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DetaDude
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hissingnoise
I was just refering to the use of ozone as a super oxidizer for use in other chem. syntheses.
I've overcome most of the pitfalls in the production of ozone . I just have not used it for chemistry stuff.
Many years back I developed an ozone generator, that runs on a 15KV neon transformer and now I'm looking to improve it with an oxygen concentrator,
much like what they use for medical breathing therapy ..
Genius creates many a great works............Labor alone finishes them!
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hissingnoise
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You're right DetaDude, I was being overly pessimistic. . .
Moist air in an ozone generator leads to the production of NOX and if the air-moisture could be controlled within tight parameters a mixture of NO2
and O3 might be formed.
After being given time to react the exhaust might consist of N2O5, theoretically, though some NO2/O3 would likely still be present.
All that's required then is dilute acid or water for absorption of the anhydride.
100% HNO3 will dissolve a sizable quantity of N2O5, leading to the nitric acid equivalent of oleum.
Of course it's easy to say. . .
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DetaDude
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I've found out through research on this subject that the time factor is more important than the moisture, but both play a part.
It seems that the speed at which the O2 (or air) moves through the ozone generator more or less governs which gas in made in the majority slow=nitrous
fast favors ozone.
As soon as I get my hands on a concentrator and hook it up to the O3 unit I'm going to play around with some HNO3 and a few other things.
Genius creates many a great works............Labor alone finishes them!
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hissingnoise
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A Jacob's Ladder could be configured in such a way that ozone would be produced along with NO2.
Output would be very small but running it continuously would build product over time.
I fear though, we may be clutching at straws.
KNO3/H2SO4 is triedand trusted.
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malford
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Some searching brought this thread to my attention, though the first couple of pages brought me disgust. It's opening post is exactly the discussion I
am looking for. However, I must preface my post with the declaration that crazyboy, entropy51, bbartlog and others involved are the top three least
sensible, to put it kindly, individuals whose writings I have read or ever will read. The unlikely alternative, of course, is that he or she each are
exceptionally skilled at trolling.
Delta specifically stated he was looking for anecdotes from using a reflux condenser (in other words, a condenser that is designed to be used for
reflux) for distilling nitric acid with the rest of the setup being that of a typical distillation. This is something I have wondered about myself. In
the unlikely event that he meant using an intact reflux setup for distilling nitric acid, even then, an ounce of brain matter should be sufficient to
conceptualize how this would work. I have even thought of using this myself previously. Examine this part. The boiling flask would be connected to the lower, right inner joint. The reflux condenser would be connected to the upper, left outer
joint. A collected flask would be connected to the lower left stopcock.
More on topic, 70% nitric acid and 98% sulfuric acid are very readily and cheaply available to anyone in the US and probably elsewhere. As such, I am
distilling the nitric acid from a mixture with the sulfuric acid. This seems to be one of the most effective approaches available to me for highly
concentrated nitric acid. I am looking for more information on what exact compounds are formed when the 30% water from the nitric acid is reacted with
the 98% sulfuric acid. Will this newly formed compound be azeotropic with nitric acid? If so, at what point is the azeotrope?
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testimento
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One shall do following reaction:
1) Roast some calcium carbonate to calcium oxide
2) Mix it with water to get hydroxide
3) Get some otc fertilizer (active ingredients are mostly AN and urea), dissolve'n'filter'n'evaporate
4) Mix CaOH into it at saturated, near-boiling water solution and lead evolving ammonia into water to recover it
5) Boil off the residual water and heat up to 500C and take the evolving ammonia and isocyanic acid fumes by leading them into water trap
6) Roast the residue, which is calcium nitrate, and it will decompose into nitrogen dioxide and calcium oxide
7) Lead NO2 fumes into water to get nitric acid up to 68%
8) Perform an azeotropic vacuum distillation to acquire WFNA
9) Reuse the CaO
1kg of calcium carbonate with 1600g AN will produce 1260g of 100% HNO3 at 100% efficiency, practically yields of 800-1000g should be achievable.
For lazy bastards, mixing hydrochloric acid with ammonium nitrate will yield ammonium chloride and nitric acid.
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Oscilllator
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Quote: Originally posted by testimento  |
7) Lead NO2 fumes into water to get nitric acid up to 68%
8) Perform an azeotropic vacuum distillation to acquire WFNA
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What??
Firstly, you can theoretically achieve 98% nitric acid by the absorption of NO2 vapors. This is how its done on an industrial scale, although
admittedly it probably isn't practical for the home chemist. (source: wikipedia)
Secondly, I fail to see how an azeotropic vacuum distillation will get you above the azeotrope... assuming that by WFNA you mean nitric acid of a
concentration greater than 95%? (definition of WFNA taken from wikipedia)
Also, do you have any sources for the production of calcium nitrate using that method?
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DetaDude
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Malford..................Thank you for your kind understanding, and your ability to understand the Kings English.
Some of those that respond here do not seem to have a very good grasp of common sense and understanding. Hissingnoise has a great deal of
comprehintion and you also seem to "get it".
Thanks again DetaDude .
Genius creates many a great works............Labor alone finishes them!
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malford
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I can now answer my own question from my previous post above.
Examine this: http://www.akersolutions.com/Documents/PandC/Mining%20and%20...
On page 2, the chart shows that 50% by weight of sulfuric acid added to the nitric acid eliminates the azeotrope. The question then becomes, what is
the vapor composition with this mixture? Using the answer to that question, we can determine whether a single distillation will suffice or many
theoretical plates are needed.
If anyone has or knows how to figure what the vapor composition is of a ternary mixture of nitric acid, water and sulfuric acid, then my appreciation
would know no bounds.
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Magpie
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The sulfuric acid is basically non-volatile at the temperatures used to distill over the nitric acid. Measure the density of your product and by
using a handbook table you will find the concentration. Or titrate it.
The single most important condition for a successful synthesis is good mixing - Nicodem
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testimento
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| Quote: Originally posted by Oscilllator |
Firstly, you can theoretically achieve 98% nitric acid by the absorption of NO2 vapors.
Secondly, I fail to see how an azeotropic vacuum distillation will get you above the azeotrope...
Also, do you have any sources for the production of calcium nitrate using that method? |
Alkali mixed with ammonium nitrate will yield ammonia and calcium nitrate.
Azeotropic distillation is performed mixing the nitric acid with sulfuric acid, as stated. The SA is recoverable by boiling off the water.
I noted the practical yield being 60-80% max.
Anyway, that's how one can get either dilute HNO3 up to 68% without SA, or conc. HNO3 with SA, both ways without wasting any acid.
Many nitrations can be carried out using fuming nitric acid, so I don't see any single practical reason to waste - for most people - precious sufuric
acid for it, if it can be avoided. For ex. PETN synthesis yields quite an equivalent amounts of product with, and without.
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