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Author: Subject: Sulfuric acid manufacture
testimento
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[*] posted on 29-6-2013 at 02:50
Sulfuric acid manufacture


I live in a totalitarian state where practically all non-customer chemicals sales are highly restricted so we have to rely on otc stuff which is highly limited.

I need sulfuric acid for several processes so I came up with an idea of using any source of sulfur or sulfur dioxide and ozone to generate sulfur trioxide and lead it into solution of sulfuric acid to generate a bulk of it. Ozone can be made with corona discharge or electrolysis, since I got a good sized electrolysis bank I rely on it, but a good source for sulfur is still on look for.

I came aware that heating iron sulfate will release SO2 and SO3 when heated to near 500C. This item is available with ease for now so I'll give it a try. Also some mining resources of pyrite and mining sulfur might be available. I would be making a dilute, 20-30% solution of H2SO4 in bottom of a large vessel where I would lead gases of SO2 and SO3 and ozone from other side and expect the SO2 to form SO3 and then it liquifies at 46C to the walls of the container and flow to the water-sa solution to form more concentrated sulfuric acid until it is in oleumic form, when more water will be gradually and carefully added. There is 1.5m high reflux column on top of this tank where the oxygen and possible unreacted ozone will vent out and it should keep the SO3 from cooking out.

How about other sulfur compounds? What'd be the easiest and cheapest way to get sulfur out from sulfur compounds? H2S could be generated too since I have a stainless steel ware and only limited glass available so my stuff dont compete with extremely corrosive substances very well. Sodium bisulfate might be available but the generated SO3 per kg is way too costly by this method.
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plante1999
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[*] posted on 29-6-2013 at 03:06


Use nitrogen oxides and oxygen to turn sulphur dioxide to sulphuric acid. Use lead as a apparatus material and use pyrite as the sulphur source, burn pyrite in an air flow to get the sulphur dioxide.

Lead chamber process... http://archive.org/stream/chemicallecturee00benerich#page/16...

[Edited on 29-6-2013 by plante1999]




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AndersHoveland
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[*] posted on 29-6-2013 at 03:32


There are several ways.

SO2 can be fairly easily oxidized in water to dilute sulfuric acid. For example, by passing in chlorine gas.

Lead chamber process uses nitric oxides to act as a catalyst, allowing air to oxidize the SO2 to sulfuric acid up to 60% concentration
reaction can be a little complicated because solid crystals of nitrosyl sulfuric acid can crystalize out of the concentrated solution also


For making sulfur trioxide:

oxidation of SO2 using vanadium pentoxide catalyst at high temperature

thermal pyrolysis of sodium bisulfate, first driving out the water leaving sodium pyrosulfate, and then finally further decomposition at 500 C.
best to use an metal bottomed container for the distillation


Another strategy is to make the less concentrated sulfuric acid using one of the corresponding methods, and then add sulfur trioxide to increase the concentration up to the desired level. Example: use lead chamber process to get 50% acid, boil off water to increase concentration to 70%, then add sulfur trioxide to get 100% acid.

It is not practical to try to get the concentration much above 85% through boiling, more of the sulfuric acid starts boiling off, makes chocking fumes, and boils away most of the acid.

[Edited on 29-6-2013 by AndersHoveland]
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testimento
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[*] posted on 29-6-2013 at 13:23


You didnt take any argument on that can SO2 be oxidized without trouble with ozone?

I can get chlorine gas and ozone gas from the same generator setup and I am not going to waste extremely precious nitrates for sulfuric acid, I'd rather use it for _producing_ nitrates if any.
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plante1999
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[*] posted on 29-6-2013 at 13:26


The nitrates are recycled in the process... You should have read the pages of the book I gave you.



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[*] posted on 29-6-2013 at 15:47


Another route is to react SO2 with Cl2. This either requires exposure to sunlight in a sealed container, or an activated carbon catalyst. The SO2Cl2 that forms can then be reacted with water (or more dilute H2SO4) to form sulfuric acid of a high concentration.
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testimento
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[*] posted on 29-6-2013 at 16:10


Could the reaction be enforced with UV light source that is used with other chlorinating processes? Does the chlorine gas return as Cl(2) after it reacts with dilute H2SO4? The chlorine way sounds better for me than NO, easier to manufacture.

Thanks about the book and sorry I missed it.

Just about the chlorine, if I make a reactor where I feed chlorine and SO2 and add continously little water, there will be SO2Cl2 formed which forms droplets and sink in the water and Cl2 is formed again to react the excess SO2 fumes again and again. Where am I gonna make the reactor walls so they wont corrode under chlorine gas? 316 steel wont hold it at all, but it can hold with ease with sulfuric acid. Should I coat the walls with PTFE foil and use glass feed tubes?

[Edited on 30-6-2013 by testimento]
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plante1999
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[*] posted on 29-6-2013 at 16:19


You better listen to me if you want good acid, look under its name:

Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!

Altough this one is true, it will give you mixed hydrochloric and sulphuric acid!




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testimento
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[*] posted on 29-6-2013 at 16:35


Are you sure? SO2Cl2 + H2O = H2SO4 + Cl2 as I count it, or should this reaction need more than one molecule of water? It could create chloric acid, but the proportion of that in water is quite minimal compared to the amount of sulfuric acid and can be cooked off by slightly heating the solution when the reactor needs to be drained.

And is the UV radiation what is needed to catalyze the reaction as does with other chlorine compounds what is wanted from sunlight?

And I dont think anyone is going to build a 100-liter reaction vessel, 5 000 watt electrolysis device and all other stuff by accidentally coming up with such info on the internet. We can speculate, somebody always knows something and when people gather around, they can come up with completed information together. Collective intelligence.

[Edited on 30-6-2013 by testimento]
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plante1999
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[*] posted on 29-6-2013 at 16:45


No comment, keep listening to him, I don't mind.

Balanced equation:

2H2O + SO2 + Cl2 -) H2SO4 + 2HCl

"And I dont think anyone is going to build a 100-liter reaction vessel, 5 000 watt electrolysis device and all other stuff by accidentally coming up with such info on the internet. We can speculate, somebody always knows something and when people gather around, they can come up with completed information together. Collective intelligence."

By myself I can come up with something pretty nice, I'm more of the guy with people gathering around, and... I'm tired of sciencemadness for the moment.

I'll see might take a break, anyway if someone want to talk with me he know where he can contact me. Tired of all the people not even able of balancing a simple F**king equation and arguing about the certainty of other member.

...

[Edited on 30-6-2013 by plante1999]




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[*] posted on 29-6-2013 at 18:49


Can you get copper sulfate root killer? If so, you can electrolyze it to get dilute H2SO4.



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testimento
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[*] posted on 30-6-2013 at 04:10


Yes, but it costs quite a lot even when bought at larger quantities. By my calculations, only some 20-30% of the total mass is actual copper sulfate which can be utilized so every liter of sulfuric acid would cost 13-16 euros.

Well, maybe junk dealer will buy the residue copper and cover part of my costs.

Should Lead dioxide work well with this process? I have a 20-stack of industrial-grade PbO2 electrodes. I'll get a small bag of this shit and run a test batch and make some calculations what will be the actual price. I calculated that I could make H2SO4 with ozone and SO2 2.5-3 times cheaper.
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