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Shalashaska
June 24th, 2007, 12:39 AM
This method of purification of HNO<sub>3</sub> struck me as one of the more simple and less dangerous ways out there, since there is no distillation, and thus, no NOx. But since this method has been but vaguely mentioned by NBK2000 about five years ago, in 2002, I have a couple questions.

1. First of all, I'm guessing that for this to work, the HNO<sub>3</sub> must be impure with NOx, and not water, since water would freeze right along with the nitric. Or would there be fractional crystallization, and the HNO<sub>3</sub> would precipitate out as the water is frozen?

2. Should the dry ice be plopped right into the nitric acid, or put around the container it's in, kind of like a CO<sub>2</sub> bath.

3. Should the HNO<sub>3</sub> be a minimum concentration, or theoretically could you do this with 20% if you had such a horrible concentration.

4. In NBK's posts about it, he mentioned use of methylene chloride; is this a necessary component of this process?

Note: I know that the HNO<sub>3</sub> should be as cold as possible, to prevent sublimation on contact, but that's about all I know for sure about this procedure.

Please excuse my complete lack of knowledge about this, but its only mentions have been rather obscure.

Edit: After finding the actual "Methylene Chloride" thread, I realize there was much more information on this subject than I previously believed. When I read it earlier, it was the archive version and there was only one page.

Enkidu
June 24th, 2007, 01:23 AM
The usefulness of the dry ice (frozen CO2) comes not from any chemical composition but its temperature. The temperature of dry ice is below the freezing point of anhydrous nitric acid. The use of dry ice has nothing to do, AFAIK, with removing NOx.

The idea is to freeze the nitric acid and thus precipitate it from the DCM (or other extraction solvent). So yes, DCM is necessary.

If you were to subject 20% nitric acid to the temperature of dry ice, you would not be able to freeze out anhydrous nitric acid.

Look up the 'Preparation of Anhydrous Nitric Acid with Methylene Chloride' patent and carefully read the threads on this board about this process. You will learn all you need to know.

Edit in response to your post below: I believe raffinate means that the DCM/HNO3 will be a separate layer than the sulfuric acid, in which case a simple medicine dropper extraction could be used; is this correct?

Yes, that's correct, but to obtain any significant amount of nitric acid, you'll need the volume of quite a few medicine droppers.

Shalashaska
June 24th, 2007, 01:38 AM
The usefulness of the dry ice (frozen CO2) comes not from any chemical composition but its temperature.

Well I knew that at least, so don't think I'm completely retarded. : /

Edit/Addition (as to not be a post whore)

Okay, so once the nitric acid is dissolved in the methylene chloride, how do you separate the DCM/HNO<sub>3</sub> from the Sulfuric? It says:
The methylene chloride raffinate is then separated from the aqueous acid solution by any conventional liquid separation techniques.

I believe raffinate means that the DCM/HNO<sub>3</sub> will be a separate layer than the sulfuric acid, in which case a simple medicine dropper extraction could be used; is this correct?

s-lab
June 24th, 2007, 04:28 AM
Where do you get your nitric anyway? all i can find is rubbish 10% stuff from my supplier. Is there a way you can make it more conc?

Rbick
June 24th, 2007, 11:52 AM
s-lab-
Search the internet for reagent grade HNO3, there are countless chemical supplier sites that will sell you 70-90 + percent nitric acid. 90% will cost you quite a bit, we're talking 100 USD or more. You're better off in the long run making your own, but if you're lazy and have lots of money, it is easy to get. And of course you will probably be put on a government watch list unless you have a damn good reason to have high conc. nitric acid. 70 percent can be bought for as low as 35 USD for 500ml. I think it is looked down upon to list specific websites, but if you take 5 minutes to google search it, you'll find it.

Shalashaska
June 24th, 2007, 03:49 PM
Oh, trust me, I have looked for nitric online. However, it was about at the 3rd chemical website that I discovered prices for 500mL 70% didn't get below $30-50 US. That's about when I decided to just stick with ANFO and various synths that can substitute a nitration bath (H<sub>2</sub>SO<sub>4</sub>+xNO<sub>3</sub>) for nitric acid.

But then I found this wonderful nitric synth for *anhydrous* nitric, which caught my attention greatly due to relative ease, and the fact that I really wanted to make RDX, and clearly, nigger-rigged bottle nitric wasn't gonna cut it.

Note: I noticed nigger-rig wasn't underlined red with spell check XD