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Author: Subject: H2SO4
Quince
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[*] posted on 19-8-2005 at 23:53


Has anyone here actually tried distillation of H2SO4 from drain cleaner? Would that remove the buffers? Would regular glassware suffice?



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[*] posted on 20-8-2005 at 02:08


From what I have read, many have tried, and while its possible to get some of the color or impurities out, most people still have the same color they did before.

Some succeed somewhat... I belive it was somewhere here last night I read about someone distilling sulfuric acid drain cleaner, and while their product was indeed clear, they lost a lot of it in some reaction that accidently took place...

Regardless, I have never heard of the color affecting any reaction that uses the acid. Sure it may look odd and may scare you, but I have never heard of anything go wrong because of it... But then again who knows...

As for normal glassware to handle it, you'll be fine. No matter the concentration, H2SO4 simply can not eat away at glass... flourine on the other hand....




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[*] posted on 20-8-2005 at 07:11


It was the battery acid thread of all places that I posted on my distillation of drain cleaner. I used regular glassware but I did the distillation under reduced pressure. I got very clean sulfuric acid from the process.

Of note is that I didn't use magnetic stirring and used boiling stones which is a no-no in a reduced pressure distillation as a result I would get occasional flash boiling. Also when initially distilling water would condense in the still head and drip back into the very hot sulfuric acid and would cause a poping in the flask shooting vapors and acid upwards, ruining my first attempt although I was more careful with my second attempt. If you did this with an apparatus under atmospheric pressure it may have come off better though I would have had to have used a better heat source.

Maybe wrap the still head in Ni-Chrome to keep it over 100C so water would not condense. Also note that at such high temperatures I probably shouldn't have used ice water in my condenser and I am somewhat lucky it didn't break, maybe use air instead.

h2so4smoke.jpg - 48kB




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Quince
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[*] posted on 20-8-2005 at 21:08


Well, I could do reduced pressure, but the issue is how long it takes to reach temperature.

I don't have a problem with the color of the drain cleaner, it's very slightly yellowish. I have a problem with the bits of cloudiness in it, which is either particulate matter (but probably easier to distill than find appropriate filter), or the buffers.

I assume with proper insulation around the still head, with the source flask in a heating mantle, it shouldn't be too bad. I'll probably give it a try next weekend, and I'll post the results.

Any use to add a vigreux column, to help with the water issue?

[Edited on 21-8-2005 by Quince]




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[*] posted on 20-8-2005 at 21:30


From what I can recall, drain cleaner is about as close to pure H2SO4 as your likely to get, that is, the water has already formed its azeotrope with water... In which case you wouldnt be seperating any water from the acid. All your doing here is just seperating your acid/water from impurities.

What a long way to say a fractional distillation wouldnt make any diffrence.

However, if it would be battery acid, or anything under 98% (I belive) then it may be *somewhat* benifical... Then again water boils sooner than the acid anyway so...

Make of it what you will, but if your just going to get impurities out, then a quick and simple distillation should get the job done.




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Quince
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[*] posted on 20-8-2005 at 21:32


Will mineral wool (the kind used to insulate the walls of houses) be OK as a filter? I'm thinking filtration is much easier than distillation at 320*C.



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[*] posted on 20-8-2005 at 21:39


I don’t see how it would help. The acid has to be the same temperature to make it to the condenser regardless of what columns it has to pass through.

edit: Two responses while I was typing, that’s unusual.

The wool should do, just make sure there is no plastic in it.

[Edited on 21-8-2005 by neutrino]
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[*] posted on 21-8-2005 at 20:49
Rooto


I've never encountered problems using the Rooto sulphuric acid despite its yellow tint.
The stuff is great for producing nitric acid.




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[*] posted on 1-9-2005 at 09:28
wow...hot stuff!


I just found a place that sells Pro-Drain Opener. Its amazingly energetic stuff... it is thick and slightly amber colored and it fumes slightly. The pro's say it is 93.5% H2So4... it does Nitration REALLY well. So no sense on trying to concentrate it. I just made some triNitromethane... using the odd ball patent using Nitric Acid on Isopropyl Alcohol. Wow, can I say wow.
I post pics soon,

[Edited on 2-9-2005 by ((Blasta))]




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[*] posted on 1-9-2005 at 10:37


Nitromethane from isopropyl alcohol? That sounds interesting. Can you explain this? What is the mechanism behind this?



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[*] posted on 1-9-2005 at 10:41


Really interesting. Patent number is?
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[*] posted on 1-9-2005 at 23:08


United States Patent: 4,122,124

read up and try it* :) with rising fuel costs this might just be a money maker. ....being sarcastic
--------------------------
Instead of using liquid Nitric Acid...I used the chemical reaction between Sulfuric Acid and Potassium Nitrate inside a glass flask. Then I pumped the vapour into another flask containing warmed Isopropyl Alcohol. The product that condensed was yellowish and sweet smelling... yep, its pure Nitroform or tri-Nitromethane. I estimate 60% yield... which isn't bad since it was my first attempt.


[Edited on 2-9-2005 by ((Blasta))]

[Edited on 2-9-2005 by ((Blasta))]




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[*] posted on 1-9-2005 at 23:16


Thats TRInitromethane, not just regular nitromethane which contains only one nitro group. Please note while messing with trinitromethane that it is quite carcinogenic.



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[*] posted on 1-9-2005 at 23:22


oh, really? Yikes. I bet triNitroMethane could be useful in making PLX or a variation of it, right?



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[*] posted on 1-9-2005 at 23:23


What the hell? This patent is for making trinitromethane, not nitromethane. Can't you tell the difference between CH(NO2)3 and CHNO2? Rising fuel costs? Talk about false advertising! Sheesh, just when I thought we had something interesting here.

Heh, I'm glad it's carcinogenic, maybe the fool will get cancer and stop spreading misinformation on this forum.

[Edited on 2-9-2005 by Quince]




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[*] posted on 1-9-2005 at 23:29


I thought I had something interesting as well... well then again maybe I don't.
What use is triNitromethane then? I thought it could be used as a fuel of sorts with other chemicals? hummm... sorry guys
oh yea, in my origional post I did specifically state that this synthasis did create pure Nitroform/ tri-Nitromethane. Anyway what do I do with 120 mL of triNitromethane...
??

[Edited on 2-9-2005 by ((Blasta))]

[Edited on 2-9-2005 by ((Blasta))]




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[*] posted on 2-9-2005 at 00:45


Further nitration to tetranitromethane for use in binary exlosives (but that's even more toxic, lethal in air is about 0.1 ppm). Check out roguesci.

[Edited on 2-9-2005 by Quince]




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[*] posted on 2-9-2005 at 01:18


That's a pity... I was really hoping to get some (mono)nitromethane in pure form :(. The trinitro stuff is not interesting to me. Up to now I only succeeded in finding mixes with methanol or petroleum for model cars and karts, but I need the pure stuff. The mixes I found only contain up to 10% or something like that :(.



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[*] posted on 2-9-2005 at 01:22


Yeah, but it would have more wear on the engine. Most aren't made for more than 10%, and a lot of plane glow engines are intended for 5% NM. Not to mention that the 2-cycle glow engine sprays non-fully burned fuel all over the place, as I found out the hard way...



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[*] posted on 3-9-2005 at 04:35


Thunder-
you prolly smelled SO2 or SO3, and possibly saw water vapor leaving the solution.
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[*] posted on 3-9-2005 at 05:14


SO2 does not smell like "burning death", it smells like burned strike-anywhere matches or firework smoke or a package of dried fruit that was just unsealed. The "burning death" description sounds more like the H2S, which as a far nastier stench than SO2, though I don't see how that could have come from the reaction. Now SO3, I don't know what that smells like, how it compares to SO2, so those that are in the know please describe it to us. Or maybe there was sulfur pollution in his water, as occasionally happens with tap water that's sourced from wells, and that also has H2S smell.

[Edited on 3-9-2005 by Quince]




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[*] posted on 3-9-2005 at 06:03


I'm guessing that the smell was an H<sub>2</sub>SO<sub>4</sub> mist.
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[*] posted on 3-9-2005 at 08:03


SO3 is rather hygroscopic, so it forms H2SO4 (of some percentage H2O, because it is also hygroscopic!) which just burns when inhaled. I haven't noticed any smell from it where hot pyrolysis isn't involved (e.g. burning refractory sulfates like CaSO4 makes a lot of SO2).

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[*] posted on 3-9-2005 at 08:10


Would it be possible to use a centrifuge to separate the dye from the acid? (referring the cheap black drain cleaner)
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[*] posted on 3-9-2005 at 09:00


If the dye is only as a very fine suspension then yes. Remember to use strong tubes, preferably made from thick PP. No glass.
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