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Author: Subject: Druken Aga Challenge (DAC) #3 - Closed (but open to discussion)
j_sum1
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[*] posted on 3-2-2015 at 01:58


DeltaH, what a great find. That is just fascinating. I have downloaded a pdf version that I can peruse at my leisure.
I noticed that he mentioned addition of CuO improved things even further. I guess if you have access to CuSO4 and NaCO3 then CuO is an easy synthesis from otc products -- that it if it is not otc itself.

I need to read carefully and thoroughly. After a quick skim my first thought was to tumble the beans/peanuts in MnO before starting. That stuff sticks to everything. (Although, in the case of battery gunk it is more the graphite powder that sticks.) I never thought of soaking in KMnO4, but that sounds promising too.

I have done a (mental) redesign of my spray system. I am still mulling over options for my redesigned furnace. Catalysts sound like a great idea and there are a couple of options that can be tried. Sopermarket over the road doesn't stock soy beans but I am sure that I can find some. Failing that, I can re-do the peanuts. Suddenly there are a whole lot of variables to play with.

Suddenly this whole thing jumped up a notch.
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deltaH
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[*] posted on 3-2-2015 at 02:26


Yeah I got lucky, but it was blogfast's suggestion of MnO2 that got me digging.

Tumbling sounds great, bashing with a propeller internally... even better.

My ten cents worth: I also suggest pre-cooling the flue gas through a water cooled condenser (if you have one) or simply a coiled pipe before feeding to the cold water absorber. I also think this final absorber could simply be a vertical plastic pipe packed with crushed ice! The ice would melt gradually (hence some precooling can economise on the speed of the melting) and would also have a nice big surface area. I'd make it a column if possible and feed the flue gas from the bottom and tap off the acid from the bottom. The top of the column can be left open and fresh ice added constantly as the level dips. This counter-current approach would maximise the concentration of the acid pulled from the bottom.




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j_sum1
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[*] posted on 3-2-2015 at 04:57


I think I mentioned before that I have no experience of choosing a catalyst but obviously transition metals are the go and I follow blogfast's reasoning on oxides. MnO2 was always going to be an obvious start point since it is so readily available.

I am not going to bash the beans. I want the air to be able to circulate around them easily during combustion. And I am trying to avoid having to construct a whole lot of pumping and mechanical equipment.
I agree wholeheartedly on cooling the flue has and ideally the water spray too. I am not so sold on the crushed ice. I think it will inhibit gas flow too much. And it won't provide the surface area of a fine spray. However, I can't see a simple way of active cooling with my modified design. What I think I will do instead is go for a high volume of spray for both cooling and absorption and plan on some serious reduction once the dilute acid is collected. It is summer here. My tank of rainwater is sitting at around 24°C and so is not that cold. But I expect some evaporative cooling to occur as well so that is something.

The whole set-up will be ridiculously simple. But I am waiting on a couple of purchases to arrive before I make another attempt.
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[*] posted on 3-2-2015 at 05:03


Best of luck j_sum1, I'm really looking forward to your results!



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[*] posted on 3-2-2015 at 10:01


j_sum1:

Don't use battery gunge though. It contains lots of graphite, a reducer. At a very minimum use pottery grade MnO2 or decent homemade.




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[*] posted on 3-2-2015 at 11:18


Would a bottle of Soy Sauce be of any use ?

http://www.ajol.info/index.php/ajb/article/download/92538/81...

Page 4 says ~16.5g/kg Nitrogen.




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[*] posted on 3-2-2015 at 11:36


Save it for your sushi :) One can also use dry lentils, which I assume is readily available in grocery stores nearly everywhere, if soybeans aren't. Lentils are pretty high in protein, though not as high as soybean. Pound for pound, soybean is the cheapest plant protein source AFAIK. A 100% protein is also not a good idea because it might be harder to combust, so I wouldn't use protein powders like those that bodybuilders do, e.g. whey powder. I think legume beans are optimal for this type of experiment, be it soy or lentil based. I know j_sum is a fan of peanuts, but they're pricey here. I always keep thinking forward in-case one of these crazy things works and one would want to scale-up.

[Edited on 3-2-2015 by deltaH]




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[*] posted on 3-2-2015 at 19:02


Is the challenge still on? If so it wouldn't be a bad idea to just make KNO3 via the french method, and H2SO4 by sulfur (tomato dust) burning [ S8 + 8O2 -> 8SO2, SO2 + H2O -> H2SO3, 2H2SO3 + O2 -> H2SO4]...
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[*] posted on 3-2-2015 at 19:03


Last time I did that I failed, but that wasn't for lack of effort. Has anyone else succeeded through that method?
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[*] posted on 3-2-2015 at 21:15


Quote: Originally posted by Hawkguy  
Is the challenge still on? If so it wouldn't be a bad idea to just make KNO3 via the french method, and H2SO4 by sulfur (tomato dust) burning [ S8 + 8O2 -> 8SO2, SO2 + H2O -> H2SO3, 2H2SO3 + O2 -> H2SO4]...

I don't believe that pathway works.
The commercial process is to oxidise SO2 to SO3 in the presence of a vanadium pentoxide catalyst. Then that is converted to H2SO4 with water.

V2O5 means that it is no longer an otc process.
SO3 more than likely means that it is not a back yard process.

Others more knowledgeable than I am may provide a work around -- perhaps using H2O2. But if there is one, I am not aware of it.
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[*] posted on 3-2-2015 at 21:37


Quote: Originally posted by blogfast25  
j_sum1:

Don't use battery gunge though. It contains lots of graphite, a reducer. At a very minimum use pottery grade MnO2 or decent homemade.

You're right. I hadn't been thinking of the graphite as a reducer. I do have pottery grade MnO2 so can use that. The thing is, I have also been disassembling cells and attempting to purify the gunk -- with limited success. (Getting the Fe out is a bit of a dog.) Since I have large volumes of the stuff I thought I might use it but I can see that the graphite will get in the way.
Pre-burning of the graphite is not likely to work either. Not unless I can get some kind of furnace with a stirred bed and filtered gas extraction to contain the fines. I am not going there. Pottery grade it is.
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[*] posted on 3-2-2015 at 22:21


I believe it was stated in that thesis that regular MnO2 doesn't work... you need to prepare it in an active form. His methods involve KMnO4. This is sold in pharmacies in South Africa... though I haven't actually checked in the last 5 years if it's still so.

[Edited on 4-2-2015 by deltaH]




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[*] posted on 5-2-2015 at 12:10


Quote: Originally posted by Hawkguy  
Is the challenge still on? If so it wouldn't be a bad idea to just make KNO3 via the french method, and H2SO4 by sulfur (tomato dust) burning [ S8 + 8O2 -> 8SO2, SO2 + H2O -> H2SO3, 2H2SO3 + O2 -> H2SO4]...

Yeah. It's still On - nobody Won it yet !




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[*] posted on 5-2-2015 at 12:24


How about preparing Nitric acid from these compounds? Can you buy these from garden or agricultural supply store or from supermarket?

(i) Calcium nitrate (Norwegian saltpeter)
(iii) Hydrochloric acid (Muriatic acid)
(iii) Potassium or Sodium metabisulfite (Campden tablets)
(iv) Apparatus to dissolve gases (delivery tube)
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[*] posted on 5-2-2015 at 12:26


Not the first one.
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[*] posted on 5-2-2015 at 12:34


oh darn, you can make both dilute sulfuric acid and dilute nitric acid by this method. Not sure about the concentration though, did not try to concentrate it when I made it last time.
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[*] posted on 10-2-2015 at 21:29


Firstly do not try to make this
Secondly do not try to make this

Any welder suppler will sell Acetylene for braising or cutting steel
Any art supplier will sell Silver nitrate for prints

As the "precipitate" falls out of solution nitric acid will be left behind.
Again do not try to make nitric acid by this method as it is highly dangerous.

Side note: When cleaning welds on stainless steel we use a compound called pickling paste/liquid it is a mixture of HF and HNO3. It doesn't follow the rules of the challenge but try to separate it if you need nitric.


@Hawkguy don't try to burn tomato dust, we make that mixture at my workplace and one of the anti-biologicals ($30K a liter) in it is very dangerous although i doubt you would get near enough of the stuff to cause injury.

[Edited on 11-2-2015 by Pasrules]




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[*] posted on 11-2-2015 at 10:08


Quote: Originally posted by Pasrules  


As the "precipitate" falls out of solution nitric acid will be left behind.
Again do not try to make nitric acid by this method as it is highly dangerous.


Dangerous? Dangerous to your bank account, that's certainly true!

Quote: Originally posted by Pasrules  
Side note: When cleaning welds on stainless steel we use a compound called pickling paste/liquid it is a mixture of HF and HNO3.


You talk about danger but have no problem removing HF from such a solution?


Quote: Originally posted by Pasrules  
@Hawkguy don't try to burn tomato dust, we make that mixture at my workplace and one of the anti-biologicals ($30K a liter) in it is very dangerous although i doubt you would get near enough of the stuff to cause injury.


A slightly contradictory statement, I feel. What is this mystery 'anti-biological' anyway?





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[*] posted on 11-2-2015 at 12:45


To retort
I choose the most expensive route to discourage people from trying it.

I am not experienced in dealing with gaseous HF nor do I expect anybody to attempt to separate pickling paste. It is just another source that somebody may not of thought of even tho it is against the rules of the challenge.

The anti-biological is actually an insecticide but the name escaped me at the time.
We use spinosad in Yates tomato dust which by MSDS is harmless but in the quantities I work with a single drop on the skin can take years for the affected area to recover. However for the concentration in the packet the evolving sulfur dioxide is more dangerous.
MSDS: http://msds.orica.com/pdf/shess-en-cds-D010-000000021922.pdf




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[*] posted on 11-2-2015 at 13:13


Quote: Originally posted by Pasrules  
To retort
I choose the most expensive route to discourage people from trying it.

I am not experienced in dealing with gaseous HF nor do I expect anybody to attempt to separate pickling paste. It is just another source that somebody may not of thought of even tho it is against the rules of the challenge.

The anti-biological is actually an insecticide but the name escaped me at the time.
We use spinosad in Yates tomato dust which by MSDS is harmless but in the quantities I work with a single drop on the skin can take years for the affected area to recover. However for the concentration in the packet the evolving sulfur dioxide is more dangerous.
MSDS: http://msds.orica.com/pdf/shess-en-cds-D010-000000021922.pdf


I have seen tomato dust that is just sulfur. It doesn't necessarily have any of the other compounds mentioned in the MSDS.
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[*] posted on 11-2-2015 at 14:17


And my tomato dust is copper oxychloride. No wonder I was confused.
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[*] posted on 14-2-2015 at 12:38


Hey, I just recently found out where to acquire 55 gallons/210 litres polyethylene drums and I thought they would make a great scrubber/dissolution vessel to produce nitric acid. All you would need to do would be to fill the drum with water (say 10 litres, that's about 3 cm of liquid at the bottom of the drum) and put a ultrasonic fogger inside the drum.

Then, any nitrogen dioxide pumped into the drum via a tube would react with the fog an make nitric acid.
Because the vessel is so large, the nitrogen dioxide spends a lot of time in it and is converted more efficiently to nitric acid. The ultrasonic fogger could be coated in a nitric acid resistant substance, or one could settle with low concentrations.

An drum with a detachable lid is probably more suited for this use, to easily recover the nitric acid at the bottom of the drum.

One disadvantage of this scrubber is that you end up with 200 litres of nitrogen dioxide (even though dilute) which needs to be completely dissolved before retrieving the nitric acid. For this reason the drum should only be opened outside (Or in your fume hood if it's large enough...).

Anyway, just an idea.




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[*] posted on 14-2-2015 at 14:46


Ultrasonic Fogger !

Sounds great.

Where on Ebay do i get one ?




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[*] posted on 14-2-2015 at 22:35


Already thunka that one. And I used to have a fogger too... until it broke. What I don't have is a large plastic drum. My next attempt is probably two weeks away and I promise lots of mist.
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[*] posted on 15-2-2015 at 04:32


Quote: Originally posted by Romain  

Then, any nitrogen dioxide pumped into the drum via a tube would react with the fog an make nitric acid.

and from where will the NO2 come?
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