View Full Version : Nitration without the use of acid?!?!
zeocrash
January 10th, 2003, 12:14 PM
OK i'm trying to manufacture chloropicrin. i'm planning to use the nitrating chlorinated hydrocarbons method. using dichloromethane (from paint srtipper)
6CH<sub>2</sub>Cl<sub>2</sub> + 4HNO<sub>3</sub> ==> 4CCl<sub>3</sub>NO<sub>2</sub> + 4H<sub>2</sub>O +C<sub>2</sub>H<sub>4</sub>
but upon closer inspection of my source (a US army field manual on chemical warfare agents) I discovered that Chloropicrin is broken down by acid to form CX a blister agent. which i'm not prepared to handle yet.
is there any way that i can nitrate the dichloromethane, without using acid. or does anyone know how i could use acid but prevent the production of CX.
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the PDF file of the field manual has been uploaded to the FTP and is now in the recent section, so take a look there if you want
MrSamosa
January 10th, 2003, 04:13 PM
Thanks Zeo, you have just given told me of a new, seemingly easier way to prepare CX :D .
Although for your little problem, might I suggest that you try the Nitromethane/Sodium Hypochlorite Method? The chemicals seem so much easier to obtain than Nitric Acid. Any concentration of the Hypochlorite works; although lower concentrations, as found in bleach, may require some heating. The entire reaction only takes about 20 minutes, and the yields are great.
From my personal experience with this method, it works wonderfully. But, if Nitromethane is difficult for you to obtain, then this method may not be helpful.
zeocrash
January 10th, 2003, 06:57 PM
where would i find nitromethane
no i chose the nitrating chlorinated hydrocarbons method because i've got a whole load of nitric acid. but the method appears imposible as any PS made is instantly converted to CX by the acid as i've mentioned previously. i was thinking that bubbling nitric oxide through the dichloromethane
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the paint stripper that contains dichloromethane is called nitromors. it also contains methanol so it may need to be distilled
the field manual is in the recent directory of the ftp as fm3-9.pdf
kingspaz
January 10th, 2003, 07:15 PM
dichloromethane doesn't react with nitric acid. it is inert towards it, hence its use in solvent extraction of HNO3 from xHSO4/HNO3/H2SO4 mixtures. do a search for a topic called solvent extraction.
nbk2000
January 10th, 2003, 08:42 PM
From my information, the PS to CX conversion needs to be done with Tin metal (though you could likely use cheaper zinc or iron) and acid, to reduce the PS to CX. Acid alone would likely achieve only trace amount conversion.
The NM/Bleach process is much easier and efficient than trying to nitrate anything. Pool bleach is 10%, more than adequate for the process.
MrSamosa
January 11th, 2003, 05:45 AM
Zeo- Nitromethane can be obtained from a local Hobby Shop. It's sold as Race Car Fuel (the RC type). If not, I'm sure you can find it from some online hobby dealer. The only problem with it, however, is that it is so bloody expensive pure. Usually it is sold in mixtures of Methanol and Castor Oil, as mine is.
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