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Author: Subject: Making own Nitric Acid
guy
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[*] posted on 27-11-2005 at 21:53


This site shows the video of the catalystic reaction of NH3 and O2 using copper in a lab. The reaction is hot enough to melt the copper.
One could make a design to collect the gas and dissolve it.




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[*] posted on 28-11-2005 at 18:52


I made some nitric acid today but had to abort about 2/3's of the way through the run due to foaming.

I don't know if this foam is normal or a result of contaminants in one or both of my OTC reactants. I used 236 g of Dexol stump remover and 122 mL of Rooto drain cleaner, and 50 mL water.

I used a 500 mL RBF which is my largest. I would have liked to have had a 750 or a 1-liter to deal with that foam. I cut the heat wnen the foam ran away but it carried reactants all the way into the condenser before subsiding. I have saved everything and will continue tomorrow. I will have to redistill to purify. I'll post pictures when I finish.

Hood works great - didn't smell any NO2 or nitric acid. The downside is that it is tough to keep the lab warm when it is in operation. But it is definitely worth it. ;)




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[*] posted on 29-11-2005 at 21:14


Finished my nitric acid preparation today. After cleaning up the condenser, etc, I just started up where I left off. Put an aluminum foil tent around pot and distilled away without incident. Never had more than 15 mm of foam. Then redistilled the 1st batch for a combined 95 mL distillate, 62% yield overall. Neutralized the waste salt brine with bicarbonate of soda and disposed down the drain.

Here's a picture with the brine carryover into the condenser and receiver. Also shown is a picture of a Keck clamp that died for the cause. I must have had a joint that wasn't aligned right and it leaked hot nitric acid vapor. It's good to have a hood.

The 2nd picture doesn't want to load but you can see the failing clamp at the top of the Claisen adaptor.

[Edited on 30-11-2005 by Magpie]

foam carryover - nitric acid.JPG - 405kB




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[*] posted on 30-11-2005 at 04:38


I had the same problem with a keck clamp, i used it for my buchi rotavapor for distillation of HNO3... it was a completely new clamp :mad:

PhZ claimed to have used a rotavapor for HNO3 distillation advantageously...so i tried the same.-Only difference: atmospheric distillation.

As i expected, the distillate was quite yellow, at least not deep red...
The rubber sealing of the rotavapor did suffer a lot(it´s made of nitrile rubber or something, but that was too much) although it was not completely destroyed, there was a lot of abrasion. :(
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[*] posted on 16-12-2005 at 19:12
Yet another idea for HNO3 production at home.


I don't know why I keep thinking about this. Maybe the idea of making something as useful as HNO3 from air and water, using some relatively simple (hopefully) apparatus, especially in an era when corrupt governments are prone to restrict access to such things, is just too romantic to easily give up on.

I didn't realize that some commercially available high-end heat guns claim to be able to reach 700 degrees C (although they apparently require 2kw or so of power to do it).

Anyway, this temperature exceeds the recommended lower limit of 500 degrees C for producing nitric oxide by way of the method of US patent 5692495, i.e., by "passing air, oxygen enriched air, or air containing a small amount of ammonia, over a noble metal catalyst at an elevated temperature".

I wonder if something as simple as a heat gun blowing 700 degree air over a piece of platinum catalyst from an automobile catalytic converter, for example, can ultimately produce a useful amount of HNO3?

I've been looking all over the place but unfortunately I haven't been able to find any additional information or documentation regarding this method of producing NO.
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[*] posted on 16-12-2005 at 19:58


I would suggest... bubble air through an ammonia solution of some concentration. (If necessary, dehydrate the air stream with KOH.) Then lead the gas through a heated copper tube. It's quite easy to heat 3/16" or so oppper tubing to red heat with a small propane torch or bunsen burner. The copper catalyzes the reaction, and if you apply insulation (kaowool or glass wool) it may even sustain itself. Then lead the gasses into more oxygen, if neccessary, to produce NO2, and bubble this into a water solution, or alkali solution if you want faster scrubbing results.

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[*] posted on 16-12-2005 at 21:23


That sounds entirely workable to me, and would perhaps lead to a higher rate of production, but at the expense of somewhat more complexity, I would say, both in construction and in operation.

However, the requirement for ammonia (ubiquitous and cheap though it may presently be), nevertheless makes the process dependent on an ingredient that is strictly the product of a large industrial process (that could theoretically become "regulated" someday)...and this makes the process inherently less appealing to me than one requiring only air and water.

[Edited on 17-12-2005 by jpsmith123]
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[*] posted on 17-12-2005 at 00:33


Just a quick jump in...

But it was posted:

"passing air, oxygen enriched air, or air containing a small amount of ammonia, over a noble metal catalyst at an elevated temperature".

I read that as oxygen enriched air OR air with ammonia...




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[*] posted on 17-12-2005 at 02:08


Hello Duster,

You're right, the patent mentions the use of air with ammonia as an option; personally however, I just have a fetish for doing it without depending on anything like ammonia, if possible.

Also, as a practical matter, I would be willing to trade some amount of production rate and/or energy efficiency, in return for not having to worry about maintaining an ammonia generator and the possibility of an unwanted byproduct of NH4NO3.
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[*] posted on 17-12-2005 at 07:11


Since a setup like this could run for hours on end without ill effect is properly designed, I would think the marginal loss of some production at the lack of an ammona generator would be an acceptable tradeoff. It would be intresting to know what sort of rate of production could be achieved by this method. After all, air is pretty abundunt :)



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[*] posted on 17-12-2005 at 10:22


>ammonia ... could theoretically become "regulated" someday...

Aqueous ammonia used for cleaning is unlikely to become severely regulated anytime soon. If all else fails, we can always resort to ammonium salts and bases.
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[*] posted on 17-12-2005 at 10:54


Ammonia isn't going to get meaningfully regulated any time while people still produce urea.
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[*] posted on 17-12-2005 at 15:31


I used to live in the U.S., now I live in a country that has "banned" all nitrates, chlorates and perchlorates, and probably other chemicals that I'm not yet aware of.

You may be right about ammonia, but it seems there is no limit to government irrationality and abuse, whether in the U.S. or elsewhere; so nothing is out of the question, IMHO.
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[*] posted on 17-12-2005 at 19:44


As long as fertilizer companies pay politicians, ammonia will be legal.

Now, back to the regularly scheduled topic.

Just leading the air/ammonia mix through the tube will only expose the outermost part of the gas stream to copper. Will this be a problem at this diameters?
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[*] posted on 17-12-2005 at 20:14


Well you could do what Organikum did, plating copper onto steel wool, and shoving that down the copper pipe to increase the surface area on the copper.



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[*] posted on 17-12-2005 at 20:16


I suppose it would depend on the geometry and construction particulars; e.g. the length of the tube, the velocity and turbulence of the air-stream, etc.

If I were going to do it this way I would probably put some "chore girl" copper scouring pad material in the tube to prevent that.

Then I would exhaust the copper tube into a stainless steel tube (or maybe glass tube with stainless steel scouring pad inserted) into which I would also inject more air for the NO to NO2 part.
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[*] posted on 2-7-2006 at 16:04


Quote:
Originally posted by neutrino
I can't remember who it was, but someone here talked about distilling at atmospheric pressure vs vacuum. Their conclusion was that a vacuum distillation was no better for decomposition that atmospheric distillation and that most of the decomposition that occurred could be blamed on sunlight.

I can't remember any specifics or which post it was. Maybe someone here remembers, I'm too busy to find it right now.


I remember ..... It was me . Ammonium Pyrosulfate was the thread I started about the dehydration of the ammonium bisulfate niter cake which remains as a residue after HNO3 distillations using ammonium nitrate and H2SO4 . The details of the distillations were described .

https://sciencemadness.org/talk/viewthread.php?tid=4689#pid5...
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[*] posted on 1-1-2007 at 20:35


Sorry to resurrect an old thread, but my lab partner (NERV) and I are distilling more nitric acid tonight and figured we would show some pictures of our setup.

We used dirty KNO3 (obtained for about .68 USD/ lb) and drain quality 95% H2SO4 to make this red fuming product. Upon dilution and addition of AgNO3, no clouding or precipitate is observed, so it's at least free of HCl.

First picture is it stored inside PFA 2L bottles (more or less teflon) we took tonight. Second is of it collected in a 1000mL RB flask. Third and final is the distillation setup with 5L 2 neck RBF and 700mm liebig. Those last two are old, but we've been meaning to post them up for some time. BTW, in the small beaker with the yellow solution, that is KCl/HAuCl4 solution for plating.










[Edited on 2-1-2007 by Fleaker]

[Edited on 2-1-2007 by Fleaker]

distillation app.jpg - 163kB




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[*] posted on 2-1-2007 at 22:17


Hello all..
i finish now to read all posts.
i tried ONE time the nitrate/H2SO4 method and mine HNO3 was too weak and expensive which i never more tried..(my problem is the very poor and improvised glasswares, but i will still try the Brainfevert's method...

so if i wish will try anothers methods, as the NH3/Cu at home...
if anyone will can help me about the NH3/Cu method (at home) (if is really reliable, what the major problems which i can have,etc), i try plain in future something based in this method ...
i now imagining something about this method and searching in web..
apparently the problems which i will can have are the oxidation of copper( if generates CuO, this still can work as catalyst????), obviously the nasty effects of ammonia or NOx on body (making the stuff in outside is a cool thing :D ), etc..

big thanks...
(and also sorry to resurrect an old thread)

[Editado em 3-1-2007 por Aqua_Fortis_100%]




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[*] posted on 3-1-2007 at 03:26


I think the dry distillation of AN is the usual method of making N2O (nitrous oxide)

And the explosition hazard is only if you accidentally distill the melt to dryness. HOWEVER I am pretty sure this is done with AR grade ammonium nitrate rather than agro fertilizer.

If you have access to H2SO4 why not ptoceed from KNO3 which is generally not as "suspicious" as AN? Sodium bisulphate (sodium hydrogen sulphate) would be a workable substitute.

Can't you buy battery acid? That's H2SO4 and almost as concentrated as the standard lab acid.

Using KNO3 (saltpeter) avoids the explosion risk of AN entirely.
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[*] posted on 3-1-2007 at 11:41


Sauron,
about nitrate/H2SO4 method, the AN should be better because is usually more cheaper than KNO3 or even NaNO3, but this should preheated to dry and no to affect the conc. of HNO3(as NaNO3 - if one wants the >95% HNO3 and using low pressures).. but if anyone as Magpie wants the 68% grade, isn't necessary pressure apparatus and the AN work well...
Quote:
Can't you buy battery acid? That's H2SO4 and almost as concentrated as the standard lab acid.

here the battery acid is no more than 40% (usually 30% or less from used batteries)
i really need buy the 98% grade, but i'm have the "right" age which the local law need ( "older than 18 years and no more than 2 liter of 98% lab grade by mounth without to present documents", etcetera...)
so my source is bring to boil the baterry acid..is free but NOTHING fun...
-----



[Editado em 3-1-2007 por Aqua_Fortis_100%]




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[*] posted on 3-1-2007 at 15:38


<IMG SRC="C:\Documents and Settings\Carlos\Meus documentos\Minhas imagens\Pyroimages\homemadeNOxandHNO3fromNH3.bmp">

[Editado em 3-1-2007 por Aqua_Fortis_100%]




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[*] posted on 3-1-2007 at 15:39


Firstly sorry all about the crap Cu/NH3 design above made in Paint yesterday (is poor because i'm
a newbie even in Paint!!!!), my english, some stupid idea, and also by made two post instead of one
(i tried for 2 HOURS(!!) upload the image ,but without sucess(not showned).only now i tried to modify
the image then works when uploading... so i made two posts to try avoid which image not shown..

I'm interested in this because which is a apparently easy method for HNO3 production at home (although isn't as H2SO4/nitrate method) using raw apparatus (which is VERY convenient for me) :D .
This image was based in some (sufficient?) search about catalytic oxidation of ammonia.
almost nothing was found in web about experiments using Cu as catalyst, so i tried search
in this forum and others..
if anyone tried this method or similar, please tell me all and details...
also,if anyone comments this design i really like, even if to only criticize me .
but some questions still affect me:
if the copper is oxodized , the CuO formed still works as catalyst (mentined by Darkflame89) ? if no, is feasible
running a CO or H2 gas in hot CuO to regenerate copper???
any impuritie (as arsenic,etc) in copper can "poisoning"and disturbing terribly the catalyst function of Cu???
Also, problems with unreacted NH3 and NH4NO3 formed..
is possible with this method make great quantities of HNO3 at home? very concentrated???
thanks..
well, about the numbers in design , it's significate which:

1 - ammonium salt/lye/some water to produce NH3 (another question is about how controling the gas flux..i tried put some faucets in design, but i'm really sure which this work best..)
2 - a Hairdryer or , air bubbler(from aquarius) or something to introduce air in system (althoug the hair dryer consume more electricity and as a disadvantage of overheating which was commented by trilobite in another thread..
3 - socket
4 - pieces made from PVC tubes , and some tape to connect them to big plastic bags or gallons containers(as in design) and some sealant or glue for no gas leak..
5 - gallon container or something to mix better the NH3 and air ( now i think which is better a plastic flexible bag , because if applied pressure in them, is better for do a gas stream flux in copper apparatus )
6 - pvc pipe caps sealed with a convenient glue for no gas leak..
7 - (old) faucets to regulate the gasses flux and allow good mix of the gasses..
8 - plastic hoses
9 - long column made with CaCl2 from antifungal or another convenient dissecant agent,to dry the mixed gasses...
10 - small metallic pipe or tube (preferably made with any metal HNO3 resistant) and some PTFE tape..
11 - coke glass bottle :D
12 - several (homemade) burners..another worry mine is which if a common alcohol burner (which releases relatively low temperatures) can works with this (???), how about a camp gas stove ??? what THE BEST temperature for this, and what the critical temp.(which the formed NO or NO2 can starts to decompose)???
13 - glass tube (from luminiscent Hg lamp).
14 - container with cooled water to receive the NOx and forms HNO3
15 - another container with cold water-ice
16 - glass "cone" made from cutted coke bottle, attached to end of glass tube (works increasing the surface of gas which has contact with water, i think..)
17 - several thin copper pipes and theirs caps (one attached to other by end) - (maybe thin steel or brass pipes works also (and do the project more cheaper). my worry is about the corrosion..the most important it's the pipe filler with Cu things..)
18 - suports for pipes
19 - pipe filler material: several Cu things as Cu plates, wires, coarser powder or fine (CuSO4 + Zn),maybe the Organikum idea ,using steelwool with copper powder ppt on this..but my big worry is if steelwool not burns with the elevated temperatures and with O2 (from NH3/air) passing through it..


edit: the brown pipes which i forget, is a steel or iron tubes which works to reduce progressively the temperature to glass(no pirex) apparatus and avoid termal "stress" of home glass..

[Editado em 3-1-2007 por Aqua_Fortis_100%]

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

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




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[*] posted on 3-1-2007 at 15:47


The idea is that CuO oxidizes NH3 to NO gas.

Unbalanced equations:

CuO + NH3 ----> NO + Cu + H2O

Cu + O2 ---> CuO
-------------------------------
NH3 + O2 ---> NO + H2O

YOu need very high temperature to selectivly produce NO or else you just get N2 or N2O.

[Edited on 1/3/2007 by guy]




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[*] posted on 3-1-2007 at 15:53


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..




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