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davidfetter
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Quote: Originally posted by chempyre235  | @PoWer:
Yes. NOx contamination is an issue with discharge ozonators, and the devices typically don't have a way to connect to a tank or a
concentrator. For this reason, I've been looking at trying the UV-C method. However, gutting and rehousing a cheap ozonator could work, too.
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The guts of such are available pretty cheaply.
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MrDoctor
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| Quote: Originally posted by bnull | | Quote: Originally posted by PoWEr | | Speaking of formic acid, If oxalic works on copper sulfate to yield sulfuric acid, why not use formic acid? The pka and structure is almost the same.
Also instead of copper sulfate which can cost a lot, why not use some cheap sodium sulfate? |
One word: solubility. Having similar structure and pKa is not important. Copper(ii) oxalate is insoluble in water, while the formate is soluble (125
g/L at 25 °C, according to Lange's Handbook 16th). Sodium oxalate and formate are soluble. If you can find a substance whose sulfate is soluble but
the formate isn't, that would be the one.
As pointed out, you can use iron sulfate with oxalic acid, if copper sulfate is too expensive.
One thing I forgot to mention: let the copper oxalate sludge rest for a day or two. You get a nice clear liquid and a compact mud.
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Does it benefit from a few heat/recrystalization cycles like manganese oxalate does? In nurdrages method, i may be mis-remembering, but at one stage
an extremely difficult to filter solid is obtained, it instantly clogs any filter, but boiling it then cooling causes small particles to dissolve and
prefferentially crystalize on the remaining ones (still goes from sludge to sludge) but it has an effect on consistency akin to melting and refreezing
ice cream, where the crystal structure becomes coarse and consequently the mass becomes porous. every so-often ill try this on difficult to filter
precipitates and it will work.
initially with going from battery manganese to clean manganese sulfate, during one particular stage, i would be limited to maybe 5-6mm of solid on the
filter, and i was mostly just dealing with decanted solution cleanup rather than running all the solids through. afterwards it took maybe 10 minutes
to vacuum filter the entire kilo or so.
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PoWEr
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Found it - assuming It's 10 grams per hour, this is quite easy to install it as it seems like there is an input and output.
The only problem with ozone generators I see is how small amounts of ozone they generate, I mean 10 grams is still better than almost every other
option (I found ones that generate 20 grams, but they are for home use) so in 4-5 hours, you would have one mol of ozone.
This is a problem because it means you have to wait days for the whole sulfur to be actually converted to SO3 and at this point, I belive It would be
easier to just burn it to SO2, then mix it in diluted H2SO4 and then blast ozone at it.
3H2SO3 + O3 --> 3H2SO4
As for the UV-C light, I found different "sources" (couldn't find even a paper, the next sentence is based on random people saying stuff on general
forums) stating about ozone production. Some say <240nm generates the most, then there's a source that says It's in the range of 100 to 200nm, then
160nm to 200nm. I also found no information whatsoever about a rough estimate on how much it actually produces.
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bnull
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| Quote: Originally posted by MrDoctor | | Does it benefit from a few heat/recrystalization cycles like manganese oxalate does? In nurdrages method, i may be mis-remembering, but at one stage
an extremely difficult to filter solid is obtained, it instantly clogs any filter, but boiling it then cooling causes small particles to dissolve and
prefferentially crystalize on the remaining ones (still goes from sludge to sludge) but it has an effect on consistency akin to melting and refreezing
ice cream, where the crystal structure becomes coarse and consequently the mass becomes porous. every so-often ill try this on difficult to filter
precipitates and it will work. |
As far as I could see, the size doesn't increase much. You can improve the process if you transfer the sludge to a tall flask. Suspend it at an angle
(from 5° up to 20° with the vertical) and the oxalate will settle down more quickly. Then it only remains to decant the liquid before it gets
discolored. Copper oxalate is soluble in acids. If you used excess oxalate, the discoloration happens in a relatively short time; if you used a small
excess of copper sulfate, you have at least a couple of days.
This is the result of my mixing hot saturated solutions of oxalic acid and copper sulfate and forgetting the tube for a few days. Notice the color of
the supernatant.
Aluminum sulfate seems to work better. The quantities that I tested were less than 1 gram and I didn't get around to purify more aluminum sulfate for
a larger scale, though. Aluminum sulfate is cheaper than copper sulfate and quite easy to purify.
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PoWEr
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Copper sulfate is not the biggest problem, oxalic acid is. In my country I looked at offers and I found only 5% conc. Getting that to a bigger
concentration and more of it will be expensive, therefore Im looking for alternatives.
Did some research and according to this paper, in 1C the solubility of nickel formate is 3g in 100g of water (if I did the pounds & farenheit conversion correctly). Lower that
temperature and you could probably get it to practically insoluble.
Lionel Spanner mentioned that you can make oxalic acid from oxalate salt, sure, but in my country It's still very expensive (It would be probably
better to just distill that 5%).
Just a quick observation, I have no idea where I've seen it, but I remember this reaction:
BaSO4 + 2H2O --> H2SO4 + Ba(OH)2
Anyone seen it too? I swear it was on the sulfuric acid wikipedia page, but now it is gone. If I remember correctly this was a historical method, Im
skeptical if this reaction could actually yield good quality sulfuric acid though.
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bnull
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You said,
That's whay I suggested iron sulfate.
You can't use metathesis with alkaline sulfates because alkaline salts of the most common acids are soluble. So, sodium sulfate and an acid won't
work. If you can find an acid whose ammonium salt volatilizes on heating, then that's the one. Mix it with ammonium sulfate, heat it and bingo. The
ones I know decompose at the same temperature, so I have no clue.
What about phosphoric acid and aluminum sulfate? Aluminum phosphate is slightly soluble in acids. Other phosphates are more soluble.
| Quote: Originally posted by PoWEr | Just a quick observation, I have no idea where I've seen it, but I remember this reaction:
BaSO4 + 2H2O --> H2SO4 + Ba(OH)2
Anyone seen it too? I swear it was on the sulfuric acid wikipedia page, but now it is gone. If I remember correctly this was a historical method, Im
skeptical if this reaction could actually yield good quality sulfuric acid though. |
Never saw that in Wikipedia. Vandalism perhaps? In my experience, Wikipedia is full of errors, some so obvious that you can't believe they are still
there, and some so small that you won't see unless you are looking for them. Always check the references given in Wikipedia. There's also the revision
history of the article; verify the past revisions if you want.
What I say is, the way it is written, just the formula with no additional information, it won't work in a million years. Barium sulfate is the most
insoluble of sulfates, sulfuric acid and barium hydroxide are soluble in water, water boils way before sulfuric acid. Mixing water, hot or not, with
barium sulfate will only make a sludge (they use it in x-ray contrasts). If sulfuric acid was produced in that way, it would instantly react with
barium hydroxide to regenerate barium sulfate and water. Could it be superheated steam instead of water, at a temperature above the boiling point of
sulfuric acid? I don't remember that as a historical method, although I do not remember everything I read.
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PoWEr
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| Quote: Originally posted by bnull |
What I say is, the way it is written, just the formula with no additional information, it won't work in a million years. Barium sulfate is the most
insoluble of sulfates, sulfuric acid and barium hydroxide are soluble in water, water boils way before sulfuric acid. Mixing water, hot or not, with
barium sulfate will only make a sludge (they use it in x-ray contrasts). If sulfuric acid was produced in that way, it would instantly react with
barium hydroxide to regenerate barium sulfate and water. Could it be superheated steam instead of water, at a temperature above the boiling point of
sulfuric acid? I don't remember that as a historical method, although I do not remember everything I read.
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Yeah, that's what I thought too. There was no additional information on that method, just the reaction written down under "historical methods"
section.
Well, I guess Im left with the ozone, which is probably the least hassle, frustration and most pure, phosphoric acid and aluminium sulfate (thought of
it before too, but then I got stuck at AlPO4 and how do I get it out) and experiment with formic acid and nickel sulfate(I can't really afford oxalic
acid or make it from oxalates).
Im quite interested in @chempyre235 project. What UVC bulb do you use and how do you plan on doing this in a suspension?
[Edited on 31-5-2025 by PoWEr]
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chempyre235
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I don't have the bulbs yet, but I've been keeping my eye out for some of the industrial ones. As for the suspension, I had planned to use a bubbler in
a glass reactor vessel with a magnetic stirrer to keep the sulfur, ozone, and water mixed. Unfortunately, it'll be a while before I have a place to
work on this project.
I did find these bulbs on Amazon, though.
https://www.amazon.com/UV-Sanitizer-Storehouse-Germicidal-St...
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PoWEr
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What about oxygen? You're going to use a tank? I have been looking for oxygen concentrators that can produce medical grade oxygen for a cheap price
but found no luck whatsoever. According to this post there are decommisioned medical units that can be bought for cheap but couldn't find anything. If they still exist (that post was made
in 2018), they would provide oxygen for practically unlimited time as long as nothing breaks.
When I get free time I will probably test both ozone generator and UVC bulb but I belive a generator is still more efficient.
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davidfetter
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| Quote: Originally posted by PoWEr |
What about oxygen? You're going to use a tank? I have been looking for oxygen concentrators that can produce medical grade oxygen for a cheap price
but found no luck whatsoever. According to this post there are decommisioned medical units that can be bought for cheap but couldn't find anything. If they still exist (that post was made
in 2018), they would provide oxygen for practically unlimited time as long as nothing breaks.
When I get free time I will probably test both ozone generator and UVC bulb but I belive a generator is still more efficient. |
Used oxygen concentrators can often be found on places like craigslist. They are, unfortunately, often being sold off after the person who was using
them has died. Bear this in mind when communicating with the people selling them.
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PoWEr
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| Quote: Originally posted by davidfetter |
Used oxygen concentrators can often be found on places like craigslist. They are, unfortunately, often being sold off after the person who was using
them has died. Bear this in mind when communicating with the people selling them. |
Well, after searching for a while, I found some that allegedly make up to 93% pure oxygen for 200 dollars with post-exhibition label. Probably going
to buy it later this day.
I've read that ozone generators apparently can overheat easily (it actually makes sense, no idea why I didn't think of this earlier). Perhaps UVC bulb
may be actually better, and they cost almost the same. Now I also wonder if mirrors could help with irradiating oxygen.
On a note I thought that decomissioned just meant that they malfunction or don't make the required purity for medical usage anymore. Sad to see this
happens :(
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davidfetter
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| Quote: Originally posted by PoWEr | | Quote: Originally posted by davidfetter |
Used oxygen concentrators can often be found on places like craigslist. They are, unfortunately, often being sold off after the person who was using
them has died. Bear this in mind when communicating with the people selling them. |
Well, after searching for a while, I found some that allegedly make up to 93% pure oxygen for 200 dollars with post-exhibition label. Probably going
to buy it later this day.
I've read that ozone generators apparently can overheat easily (it actually makes sense, no idea why I didn't think of this earlier). Perhaps UVC bulb
may be actually better, and they cost almost the same. Now I also wonder if mirrors could help with irradiating oxygen. |
Not all that easily, and the ones you get that are mostly fin are set up to handle this. You might grab a fan if you have a spare one. Another way to
deal with this is a lamp timer or similar to let it cool on a cycle. This will require some tuning, but it requires less by way of extra gear.
| Quote: Originally posted by PoWEr |
On a note I thought that decomissioned just meant that they malfunction or don't make the required purity for medical usage anymore. Sad to see this
happens  |
Yeah, so please be kind to the people selling them. You don't have to pry or even offer sympathy, but you can say something along the lines of "I'll
take good care of it."
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chempyre235
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| Quote: Originally posted by PoWEr |
What about oxygen? You're going to use a tank? I have been looking for oxygen concentrators that can produce medical grade oxygen for a cheap price
but found no luck whatsoever. According to this post there are decommisioned medical units that can be bought for cheap but couldn't find anything. If they still exist (that post was made
in 2018), they would provide oxygen for practically unlimited time as long as nothing breaks.
When I get free time I will probably test both ozone generator and UVC bulb but I belive a generator is still more efficient. |
| Quote: Originally posted by davidfetter | | Used oxygen concentrators can often be found on places like craigslist. They are, unfortunately, often being sold off after the person who was using
them has died. Bear this in mind when communicating with the people selling them. |
I got my concentrator from an online auction a few months ago, but I recently saw one at a garage sale (for less than I bought mine  ).
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davidfetter
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| Quote: Originally posted by chempyre235 | | Quote: Originally posted by PoWEr |
What about oxygen? You're going to use a tank? I have been looking for oxygen concentrators that can produce medical grade oxygen for a cheap price
but found no luck whatsoever. According to this post there are decommisioned medical units that can be bought for cheap but couldn't find anything. If they still exist (that post was made
in 2018), they would provide oxygen for practically unlimited time as long as nothing breaks.
When I get free time I will probably test both ozone generator and UVC bulb but I belive a generator is still more efficient. |
| Quote: Originally posted by davidfetter | | Used oxygen concentrators can often be found on places like craigslist. They are, unfortunately, often being sold off after the person who was using
them has died. Bear this in mind when communicating with the people selling them. |
I got my concentrator from an online auction a few months ago, but I recently saw one at a garage sale (for less than I bought mine ). |
On the bright side, you have some pretty good idea that the one you have actually works.
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BAV Chem
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Here's something that I think should be mentioned in this discussion:
This thread covers another method of cheaply producing sulfuric acid and i feel like it's being disregarded as being too simple to actually work
by most. Sodium bisulfate will dissociate in ethanolic solution to yield sulfuric acid and sodium sulfate which precipitates out. Boiling/distilling
off the ethanol and water will give relatively pure sulfuric acid.
It does look too good to be true but I have found it to work quite well and it seems to scale nicely too.
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PoWEr
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| Quote: Originally posted by BAV Chem | Here's something that I think should be mentioned in this discussion:
This thread covers another method of cheaply producing sulfuric acid and i feel like it's being disregarded as being too simple to actually work
by most. Sodium bisulfate will dissociate in ethanolic solution to yield sulfuric acid and sodium sulfate which precipitates out. Boiling/distilling
off the ethanol and water will give relatively pure sulfuric acid.
It does look too good to be true but I have found it to work quite well and it seems to scale nicely too. |
250g of NaHSO4 turns into 50ml of sulfuric acid with potentially 7,4 grams of NaHSO4 dissolved in it. I saw that post before making this one but that
method doesn't seem to be that pure and you need a lot of sodium bisulfate to actually obtain a good amount of it.
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MrDoctor
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over there the cost of that would be about $20 for around 600ml worth then. pricing would be vastly better if you sourced 10-20kg bulk bags instead of
3kg off the shelf ones
assuming not much ethanol is lost, esp to dehydration, or any non reversible polymerization therafter, then you really are just looking at under $40/L
for conc sulfuric acid, assuming that 50ml was meant to be concentrated volume, i didnt read much into it. I just wanted to point out that
economically this isnt bad at all, until recently that would have actually been like half the cost of what was available to me, not worth the effort
but, still more economical than actual otc sulfuric acid
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Nikotin
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Hey PoWEr, consider buying Normatek Hydraulik drain cleaner. It is a Polish brand and is crystal clear 96% Sulfuric acid. Just a small recommendation
from me.
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PoWEr
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| Quote: Originally posted by Nikotin | | Hey PoWEr, consider buying Normatek Hydraulik drain cleaner. It is a Polish brand and is crystal clear 96% Sulfuric acid. Just a small recommendation
from me. |
On a website I found in bold big letters that Its technical grade, good, then I look down to description and find this: "Substancje aktywne w nim
zawarte sprawiają, że jest on wysoce skutecznym środkiem do udrażniania rur.". Which basically translate into (for the english fellows)
"Substances included in this product make it very effective for unclogging pipes". What substances is the question. The reason why I didn't buy a
drain cleaner before is because there is always something else in it and Its usually not written down anywhere.
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Nikotin
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| Quote: Originally posted by PoWEr | | Quote: Originally posted by Nikotin | | Hey PoWEr, consider buying Normatek Hydraulik drain cleaner. It is a Polish brand and is crystal clear 96% Sulfuric acid. Just a small recommendation
from me. |
On a website I found in bold big letters that Its technical grade, good, then I look down to description and find this: "Substancje aktywne w nim
zawarte sprawiają, że jest on wysoce skutecznym środkiem do udrażniania rur.". Which basically translate into (for the english fellows)
"Substances included in this product make it very effective for unclogging pipes". What substances is the question. The reason why I didn't buy a
drain cleaner before is because there is always something else in it and Its usually not written down anywhere. |
Put more trust into the people here! :D
And btw it is crystal clear!
[Edited on 19-6-2025 by Nikotin]
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PoWEr
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I think I actually should :)
How this was even approved? Every video I've seen about using drain cleaners always contained a part where they get rid of pigments and other
impurities. There's no way they literally just sell pure sulfuric acid under the brand of a drain cleaner, but I mean, I guess Its time to buy finally
something, perhaps I will still try the other methods so this thread wasn't created for nothing.
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RU_KLO
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just in the spirit of this post, could this be a viable way? (could it work?)
from :
Nitrous acid reacts very rapidly and quantitatively with sulfamic acid:
HSO3NH2 + HNO2 −→ H2SO4 +H2O+N2
"Kirk-Othmer Encyclopedia of Chemical Technology.
Copyright c John Wiley & Sons, Inc. All rights reserved.
SULFAMIC ACID AND SULFAMATES"
from our wiki:
Dinitrogen trioxide (nitrous acid anhydride)
Can be prepared by mixing equal parts of nitric oxide and nitrogen dioxide
NO + NO2 ⇌ N2O3
Both gasses can be obtained by dissolving copper in conc. nitric acid.
There are other methods to obtain nitrous acid, also read somewhere (could not recall where) that getting the right 50/50% (NO/NO2) its very difficult
and has to do with temperature, nitric acid concetration, etc)
(our wiki:
8 HNO3 + 3 Cu → 3 Cu(NO3)2 + 4 H2O + 2 ·NO
If this reaction occurs in the presence of air, the resulting nitric acid will react with oxygen to give the brown nitrogen dioxide)
So "simply" dissolving copper in nitric acid and directing (bubbling) its fumes to the sulfamic acid solution, will it convert to sulfuric acid?
(maybe first purging the apparatus with N2 because of the oxidation of NO with oxigen)
If not purged with N2, adding a NO2 to NO convertion , from this patent (US8226916B2):
" A nitric oxide delivery system that converts nitrogen dioxide to nitric oxide employs a surface-active material, such as silica gel, coated with an
aqueous solution of antioxidant, such as ascorbic acid."
the whole train would be:
1) nitric oxide generatord (Cu + HNO3)
2) gas scrubber used as convertion, with sillica gel saturated with ascorbic acid (dry)
3) gas scubber with sulfamic acid
4) sucking pump to produce negative pressure.
It seems viable.....
Go SAFE, because stupidity and bad Luck exist.
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teodor
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RU_KLO,
any method of getting H2SO4 published here is worth studying. Not for its results but for getting practice with manipulations, approaches of analysing
results and accurate reports of experiments. This is what costs most. H2SO4 costs almost nothing comparing to getting laboratory experience. And if in
some parts of the universe this is not true, I don't think any new ideas would be able to help in this situation but work only - it is better to get
enough practice with some checked method, this way you will be able to get the desired result much faster.
What is your experience of working with nitrogen oxides? Could you plan and perform some experiments in the order of increasing complexity with them
before building so complex imaginary construction? There is no possibility to get any result without careful studying of every step. Honed skills in
every single steps will allow combine those steps to get any result you want, unability to make even a single step will no allow to go anywere with
the best method in a world.
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clearly_not_atara
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If you are not too concerned with economics, there is no need to worry about the NO/NO2 ratio. Nitric oxide alone disproportionates in alkali to
produce nitrite alongside nitrous oxide and nitrogen, the latter gases being mostly harmless. When I have considered this question previously I was
mostly interested in good ways to produce NO alone, but really any NO:NO2 ratio between 1:0 and 1:1 should work.
The kinetics of the reaction are... not always great. There is plenty of literature about it. See attached.
Attachment: barnes1931.pdf (1.1MB)
This file has been downloaded 99 times
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RU_KLO
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| Quote: Originally posted by teodor | RU_KLO,
What is your experience of working with nitrogen oxides? Could you plan and perform some experiments in the order of increasing complexity with them
before building so complex imaginary construction? |
Are you saying that if I dont have the experience, should not post ideas?
A lot of discoveries came from ingenuity.
It was an idea, a brainstorming. A paper says nitrous acid + sulfamic acid -> sulfuric acid.
Of course there are simplier and known ways to make nitrous acid (nitrite + acid for example - I personally did not do it, but there are a lot of this
in SM posts and youtube videos), but I took a step further (because I though that nitrite is hard to come by)
When I post I expect contructive responses, like "this cant be done because xxxx" or its dangerous because.... but saying that you need to have
experience "before building so complex imaginary construction?" I dont find it constructive.
Go SAFE, because stupidity and bad Luck exist.
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