piece of metal. I'm afraid these are trinitromethane salts of the metal I used. I assumed it was some leftover nitric acid reacting with the metal but now I'm really worried.

I want to get rid of this stuff. I can't just throw away this stuff, especially not with a big "UREA NITRATE" label on it. Is there any way to destroy this stuff easily? Or do I just need to add water?
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[*] posted on 11-1-2017 at 12:54


Here you will find all you ask.

http://parazite.nn.fi/roguesci/index.php/t-131.html

SASQ UTFSE !!!!

p.s. It generally works with acetone, it needs really huge excess of NA or impure starting products in order not to work...

lalalympo - I am going to advise you to not continue working with explosive substances as you do not understand the simplest principles! Why did you add water to the reaction mixture and so on and so on. Keep away from accidents!!!

[Edited on 11-1-2017 by simply RED]




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[*] posted on 11-1-2017 at 13:06


Quote: Originally posted by lalalympo  
As a little update I added more acetone, twice. After the second addition the Nitric acid/nitric oxide smell wasn't present anymore. I transferred the product to a HDPE container. I'm gonna try to blow it up in a few days. Any suggestions on how to detonate it? Getting a blasting cap where I live will be a pain if it's even possible at all. With a hammer and anvil maybe?



Good luck with the hammer and anvil...you will explode your hammer and anvil before it goes off.

UN (urea nitrate) is not an easy to detonate stuff...requires a detonator or a good initiating charge of more sensitive HE.

Also the large critical diameter of detonation (> 3cm) implies you to work with large charges --> big quantities --> a lot of noise when detonating and unsafe --> will bring attention to you as a possible terrorist.

[Edited on 11-1-2017 by PHILOU Zrealone]




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[*] posted on 11-1-2017 at 13:10


Quote: Originally posted by lalalympo  
Okay so I looked up some info and damn. I left a bare piece of steel (not stainless) in the drying pan to test the dryness without touching the product itself. Some yellow crystals formed close to the piece of metal. I'm afraid these are trinitromethane salts of the metal I used. I assumed it was some leftover nitric acid reacting with the metal but now I'm really worried.

I want to get rid of this stuff. I can't just throw away this stuff, especially not with a big "UREA NITRATE" label on it. Is there any way to destroy this stuff easily? Or do I just need to add water?

If it doesn't stay long into contact...aceton is not a problem.
If no concentrated HNO3 in large excès (8/1) then no risks of nitroform formation.
No risk of very poisonous product (exept NxOy fumes)




PH Z (PHILOU Zrealone)

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[*] posted on 11-1-2017 at 13:15


Quote: Originally posted by simply RED  
Here you will find all you ask.

http://parazite.nn.fi/roguesci/index.php/t-131.html


You and I are definitely old dinosaurs :cool:;):P:) back to 2001 and the EWP forum before the SM forum starts




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simply RED
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[*] posted on 11-1-2017 at 13:22


We (and the other participants) have milked the UN topic sand dry back in the days :) .

As you see, the first topic starts with 5 kg, I was 17 back then... Got older, hardly smarter...

Greetings!

[Edited on 11-1-2017 by simply RED]




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lalalympo
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[*] posted on 11-1-2017 at 13:24


Quote: Originally posted by simply RED  
Here you will find all you ask.

http://parazite.nn.fi/roguesci/index.php/t-131.html

SASQ UTFSE !!!!

p.s. It generally works with acetone, it needs really huge excess of NA or impure starting products in order not to work...

lalalympo - I am going to advise you to not continue working with explosive substances as you do not understand the simplest principles! Why did you add water to the reaction mixture and so on and so on. Keep away from accidents!!!

[Edited on 11-1-2017 by simply RED]


SASQ UTFSE? What does that mean?

Yeah, I think you're right. I need to learn more chemistry before continuing with explosive substances. I actually made nitroglycerin in the same unprofessional manner. Thank you for the good advice.

I added water to the reaction mixture improve visibility and ease of pouring the remaining liquid off. It's below zero centigrade outside here so the urea did not fully dissolve (decreasing visibility in the mixture) and temperature differences were not measurable for me.

Anyway I'm now stuck with a small amount of urea nitrate that I can't detonate with anything I have at hand. Is there any way to detonate or at least destroy it?
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[*] posted on 11-1-2017 at 13:26


Go fertilize some soil with it....



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lalalympo
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[*] posted on 11-1-2017 at 13:30


Quote: Originally posted by PHILOU Zrealone  
Quote: Originally posted by lalalympo  
As a little update I added more acetone, twice. After the second addition the Nitric acid/nitric oxide smell wasn't present anymore. I transferred the product to a HDPE container. I'm gonna try to blow it up in a few days. Any suggestions on how to detonate it? Getting a blasting cap where I live will be a pain if it's even possible at all. With a hammer and anvil maybe?



Good luck with the hammer and anvil...you will explode your hammer and anvil before it goes off.

UN (urea nitrate) is not an easy to detonate stuff...requires a detonator or a good initiating charge of more sensitive HE.

Also the large critical diameter of detonation (> 3cm) implies you to work with large charges --> big quantities --> a lot of noise when detonating and unsafe --> will bring attention to you as a possible terrorist.

[Edited on 11-1-2017 by PHILOU Zrealone]


I read about people detonating RDX using a hammer and anvil, surely urea nitrate isn't more stable than RDX? Couldn't I use magnesium powder to create a very high temperature and get the urea nitrate to decompose?
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[*] posted on 12-1-2017 at 06:45


Urea Nitrate is an excellent high nitrogen fertilizer. I use if for feeding non-flowering plants.



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