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Author: Subject: Druken Aga Challenge (DAC) #3 - Closed (but open to discussion)
blogfast25
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[*] posted on 2-8-2015 at 09:38


Dangle89:

The amounts (concentration) of NO<sub>x</sub> in non-catalytically treated exhaust gases is very small. Apart from the inherent problems of processing large amounts of hot gas, this is by no means a practical method of preparing nitric acid.

[Edited on 2-8-2015 by blogfast25]




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[*] posted on 2-8-2015 at 10:03


Quote: Originally posted by Dangle89  
I believe Aga said distillation is allowed :)

Distillation is fine.

Just not KNO3 (or any other nitrate salt) with H2SO4




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[*] posted on 2-8-2015 at 10:04


Quote: Originally posted by Dangle89  
I believe Aga said distillation is allowed :)

Distillation is fine.

Bashing it 5 times a second with a hammer is also fine.

Rubbing it rapidly between burnt bamboo stems is also good.

Just not KNO3 (or any other nitrate salt) with H2SO4

[Edited on 2-8-2015 by aga]




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[*] posted on 2-8-2015 at 15:07


Scrubbing the exhaust from a combustion engine was an idea I had too. And i had an old lawnmower engine that I could use. ("Had". It's gone now. It was beyond repair as it turns out -- at least with my skills.)

Other than the fact that I couldn't get the mower to work, I abandoned the idea for two reasons.
1) Oxidation of atmospheric N2 really only happens at high temperatures. I wasn't confident that the engine I had would get there -- particularly without a load on.
2) I could think of better things to do than spending several hours babysitting a noisy engine at high revs blowing bubbles in a bucket.
3) It seemed like a good way to get carboxyllic acid that I would then need to separate from the nitric acid. I figured CO2 would displace a lot if not all of the dissolved NOx.
4) I reasoned that nitrogen in the fuel was going to give a better yield than incidental reactions with N2 in the air.
5) I never was much good at counting.

J.
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[*] posted on 3-8-2015 at 03:51


Ok I am back on this :D, I have a source for ammonia thats a bit wild lol but getting from ammonia to nitric acid without platinum is my sticking point. can it be done without the catalyst? my source for ammonia is maggots! Ive checked and double checked and they produce loads if you keep them 3-4 days in a bait box with sawdust and few vent holes (tiny ones) then clean them with clean sawdust and repeat for second load sawdust soaked in ammonia. I also found a paper on maggot treatment that also states they produce ammonia, ok its not huge amounts but I have 10 pints of them on the go and a fair bit of liquid to process. Next step is how can I get that to the monoxide?



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[*] posted on 3-8-2015 at 05:22


Aga can we use a battery and copper wire? I cant remember all the rules. I used an aquarium test kit and sure enough the maggot liquid is off the scale for ammonia even diluted 20x :D. Still totally unsure how to get around the platinum but there must be a way :D



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[*] posted on 3-8-2015 at 19:44
copper method


So I'm back after much ruminating and I have a theoretical reactor design with one or two kinks to be worked out yet.

step 1: acquire a copper cooling unit. I used the radiator from an old dehumidifier, however an old window AC would work.

step 2: obtain ammonia (for my purposes source doesn't matter, but for the competition one could boil down urine or some such)

step 3: strip the a aluminum fins off a short section in the middle of the unit. My thought process is leave just enough fins on to cool the reaction and prevent a copper melting runaway while leaving a section behind to fully cool the gasses to room temperature. (sorry if this is confusing, please ask for clarification if needed)

step 4: walk into fleet farm or a hardware store and pick up a small oxygen tank for around $5 USD

step 5: Set up a beaker and attach a rubber/vinyl/whatever hose from the beaker going to a T where the O2 and the NH3 can mix (make the O2 adjustable to optimize the reaction?). Then pipe this into the copper unit. Pipe the exhaust into water/H2O2/silica gel.

step 6: here is where the kinks come in. if you have anhydrous ammonia laying around in your shed this is pretty easy Pour NH3 in the flask, allow it to boil off. turn the oxygen on and then pre-heat the barred copper line to a red glow with a torch.
step 6b: obtain .880 ammonia either as is or through concentration. boil this off into the line. proceed as above. Be wary of water vapor forming HNO3 in the copper tubing and dissolving it.
step 6c: get dilute ammonia, boil off as above, and find a way to dry the ammonia vapor.

Thoughts: Running Oxy through rubber/vinyl line poses a fairly large fire/explosion risk, especially near red hot copper. This is kink one, how to do this without risk of lighting the oxy/vinyl line on fire. The second problem would be how to dry ammonia gas. From the research I've done CaCl won't work as it forms a complex, neither will conc. H2SO4 due to acid base reactions, and MgSO4 will form MgOH.
Finally, I'd recommend a large bucket of water nearby in case of a meltdown and a fire extinguisher in case the oxy gets away on you.

Thoughts, comments, questions or concerns are welcome!
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[*] posted on 4-8-2015 at 04:44


Ah cool cool :D

Just though I would chuck it out there in case it was one of those things that are so simple it gets over looked by accident!

Did some more research on it and is definitely not simple! On an industrial scale it is possible but would not fit our desert island scenario!

On that, Just wondering why Pt was deemed out of bounds? Happy with the rule as it is expensive and wouldn't be a "cheap" method, which was one of the goals, But surely Pt could be obtained anywhere in the world OTC at a jeweler or bullion dealer (or maybe the Island has Pt nuggets in the river or buried pirate treasure :P)?

Aga, you would be surprised at how many things you can fix in mechanics by bashing them with a hammer 5 times a second :P
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[*] posted on 5-8-2015 at 09:05


I am thinking electrolysis of water for oxygen and bubble that into it. first trial tomorrow, how do I titrate ammonia? smells pretty strong so maggots seem great at ammonia production and if you killed your mate on the desert island you would have loads of maggots after a couple of meals of course.



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[*] posted on 5-8-2015 at 10:37


Quote: Originally posted by NWS  
The second problem would be how to dry ammonia gas. From the research I've done CaCl won't work as it forms a complex, neither will conc. H2SO4 due to acid base reactions, and MgSO4 will form MgOH.


You can dry NH3 with alkali and alkaline earth oxides and hydroxides. CaO works well, as does NaOH or KOH. First run it through a really cold and efficient condenser which will remove most the water, then use the chemical water trap. You may also be able to use molecular sieves or silica gel.

While CaCl2 does suffer from complexation with ammonia, it can still be used at the expense of ammonia yield. The complex itself is highly hygroscopic.




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[*] posted on 5-8-2015 at 15:07


Hey NWS, I have a similar setup waiting for me to get time to test it, maybe we could compare our results later on.
My setup is:
Ammonia being generated by reaction of ammonium chloride with NaOH in a glass container;
Connected to this container is a dry air inlet and the mixed stream then goes into copper tubing bought from local AC supplier;
A MOT pumps a huge amount of current into a section of the cooper pipe heating it, this part is problematic as the transformer and its wiring needs to be actively cooled as the copper pipe isn't particularly resistive. I'll either change to a tungsten resistance or get myself a propane torch (less likely due to limited budget);
The product gas stream then goes into a packed bed wet scrubber containing H2O2 solution (I'm expecting that most of the NO will be oxidized to NO2 and should then react to form nitric acid). Further in line I'll put another scrubber with water to keep any unreacted ammonia from leaving, and last I'll improvise some flow rate meter or just measure the volume of gas that will have left when its done.

Now, assuming full oxidation of NO to NO2 and that all NO2 would be captured in the first scrubber I can check how acidic the peroxide solution became and then use MnO2 to catalyze the decomposition of leftover peroxide into water, then boil the water/acid mixture down and see how much ammonium nitrate I got.
From the second scrubber I can see how much Ammonia was dissolved and given the amount of ammonia on the second scrubber + ammonia reacted to ammonium nitrate I can calculate the unreacted ammonia.

From the volume of inert gas (or from the flow rate of inert) I can calculate the selectivity of the reaction that is taking place and try varying the parameters of the reactor until I find the best yield of nitrogen oxides versus N2.

Overall that's what I plan on doing, if anyone could point mistakes on the experiment or in my proposed result analysis I'd appreciate it.


[Edited on 5-8-2015 by battoussai114]
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[*] posted on 5-8-2015 at 16:35


@battoussai114
The critical part is going to be the oxidation of NH3 to NOx. Ie, it doesn't happen without very high temperature, very high pressure and a platinum group catalyst. Even then, conversion to NO2 is low. Real world systems divert the NO produced back through the stream for further oxidation. (Not an easy thing to do at high T & P for a home chemist.) Now that is based on what I have read (and remembered). Feel free to do some more reading yourself and don't let my comments deter you from experimenting.
Then you have the problem of dissolving a hot gas stream in a liquid. Not ideal.
The other thing to consider is that ammonia is going to be a lot more soluble in your water/H2O2 mixture than your nitrogen oxides. In other words, you really don't want to have any NH3 left. In solution (or before) it will react with your nitric acid produced. Ammonium nitrate might not be a bad result but it is not your primary target.
https://en.wikipedia.org/wiki/Ostwald_process
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[*] posted on 5-8-2015 at 17:10


@J_Sum1,
Thanks, I've read a bit on the industrial ammonia to NOx conversion process, but since platinum group metals aren't very interesting in our situation I'm skipping these and going for things that are available to us. For instance someone here on the board tested cooper with results, although with low yields, and there are quite a few novel catalysts that could be tested, anything from cooper over various supports to maybe manganese nanoparticles... after all, catalysis is such diverse field.
I think the biggest point in the industrial use of platinum is how good it performs and, since there is going to be a huge investment in their production plant anyway, it's just easier to pay a lot for some rare metal that will definitely give good results albeit making the factory take longer to pay for itself instead of spending on R&D for something different.

For instance, I remember talking to a researcher of the university I study and he was commenting on how they presented to a local company a concept that would allow for higher efficiency for their soy dryers just to get turned down with the answer that in the case they needed higher soy drying rates they'd just buy another equipment.

Anyway, What I intend to do is first get the equipment to analyze the product stream of gas right, and then start working on different reactor parameters and various catalysts... And you have no idea how much I wish I could get a permit to use the gas chromatograph at the university....
Now, considering that ammonia is indeed more likely to dissolve in the peroxide solution, I'd better first scrub the gas with water and then put a H2O2 scrubber next.
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[*] posted on 5-8-2015 at 17:28


So if I drive to Lowe's and buy non-concentrated Nitric acid and distill it does that count



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[*] posted on 7-8-2015 at 19:10


battoussai114 I had the same idea with the MOT, but I'm leaning towards a propane torch right now as I'd rather not add lethal amounts of electricity to the things that could possibly go wrong, btw a propane torch can be obtained at fleet farm for $10 + a $3 propane tank, and that's for a pretty nice simple one. The formula I've been using is:
16 NH3 + 21 O2 → 6HNO3 + NO + NO2 + 21 H2O
This means that an air stream with 56.7% Oxy and 42.3% NH3 will give around 70% nitric acid along with NOx. Now I know I'm not going to get that accurate with the gas streams, however I'd like to have excess oxy to oxidize the NO. And rather than bubble it through anything I was going to dissolve it in the water produced from the oxidation of ammonia by containing and cooling the output gasses.
Camrock, first, read the rules. second what Lowe's has nitric acid and where? I want in on this.

Edit: My source of ammonia is probably going to be heated cleaning ammonia ~15%, possibly with some NaOH added, depending on preliminary testing. My source for anhydrous ammonia switched to urea this year. :(
Edit2: I also stopped worrying about drying the ammonia after realizing the oxidation will produce water anyhow.
P.S. battoussai114 I doubt the Mot will be needed for very long as the oxidation is highly exothermic, the change in gibbs free energy for the reaction listed above is around 4800KJ, which if we calculate the change in temperature of the products we get
18.02 g/mole*21 mole * 4.181 J/g*K =1582(H2O)
30.01 g/mole*1 mole*0.995 KJ/Kg*K= 29.9(NO)
1 mole * 37.5 J/Mole*K=37.5
63.01 g/mole * 6 mole * 1.72 KJ/Kg *K= 650
1582+29.9+37.5+650=2.299 KJ/K
4800/2.299=2087 Kelvin
2087+21C (room temp) = 2098 degrees C (temp of products assuming full reaction)
now this temp feels wrong, and it's a bit late for math, so if someone can find any flaws in my math, please point it out. However if it is correct, then not only is continuous heating unnecessary, active cooling would be needed.

[Edited on 8-8-2015 by NWS]

[Edited on 8-8-2015 by NWS]
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[*] posted on 10-8-2015 at 23:49


how did you get to this?

18.02 g/mole*21 mole * 4.181 J/g*K =1582(H2O)
30.01 g/mole*1 mole*0.995 KJ/Kg*K= 29.9(NO)
1 mole * 37.5 J/Mole*K=37.5
63.01 g/mole * 6 mole * 1.72 KJ/Kg *K= 650
1582+29.9+37.5+650=2.299 KJ/K
4800/2.299=2087 Kelvin
2087+21C (room temp) = 2098 degrees C (temp of products assuming full reaction)




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[*] posted on 11-8-2015 at 03:06


Hello again :)

Found this (making Nitrates from dirt):

https://www.youtube.com/watch?v=VaGykqoNhJk

Not sure why the guy tastes it but hey! Personally I wouldn't stick anything I've made in the backyard lab in my mouth and anything made of poo would be no exception! Whatever floats your boat though :P

Does anyone knows how to make another acid from OTC compounds? I believe all strong acids of any concentration were out of bounds for this challenge weren't they?

If you could make say H2SO4 or HCl from OTC materials, mix it with nitrates made from poop dirt would that be a winner?

Not sure if this is a good / stupid idea and have done next to no research on any of this proposed process but saw the video while looking at other stuff and thought I would put it out there as I remembered someone talking bout chicken poop early on in this thread :D

Hope this is of some use!

Dan
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[*] posted on 11-8-2015 at 22:21


how about ammonium nitrate from ice cold packs?
if h2so4 is allowed then it's a piece of cake to make HNO3
that guy codylab has made HNO3 in many ways check out his videos

[Edited on 12-8-2015 by gatosgr]




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[*] posted on 12-8-2015 at 01:46


Quote: Originally posted by gatosgr  
how about ammonium nitrate from ice cold packs?
if h2so4 is allowed then it's a piece of cake to make HNO3
that guy codylab has made HNO3 in many ways check out his videos

[Edited on 12-8-2015 by gatosgr]


Na mate.

Bought Nitrates are a no no. As is H2SO4.

The situation is pretty much what you could find in a supermarket in the year 2050 where anything of any scientific value is regulated so far up the bum that you might have to sign your life away to buy 5g of NaCl.

Or what you can find on a desert island now :P
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[*] posted on 12-8-2015 at 04:21


Quote: Originally posted by gatosgr  
if h2so4 is allowed then it's a piece of cake to make HNO3

Exactly. That's why it's not allowed.

If it was easy, it wouldn't be a Challenge would it ?




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[*] posted on 12-8-2015 at 06:54


One easy way that requires no chemicals at all is with high voltage from the sky, it's 100V/m the higher you go when it's about to rain. It would take a lot of time to make amounts of HNO3 but still...



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[*] posted on 12-8-2015 at 13:51


I'll try and figure something out...
That money is as good as mine! muahahaha

[Edited on 13-8-2015 by Big Boss]




Kept you waiting, huh?

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[*] posted on 12-8-2015 at 14:19


It's still mine ! All mine ! muahahaha

Can anyone remember how much it is ?

I think i increased it at some point.

[Edited on 12-8-2015 by aga]




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[*] posted on 12-8-2015 at 18:07


Fun fact, a single MOT is not enought to strike a decent plasma arc... but it certainly is enough to get a tungsten electrode really really hot, like incandescent hot, and then the insulation on the secondary melt... One of these days I'll drop by the scrap yard and get more wire and another transformer to put in parallel with the first one.
And yes, all these days and this is the only thing worth or report I done in this matter.

Quote: Originally posted by aga  
It's still mine ! All mine ! muahahaha

Can anyone remember how much it is ?

I think i increased it at some point.

[Edited on 12-8-2015 by aga]

No idea... I didn't even read all these pages.
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[*] posted on 12-8-2015 at 20:57


Quote: Originally posted by aga  
It's still mine ! All mine ! muahahaha

Can anyone remember how much it is ?

I think i increased it at some point.

[Edited on 12-8-2015 by aga]


I think it was now 350euros wasn't it?

Started at 250 but pretty sure it increased to 350!

With the Australian dollar the way it is that is around $1,000,000 :D Hahaha Na :P Is a LOT of moneys though :)

Quote: Originally posted by aga  
Amazing finds WGTR and j_sum1

A Nitric Acid Competition, and a Bug Exterminator discovered !

The sheer innovation and imagination you guys are demonstrating is what this is all about.

For those that don't know, bugs tend Not to eat things that kill them, much like us, and most living things.

Finding something they Will eat, yet kills them, is the entire Bug Poison Industry's secret.

Prize fund increases to 350 euros.

Edit:

Anyone Stressing Plants by shouting 'Harvester' or 'Sheep' at them in order to increase their nitrate levels will be disqualified.

[Edited on 23-2-2015 by aga]


Here you go :)

[Edited on 13-8-2015 by Dangle89]
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