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Author: Subject: Alternative to Nitrosyl Tetrafluoroborate?
APO
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[*] posted on 2-7-2013 at 00:28
Alternative to Nitrosyl Tetrafluoroborate?


Obviously, this chemical is very hard to get at all, but can something replace it for the HNIW synthesis here? I think I heard somewhere that Dinitrogen Pentoxide and/or White Fuming Nitric Acid can replace Nitrosyl Tetrafluoroborate for this? Alternatively I could get Nitronium Tetrafluoroborate from Reagent Shop, although I'm not sure if it can replace Nitrosyl Tetrafluoroborate for this though. Yes, I've actually bought from these guys and haven't had any problems, not sure if that would change when ordering something this exotic though...

Any solutions are largely appreciated, thanks.

[Edited on 2-7-2013 by APO]




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[*] posted on 2-7-2013 at 04:18


Just a random question, what had you ordered?

I do not recommend you to start chemistry with such exotic reagents, or explosives but nitrosylsulphuric acid can be made from sulphur dioxide and nitric acid, or N2O3 and H2SO4. All the nitronium salts can be made similarly, by passing the N2O3 in the very concentrated acids.




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[*] posted on 3-7-2013 at 10:56


I got some 4-Nitrobenzoic Acid, nothing that special, but I needed some. I ran a Titration, and it was at stated purity, so I'm happy with them. I'm not going to use Nitrosyl Tetrafluoroborate anytime soon, I just want it for when I need it. Anyways, can Nitrosyl Tetrafluoroborate be made by passing various Nitrogen Oxides through Fluoroboric Acid? Or will it hydrolyze like usual? Also I think you forgot that I'm wondering about an alternative to Nitrosyl Tetrafluoroborate that would work for where it's used in HNIW synthesis.



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[*] posted on 8-7-2013 at 20:59


Anhydrous fluoroboric acid and NOx will make your salt, but I'm not responsible of any injury you may have. I gave you alternative, you could make nitrosyl perchlorate, nitrosylsulphuric acid etc...



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AndersHoveland
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[*] posted on 8-7-2013 at 22:56


Quote: Originally posted by APO  
can something replace it for the HNIW synthesis

You do not know enough about chemistry to make it work, but if anyone else was curious...

One might be able to gradually add in some NaNO2, using a small amount of BF3 as a catalyst, similar to the RDX "E method". I would recommend not letting the reaction sit too long though, because NO2 tends to degrade the product. If the reaction mixture turned brown, that would be a bad sign.

Actually, you probably do not need nitrosyl tetrafluoroborate (NOBF4). The main reason I think it is called for in the synthesis is that nitronium tetrafluoroborate (NO2BF4) is overkill. The former is less reactive, and is actually more ubiquitous, relatively speaking.

Basically, after the use of Pearlman's catalyst, 4 of the substituted benzyl groups will have been replaced with acetyl groups. The addition of the NOBF4 is to remove the last 2 remaining benzyl groups, nitrosating those 2 positions on the hexaazaisowurtzitane cage.

Finally, the addition of the NO2BF4 hydrolyzes off the remaining acetyl groups, and nitrates the molecule. (Honestly, I am not sure if those nitroso, part of nitrosamine, groups get hydrolyzed off or oxidized to nitramine).

So I am sure you could just directly use NO2BF4, likely with moderately lower yields. If anyone is knowledgeable about this, correct me if wrong.

Quote: Originally posted by plante1999  
nitrosylsulphuric acid can be made from sulphur dioxide and nitric acid, or N2O3 and H2SO4. All the nitronium salts can be made similarly, by passing the N2O3 in the very concentrated acids.

Yes, it contains the equivalent of the nitrosyl cation, but it would probably be very problematic. It is basically sulfuric acid here, and you know that the formation of RDX does not go so well in the presence of concentrated sulfuric acid.

What you might be able to do is precipitate out solid crystals of the nitrosyl sulfuric acid, and then dissolve those in the acetic anhydride. Again, I would strongly recommend a little BF3 still be present as a catalyst here

Nitrosyl sulfuric acid tends to start precipitating out from solution within a narrow acid concentration, higher or lower than that it completely dissolves. too complicated to go into detail here




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[*] posted on 24-7-2013 at 03:23


According to this, Dinitrogen Pentoxide has been used to convert TAIW to HNIW.

Obviously, making Dinitrogen Pentoxide is much less work than making Nitrosyl Tetrafluoroborate and/or Nitronium Tetrafluoroborate, so lets say I managed to make HBIW and convert it into TAIW.

How would I go about converting it to HNIW with Dinitrogen Pentoxide?


[Edited on 24-7-2013 by APO]




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[*] posted on 27-7-2013 at 14:25


Quote: Originally posted by APO  
According to this, Dinitrogen Pentoxide has been used to convert TAIW to HNIW

Not surprising. The reason why nitronium tetrafluoroborate is often used in laboratory synthesis is that it is a more stable regent, it can be stored without degradation. N2O5 also has a potential explosion hazard.

Usually the two regents are interchangeable, but I am aware of at least two other specific reactions where the nitrate anion (or resulting nitric acid) can interfere, where nitrononium tetrafluoroborate has to be used.

[Edited on 27-7-2013 by AndersHoveland]
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[*] posted on 27-7-2013 at 19:31


Quote: Originally posted by AndersHoveland  

N2O5 also has a potential explosion hazard.
[Edited on 27-7-2013 by AndersHoveland]


??? What makes you think so? Liquid N2O may explode, yeah, but even NO2 despite it is the endothermic compound hardly can explode. N2O5 as well. It is unstable and must be kept under low temperature, but it is not an explosive.




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[*] posted on 27-7-2013 at 20:24


Quote: Originally posted by caterpillar  
N2O5 is not an explosive.

I think it actually is. Not extremely sensitive though

Quote: Originally posted by caterpillar  
Liquid N2O may explode

Never heard of this, perhaps if the pressurized tank ruptures. I have read some things suggesting that liquefied nitric oxide might be able to detonate under certain conditions though:
http://www.sciencemadness.org/talk/viewthread.php?tid=20368

[Edited on 28-7-2013 by AndersHoveland]
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[*] posted on 28-7-2013 at 03:35


I cannot find immediately this info, but in row N20-> NO -> N2O3 -> NO2 (N2O4) -> N2O5 the first compound is the most endothermic and therefore can explode like C2H2. N2O5 is only slightly endothermic- heat of hydration makes HNO3 exothermic compound. It means, that some powerful catalyst might convert air and water to nitric acid and generate simultaneously some energy. In fact, this process takes place in some vegetables- beans, for example.



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[*] posted on 28-7-2013 at 03:57


found this, which is suggestive that it may be able to explode:
Quote:
"N2O5 ... is prepared by passing chlorine gas over argentic nitrate, and condensing the products in a receiver cooled to a very low temperature. It is a solid crystalline compound, possessing the composition N2O5. When brought in contact with water it combines, with evolution of heat... When kept in a closed tube it has been found to explode with violence, and without any external aid."
Chemistry for Students, Alexander William Williamson, (1865)


Quote:
"It is a white crystalline solid (m.p. 30 °C). With the rise in temperature, it becomes yellow due to partial decomposition into brown NO2. When heated above melting point it decomposes with explosion."
Objective Question Bank in Chemistry, B. K. Sharma


[Edited on 28-7-2013 by AndersHoveland]
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[*] posted on 28-7-2013 at 23:55


OK, may be I'm wrong about it. In any event, the only way for us poor boys to use N2O5 is to add some P2O5 to FNA. This mixture will never explode (but contact with skin may be very unpleasant).



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