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Author: Subject: Making own Nitric Acid
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[*] posted on 3-1-2007 at 16:06


Quote:
Originally posted by Aqua_Fortis_100%
guy,
if i attach a blow torch or then even burner with a oxigen cylinder (with proper care..cylinders of compressed gas has a LOT of hazards..) can work well?
but another worry is if the burns is too hot and melt apparatus..
thanks about CuO.. so this project can be really real...
in next holidays certainly i will try..


I think that will work. The good thing is that once it has started, the reaction is so exothermic that it will sustain itself,even melt the copper!

I have tried to do this but never had a good heat source. Maybe you can be the one to finally make it work.

Catalytic Oxidation of NH3 with copper




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[*] posted on 3-1-2007 at 16:14


OH Thanks again guy!
i printed infos from this site, and other site which showns in 1 page of this thread ,yesterday!

about the exothermic reaction: i think which maybe works as solution or as problem ("even melt the copper!")..and from site:

Ammonia is catalytically oxidized at the platinum surface according to the following reaction.
5 NH3 (g) + 5 O 2 (g) ---> 4 NO (g) + 6 H2O (g)
The reaction is exothermic and as written releases 920 kJ of energy. A second reaction proceeds automatically from the first reaction.
2 NO (g) + O 2 (g) ---> 2 NO2 (g)
The second reaction is also exothermic and as written releases 112 kJ of energy.

-------------
How about Another thing which i will try is one "improvised" way to gets HNO3 in another thread where

Quote:
Lambda said:
Making Nitric acid with Potassium permanganate, Ammonia gas and recycling the process with Air (Oxygen) ???



I have forgotten the title of this book, but I think it was written by Robert Gatling. The Paladine Press once published it, and I have the book. When I find it, a scan will be made.

What doese the author of this book claime ?:

According to the author of this book, Nitric acid can be made by bubbling Ammonia gas through a solution of Potassium permanganate. The Ammonia gas is oxidized to Nitric acid in this way. Potassium permanganate may again be obtained by bubbling Air (Oxygen) through this solution (?). And thus, the whole process may be repeated, by only applying Ammonia gas, and again recycling with Air. A continuos process, may thus be astablished for the production of Nitric Acid.

Do you think that this process is feasible ?

but i'm not sure if this method works when anyone wants conc. HNO3, and how to separe the HNO3 from Mn salts solution..(maybe distillation?)....maybe isn't a "EASY" way as showns... how about?

[Editado em 4-1-2007 por Aqua_Fortis_100%]




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[*] posted on 3-1-2007 at 17:21


Quote:
Originally posted by Aqua_Fortis_100%
OH Thanks again guy!
i printed infos from this site, and other site which showns in 1 page of this thread ,yesterday!

about the exothermic reaction: i think which maybe works as solution or as problem ("even melt the copper!")..and from site:

Ammonia is catalytically oxidized at the platinum surface according to the following reaction.
5 NH3 (g) + 5 O 2 (g) ---> 4 NO (g) + 6 H2O (g)
The reaction is exothermic and as written releases 920 kJ of energy. A second reaction proceeds automatically from the first reaction.
2 NO (g) + O 2 (g) ---> 2 NO2 (g)
The second reaction is also exothermic and as written releases 112 kJ of energy.

-------------
How about Another thing which i will try is one "improvised" way to gets HNO3 in another thread where

Quote:
Lambda said:
Making Nitric acid with Potassium permanganate, Ammonia gas and recycling the process with Air (Oxygen) ???



I have forgotten the title of this book, but I think it was written by Robert Gatling. The Paladine Press once published it, and I have the book. When I find it, a scan will be made.

What doese the author of this book claime ?:

According to the author of this book, Nitric acid can be made by bubbling Ammonia gas through a solution of Potassium permanganate. The Ammonia gas is oxidized to Nitric acid in this way. Potassium permanganate may again be obtained by bubbling Air (Oxygen) through this solution (?). And thus, the whole process may be repeated, by only applying Ammonia gas, and again recycling with Air. A continuos process, may thus be astablished for the production of Nitric Acid.

Do you think that this process is feasible ?

but i'm not sure if this method works when anyone wants conc. HNO3, and how to separe the HNO3 from Mn salts solution..(maybe distillation?)....maybe isn't a "EASY" way as showns... how about?

[Editado em 4-1-2007 por Aqua_Fortis_100%]


I don't think the permanganate route is feasible. I once tried putting potassium permangate in ammonia solution and I did not see any MnO2. And O2 cannot regenerate MnO4- because it is not a strong enough oxidizer.




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[*] posted on 3-1-2007 at 17:29


but and the tracherous Mn2O7 gas? mixed with NH3 gas can be a stupid idea? (BOOOM!) or the oxidation isn't too violent?
i think also which make this in gas isn't a good idea, because of the great risks..(with several accidents mentioned in some threads..)
-------
but if anyone will can make a Ozone generator? this is sufficient to oxodize ammonia in NOx ???
thanks

[Editado em 4-1-2007 por Aqua_Fortis_100%]




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[*] posted on 3-1-2007 at 17:40


Quote:
Originally posted by Aqua_Fortis_100%
but and the tracherous Mn2O7 gas? mixed with NH3 gas can be a stupid idea? (BOOOM!) or the oxidation isn't too violent?
i think also which make this in gas isn't a good idea, because of the great risks..(with several accidents mentioned in some threads..)
-------
but if anyone will can make a Ozone generator? this is sufficient to oxodize ammonia in NOx ???
thanks

[Editado em 4-1-2007 por Aqua_Fortis_100%]


Ozone will oxidize ammonia to ammonium nitrite and ammonium nitrate.

from Wikipedia
Quote:

2 NH3 + 4 O3 → NH4NO3 + 4 O2 + H2O




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[*] posted on 3-1-2007 at 18:33


really thanks guy, to shown me the true..
although now i'm dissappointed about ozone and others oxodizers(KMnO4,etc..)..
so i now will concentrate on Cu/NH3 method, and if all gives right, i post my experiments in next holidays... i tried think about some more oxodizer to oxodize the amonia into HNO3 ,but have'nt success..:mad:
with solid oxodizers (alone or in solution) : even if oxodizes ammonia, one will has great problems probably due the difficults in separate this HNO3 from others products,etc moreover can be a lot expensive...
about the gas oxodizers, ozone is now discarded because

Quote:
originally posted by guy
Ozone will oxidize ammonia to ammonium nitrite and ammonium nitrate.


so, others oxodizer as N2O under high temp. can work also (releases more O2 than which air contains..) .. i can meke it simple reacting (NH4)2SO4 with nitrate under heating but should be unfeasible and MUCH more expensive than using free air as O2 source.. but about the measures, i read also in wikipedia which

Quote:

The most important single use of ammonia is in the production of nitric acid. A mixture of one part ammonia to nine parts air is passed over a platinum gauze catalyst at 850 °C, whereupon the ammonia is oxidized to nitric oxide.


wow,apparently my future difficult should be mix in this rate an allow reacting CONTINUOUSLY in homemade NH3 oxodizer (previous)..

aboout nitrate/H2SO4 method ,another thing if anyone has some Ca(NO3)2 , can make relatively "pure"(with slighty amounts of H2SO4 excess or Ca(NO3)2 excess) HNO3 without need destill the mix...simple passing in glasswool for remove the CaSO4 ppt in solution... (although isn't better than conventional H2SO4/nitrate destillation and moreover is almost impossible get HNO3 of high conc.. (maybe using oleum instead????))
using others nitrates as Pb(NO3)2, Ba(NO3)2,AgNO3, etc also will work but i think which this is almost a insane act.. these chemicals , (specially the AgNO3) are even MUCH more expensive than HNO3! and moreover, with these nitrates some fun things can will be created..(as Ag2C2 or Ag3C2NO3, with Pb(NO3)2 is possible to make some monomethylamine nitrate without need HNO3, etc..)
Cu/ammonia maybe will be the future for improvisational chemists!!!

[Editado em 4-1-2007 por Aqua_Fortis_100%]




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[*] posted on 6-1-2007 at 10:18


Quote:
Originally posted by garage chemist
Of course you can also distill fuming acid from conc. H2SO4 and KNO3 at ambient pressure, but it will be only of about 90% concentration and of yellow color, due to slight decomposition.


Can one get a slightly higher yield by distilling at a lower temperature or is the only way to prevent decomposition of HNO3 by distilling at reduced pressure?

BTW, is the use of a certain nitrate in the production of HNO3 just a preference, will they all work, or is there a reason why some use potassium nitrate, others ammonium nitrate, etc?
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[*] posted on 6-1-2007 at 11:03


Quote:
Originally posted by gnitseretni :

Can one get a slightly higher yield by distilling at a lower temperature or is the only way to prevent decomposition of HNO3 by distilling at reduced pressure?


Maybe really reduce the decomposition of HNO3 but in other hand, works too slow if distill in low temperatures using ambient pressure.
so i really need buy all of distill apparatus (specially the low pressures apparatus).. :(

Quote:
Originally posted by gnitseretni :

BTW, is the use of a certain nitrate in the production of HNO3 just a preference, will they all work, or is there a reason why some use potassium nitrate, others ammonium nitrate, etc?


i think which depends of what nitrate is more cheap to one obtains or then, major prefer KNO3 because using NH4NO3 or NaNO3 is more prone to contain some water which prejudices the Fuming HNO3 production.. so who uses NH4NO3 or other hygroscopic nitrate must DRY perfectly instants before distill with high conc. of H2SO4...




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[*] posted on 6-1-2007 at 21:04


Quote:
Originally posted by Aqua_Fortis_100%
so i really need buy all of distill apparatus (specially the low pressures apparatus).. :(


Something like this
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[*] posted on 10-2-2008 at 12:43
68% nitric acid production


I've refrained from asking this, as it seems TFSE should yield the answer I want, but I haven't been able to find a definitive answer. So, I'd like to appeal to those here with direct experience.

I have concentrated sulfuric acid drain cleaner (I haven't titrated it, but I assume it's >90%). I have sodium and potassium nitrate. I have sufficient ST glassware to do straight or fractional distillation. I have some vacuum equipment, but I'd rather not use it if I can avoid it; I don't want to run an aspirator because of a severe regional drought, and I don't want to run acidic vapors through the oil of my mechanical pump.

I want NOT to produce nitric acid in anything greater than the standard 68% azeotropic mix with water. I do NOT want fuming nitric acid, red, white, or chartreuse.

From previous threads, I have the impression that just grinding the NaNO3 and boiling it at standard pressure in the H2SO4 will produce something like 90% HNO3, with lots of oxide contamination. I get the impression that diluting the reaction mix with water might reduce this problem, and allow me to take off the azeotrope (at 120.5C) without significant decomposition. I don't know whether to expect an H2O fraction to come off first. I don't know whether a Vigreux column is necessary, insufficient, or overkill; I'd be inclined to try it without one.

Am I on the right track? Am I on a dangerously wrong track? Any tips on more effective ways to UTFSE -- I've been using Google search with site:sciencemadness.org, as the forum's form-based search engine seems a bit limited.

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[*] posted on 10-2-2008 at 13:50


You're on the right track. Read the following thread:

http://sciencemadness.org/talk/viewthread.php?tid=1851&p...

If you still have questions just fire away. ;)




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[*] posted on 10-2-2008 at 14:00


First off, how much acid are you in need of?

With a water/ azeotrope boiling point separation of only 20C, I would be inclined to use a vigreaux collumn.

You will not want to use concentrated sulfuric acid with the nitrate, as that will produce a ~65C fraction of fuming red acid if done under atmospheric pressure. The sulfuric should be diluted to such a concentration that when you calculate it out, there is enough water, plus a slight excess, to not have greater than azeotropic acid when mixed with nitrate. Then fractionally distill with the vigreaux collumn, you should collect a small ~100C fraction of water, then collect the ~120C fraction of azeotropic acid

This thread(http://www.sciencemadness.org/talk/viewthread.php?tid=4689&a...) discusses azeotropic distillation, but if I can find a more applicable thread, I will merge this into it.




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[*] posted on 10-2-2008 at 14:16


Quote:

I don't want to run an aspirator because of a severe regional drought,


A minor point, but you could use a closed system with a pump instead
of attaching the aspirator to the sink. Of course there is the issue of
the acidic vapors dissolved in the water not being too good for the
water pump, but this might not be so bad because a. they would be
diluted, b. something like the typical plastic sump pump should stand
up to dilute acids just fine and c. one could always add some soda to the
water to neutralize the acid.
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[*] posted on 10-2-2008 at 15:33


Quote:
Originally posted by The_Davster
First off, how much acid are you in need of?


Well, technically, I guess I don't need any. :P I'd probably be looking at something on the order of a hundred grams at a time. Going large, I can't imagine ever making more than a kg at a time. Going small, my gear is 24/40, so running down in the 10g scale would probably mean I'd hold up more product than I'd collect.

Quote:
With a water/ azeotrope boiling point separation of only 20C, I would be inclined to use a vigreaux collumn.

You will not want to use concentrated sulfuric acid with the nitrate, as that will produce a ~65C fraction of fuming red acid if done under atmospheric pressure. The sulfuric should be diluted to such a concentration that when you calculate it out, there is enough water, plus a slight excess, to not have greater than azeotropic acid when mixed with nitrate. Then fractionally distill with the vigreaux collumn, you should collect a small ~100C fraction of water, then collect the ~120C fraction of azeotropic acid

This thread(http://www.sciencemadness.org/talk/viewthread.php?tid=4689&a...) discusses azeotropic distillation, but if I can find a more applicable thread, I will merge this into it.


That's exactly the kind of information I'm looking for. Thanks, and thanks for moving this to the appropriate spot!



(EDIT By Davster: Credit where it is due, my laptop froze, and when I bothered to restart a couple hours later, someone else moved it here.)


[Edited on 10-2-2008 by The_Davster]
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[*] posted on 10-2-2008 at 15:35


Quote:
Originally posted by microcosmicus
Quote:

I don't want to run an aspirator because of a severe regional drought,


A minor point, but you could use a closed system with a pump instead
of attaching the aspirator to the sink. Of course there is the issue of
the acidic vapors dissolved in the water not being too good for the
water pump, but this might not be so bad because a. they would be
diluted, b. something like the typical plastic sump pump should stand
up to dilute acids just fine and c. one could always add some soda to the
water to neutralize the acid.


Interesting idea. I'd sort of assumed that an aspirator would require more head pressure and/or flow than a small, cheap, not intolerably loud pump could provide. I already have a closed system for cooling water -- a box on wheels I bought at surplus, containing a tank, a stirrer, a peristaltic pump, some tubing, and a pressure gauge. For that matter, I suppose I could rig a small aquarium pump for circulation, and use the peristaltic pump for vacuum, as discussed in a recent thread.
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[*] posted on 16-2-2008 at 20:38


So I'm thinking about testing the viability of a batch process to produce easy NO2 from NH3 and O2. I'm thinking some kind of steel vessel that you could simply fill with NH4 and then pressurize with O2 from a torch up to the appropriate ratio of gases. A copper wire of decent thickness could be electrically heated to initiate the reaction.

What I'm not sure about is how much NH4NO3 would be produced, thus wasting the NO2. Do you think this would be a problem? I'm going to try to test it on a small scale tonight if all goes well.

Edit:

Not good results, it mostly produces a cloud of ammonium nitrate. Too bad. I'll have to try something else.

[Edited on 16-2-2008 by 497]
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[*] posted on 2-3-2008 at 13:46


Sorry for digging up this old thread but I have a question. I would like to distill nitric acid in an all glass distillation setup (no shortcuts) but from what I have read the resulting nitric acid will be of the red fuming variety. Wouldn’t that mean its no good for nitrations? If so is there a way to avoid the red fuming variety? Also in the TNT preparation thread there is mention of reusing acids by heating 70% nitric with 93%-98% sulfuric acid resulting in 99% purity. Would this be white fuming or red fuming nitric acid? If it is white fuming what would be a good ratio of 70% nitric acid to 98% sulfuric acid (not spent acid) to distill 99% nitric? Thanks for all the help.



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[*] posted on 2-3-2008 at 14:31


The nitric acid indeed contains some NO2. I myself also did this distillation, and I obtained some yellow acid, which I think has concentration better than 90%. One way to get rid of the NOx is the addition of a small amount of urea. This reacts to form N2, CO2 and H2O. It of course does decrease the concentration of the acid a little, but if you start with yellow acid, then the decrease is not dramatic.

This is the setup I used for making a small amount of the concentrated acid:

http://woelen.homescience.net/science/chem/exps/raw_material...

I understood (but did not try myself) that redistilling the red or yellow acid in vacuum allows for a much whiter acid, if the first part of the distilled matter is discarded (it contains the NOx). The last part of the distilled matter also should be separated as well (it is more dilute, its concentration goes towards the azeotrope of 68%, don't discard it, its useful for other things, but keep it separately).

Edit(woelen): Made link work again.

[Edited on 30-7-16 by woelen]




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[*] posted on 30-5-2010 at 15:52


Manufactue of Nitric Acid
http://www.platinummetalsreview.com/pdf/pmr-v11-i1-002-009.p...

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[*] posted on 3-9-2010 at 14:08


Nurdrage made nitric acid with reaction of nitrate salt, hcl and copper to make no2 and dissolved it in the water to make HNO3.

I am interested in doing that, but I am afraid of NO2 poisoning. Is it really that dangerous?
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[*] posted on 3-9-2010 at 21:48


Quote: Originally posted by Random  
Nurdrage made nitric acid with reaction of nitrate salt, hcl and copper to make no2 and dissolved it in the water to make HNO3.

I am interested in doing that, but I am afraid of NO2 poisoning. Is it really that dangerous?


You can make a very weak Nitric Acid that way. As long as you don't breathe the NO2 you will be fine. The smell is obvious if you get a whiff.
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[*] posted on 4-9-2010 at 08:53


What could happen if I will get more than a whiff?
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[*] posted on 4-9-2010 at 11:11


If you do the chemistry outdoors or in a fume hood, and don't stick your face in the beakers, you are not going to get more than a whiff.

I've done chemistry where I made tons of NO2 and did it outside. The gas is dark brown and obvious.
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biggrin.gif posted on 8-9-2010 at 07:45
HNO3 from Aluminum Nitrate + H2SO4 electrolyte


It has been an intriguing idea for which I have never done any experiments to see if this idea would work or not. But it may be possible to use a cheap alternative nitrate precursor which may produce a good, possibly better yield of nitric acid from the distillation using H2SO4 by reacting with both hydrogens of H2SO4 rather than just one, not producing an acid sulfate byproduct "niter cake" as is the usual result, but producing a normal sulfate byproduct instead, thereby also producing twice the amount of HNO3 from the same amount of H2SO4, which would be a doubling of the efficiency of the commonly known reaction. A nitrate of a metal which may possibly work in this manner is Aluminum Nitrate, Al(NO3)3. Aluminum Nitrate could possibly be gotten from amalgamated scrap aluminum decomposition in an ammonium nitrate solution. Alternately the reaction of Calcium Nitrate with Aluminum Sulfate may be convenient,
and would provide a recycle loop for the Aluminum Sulfate byproduct, if Calcium Nitrate is the easily available nitrate feedstock. The terminal waste byproduct of the process would be Calcium Sulfate, gypsum. Because of the water sequestering properties of both the Aluminum Nitrate and the Aluminum Sulfate byproduct in the distillation mixture, a lower concentration H2SO4 may be workable for producing a higher concentration HNO3 distillate since both salts would tend to break the azeotrope in the reaction mixture itself.
How pronounced would be the effect is not known but it would seem possible that even ordinary electrolyte strength H2SO4 may be sufficient for distillation of azeotropic HNO3.
This has not been described in the literature which I have read and I really don't know if it would work or not, but the idea is certainly intriguing and is on my experiments to do list.

There is a decomposition temperature for Al(NO3)2 at 14C higher than the temperature of distillation for azeotropic HNO3, but that seems to be an acceptable margin for a carefully conducted process, unless the decomposition temperature is lowered by the acid conditions of the reaction mixture .....which could be the "hitch" that may prevent the process from being workable.

2 Al(NO3)3 + 3 H2SO4 -----> Al2(SO4)3 + 6 HNO3

Anyone having any further information on this idea for
possible use of Aluminum Nitrate as an HNO3 distillation precursor please share your thoughts and / or information :D

It seems likely somebody may have already been there - done that, and it is just an obscure matter for which I haven't found a thing written ...yet.

[Edited on 8-9-2010 by Rosco Bodine]
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[*] posted on 8-9-2010 at 10:06


Al(NO3)3, hygroscopic, normally containing considerable water of hydration and decomposing below 140*C doesn't IMO, look very promising as a source of HNO3.
If it was a viable method, I think it would be fairly common knowledge. . .
If it can be dehydrated without the salt decomposing it might have interest.




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