APO
National Hazard
Posts: 627
Registered: 28-12-2012
Location: China Lake
Member Is Offline
Mood: Refluxing
|
|
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]
"Damn it George! I told you not to drop me!"
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
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.
I never asked for this.
|
|
|
APO
National Hazard
Posts: 627
Registered: 28-12-2012
Location: China Lake
Member Is Offline
Mood: Refluxing
|
|
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.
"Damn it George! I told you not to drop me!"
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
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...
I never asked for this.
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
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
I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
|
|
|
APO
National Hazard
Posts: 627
Registered: 28-12-2012
Location: China Lake
Member Is Offline
Mood: Refluxing
|
|
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]
"Damn it George! I told you not to drop me!"
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
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]
|
|
|
caterpillar
Hazard to Others
Posts: 472
Registered: 8-1-2012
Member Is Offline
Mood: No Mood
|
|
??? 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.
Women are more perilous sometimes, than any hi explosive.
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
I think it actually is. Not extremely sensitive though
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]
|
|
|
caterpillar
Hazard to Others
Posts: 472
Registered: 8-1-2012
Member Is Offline
Mood: No Mood
|
|
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.
Women are more perilous sometimes, than any hi explosive.
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
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]
|
|
|
caterpillar
Hazard to Others
Posts: 472
Registered: 8-1-2012
Member Is Offline
Mood: No Mood
|
|
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).
Women are more perilous sometimes, than any hi explosive.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
