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Korialstrasz69
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HELP(sulfuric acid)
Hey everyone.New member here.
I have some questions :
1-
how to synthesis a small amount of sulfuric acid from Ammonium sulfate without the use of any acids ?
please suggest your method in details with description of every case of things going wrong(as far as you know)
i don't have any acids and i cannot buy them nor online nor offline(Welcome to syria)
but i have some lead to be used as an electrode.(No i can't get platinum)
Now i have a lil questions:what other materials than pyrex resist Corrosive acids/bases ?and conducts heat good ?it's not necessary to resist high
temperatures.
Thanks anyways :3
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Sulaiman
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If there is no Sulphuric acid available,
what do you use in lead-acid batteries ?
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Bert
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Thread Moved
24-9-2015 at 02:49 |
100PercentChemistry
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Electrolysis
https://m.youtube.com/watch?v=5dUSF9Gl0xE this way uses copper sulphate. I will keep looking for an ammonium sulfate method.
[Edited on 24-9-2015 by 100PercentChemistry]
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100PercentChemistry
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sorry
Most methods use hcl. https://m.youtube.com/watch?v=_RglgJQ8vIg. This uses sodium bi sulphate or ph down. Is this available in Syria? After you are done, just boil it
to the concentration you want and titrate.
[Edited on 24-9-2015 by 100PercentChemistry]
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100PercentChemistry
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I guess borosilicate glass resists heat good. I've only had one temperature related breakage. That was when it was really hot and I added ice cold
water, it shattered. It also resists common acids except HF. Regular glass will work against most acids, but is not for heating.
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Korialstrasz69
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Sulfuric acid is only provided to battery repairing specialists and these are watched by the government,and if you ask one of them for some sulfuric
acid you will probably be arrested for terrorism since you know what "Sulfuric" means.
And i need a renewable source like i can always buy NH4SO4 but i can't afford 80$ battery for each batch of acid.
anyways the copper sulfate seems good,but can i by any way transform ammonium sulfate to copper sulfate ?maybe melting the salt with copper wire would
work ?
i saw like most of them videos by NurdRage and as i said,no acids available here.And i highly suspect the bisulfate is available or even provided to
the public.And i have no idea where to search and no one to ask for a "Pool chemical supplier".
anyway thanks for all the responses,looking forward for my first batch.
btw does anyone around suffer the same shit as here ?
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100PercentChemistry
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"btw does anyone around suffer the same shit as here ?"
I live in the U.S. it is not as bad here. But slowly it is getting harder. Some stores have stopped selling sulfuric acid drain cleaner. Also iodine
became a list 1 chemical in th east couple of years.
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aga
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Where are you Korialstrasz69 ?
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zed
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Well, apply a vacuum to it, while heating in a microwave oven.
Should be in the search engine somewhere. I'll look.
http://www.google.com/patents/US20040234441
US5951831.Condensation.Polymerization.Phosphoric.Acid.pdf
[Edited on 25-9-2015 by zed]
[Edited on 25-9-2015 by zed]
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Korialstrasz69
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aga Lattakia-Syria,why ?
Zed i do know the pattern and it gives me hope in dark nights,but i need one little batch to start off the production.
what are you talking about,vacuuming and heating ?i can't vacuum.my tools are as simple as a cookware but if you're talking about transforming the
ammonium => copper sulfate i can maybe get a teflon pan,or i don't even mind ruining an aluminum can for that purpose,it's a one time process and
then i can apply the pattern.
besides what are you talking about phosphoric acid and polymerization and shit ?
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macckone
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Simple method of converting ammonium sulfate to copper sulfate.
Requires copper carbonate.
This is a double displacement reaction.
Mix ammonium sulfate with an excess of copper carbonate.
Mix enough water to form paste.
Then heat it while stirring with good ventilation.
The ammonium carbonate will decompose and leave the
mixture. This requires high heat and teflon is not advised.
Repeat with more water until you have a nice blue.
Then dissolve your copper sulfate and recrystallize.
Sodium bisulfate can be decomposed to make sulfur trioxide
as can ferrous or ferric sulfate and copper sulfate.
These are relatively low heat.
But require a distillation apparatus or ceramic retort.
If you have access to pottery supplies then a ceramic retort
should be relatively easy to make.
Magnesium sulfate aka epsom salt (which should be readily
available) can be electrolized in a diaphram cell.
Both calcium sulfate and magnesium sulfate give off
sulfur trioxide and sulfur dioxide at very high temperature.
The lead chamber method is workable for a home chemist.
There is a thread on here about that method.
Finally there is also a thread on burning sulfur and
using vanadium pentoxide to produce sulfur trioxide.
Last method, get some lead acid batteries and pour
the sulfuric acid out. Then heat to concentrate the
sulfuric acid. It may be contaminated with lead
but the solution to that is to dilute it to 10% then
filter as lead and lead sulfate are less soluble at
that concentration. Then reconcentrate it.
If you only need a small amount the last method
is probably your best bet.
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Korialstrasz69
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macckone,You're god mate ! thanks !
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zed
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The method used to convert Ammonium Phosphate to Phosphoric Acid and Poly-Phosphoric acid...may be applied to Ammonium Sulfate, to produce Sulfuric
Acid. Heat a little Ammonium Sulfate in a microwave. If you smell Ammonia, the reaction is Working. Sulfuric Acid is a high boiler. It is possible
to boil off Ammonia and Water vapor, while leaving the Sulfuric Acid behind.
Think about it.
Since you are in Syria, what the hell do you need Sulfuric Acid for? Seems to me, there has been a war raging, and unauthorized possession of such an
item might result in serious punishment.
Just assuming access to Microwave ovens. Where I live, folks sometimes discard working units, with their trash. But, it is a big world, and
conditions vary.
Guys from the UK, have reported difficulty in obtaining regular ice. While, Dry Ice, is something they can only dream about.
[Edited on 25-9-2015 by zed]
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Korialstrasz69
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Pretty sure it will be no more than ammonium bisulfate,plus i cannot afford to fuck our microwave up with ammounia :3 Am thinking melting the salt and
decomposing it then separate the bisulfate with alcohol and then reheat it with copper,maybe it works.
Now imagine your lab without acids.the only reaction you can do is probably hot ice ._. .from sulfuric i can get hydrochloric and might get my hand on
some nitrate.from that point i can have some fun and do real reactions.Since i started i made sure no one suspects it,i don't go around asking stores
for nitric acid and i never order big supply and never online and never mail delivery.And please,ammonium sulfate is the most "unsuspectable"material
and it seems i can access everything from it.so pretty safe i assume.
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ave369
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1. Heat ammonium sulfate in a microwave oven to produce ammonium bisulfate. Nothing can go wrong here, except some stench of ammonia, but this is
expected.
2. Dissolve this in water, add bicarbonate of soda, and boil. The stench of ammonia will appear again. Ammonium will be removed, you will have a
solution of sodium bisulfate. Crystallize it.
3. Melt and calcine sodium bisulfate, it will turn into pyrosulfate. Use a porcelain cup instead of a crucible, if you have no access to proper
crucibles. Stop the calcination when you see persistent, corrosive white fumes emerging instead of common water steam. This is your sulfuric acid
escaping.
4. Put sodium pyrosulfate in sacrificial glassware (or, better, a tube made of some corrosion-resistant metal) and heat it like hell on a gas burner.
Evolving SO3 should be directed into sulfuric acid (this results in oleum), but since you have no sulfuric acid at start, try to just condense it. Be
careful: this anhydride is extremely hazardous! Do this outside, wear goggles and a respirator or, better, a gas mask! (obtaining one of those in
Syria should be easy; with all those gas attack scares, you should have a lot of these distributed among the civilians as civil defense). White,
extremely corrosive fumes will escape the apparatus, and they will also emerge when you VERY CAREFULLY drip the anhydride into water. Do it only after
you put the water on the bottom of a large round-bottom flask, so the flask walls will protect you from any acid sprays and sprinkles!!! Do not, under
any conditions, drip water into pure SO3!!! But you only have to deal with the pure pandemonium trioxide the first time, later you will have some
sulfuric acid to be turned to oleum.
You can also pyrolyze the halfway calcined bisulfate which still has some water in it. This way, you will condense oleum instead of pure sulfur
trioxide. This should be preferable if you have no sulfuric acid to absorb the trioxide.
5. I have some unverified info that adding magnesium sulfate (sold in drugstores under the name of Epsom salt, calcine it beforehand to make sure it's
anhydrous!) to sodium pyrosulfate makes the pyrolysis easier. I'll check it out soon.
6. When you have prepared oleum, be extremely careful when diluting it to 98% sulfuric. Normally, you dilute oleum with 70-80% sulfuric (the
boiled-down Bat), such a dilution is calm and does not produce any spectacular and destructive special effects. Since you don't have that, pour your
oleum on a bottom of a large round-bottom flask and carefully, drop by drop, drip water. Oleum will spray and sprinkle, water will flash-boil.
However, any sprays and sprinkles of acid will be stopped by the flask walls. Continue to do this until the oleum no longer fumes.
You can make a retort for pyrolysis out of steel plumbing and a thin steel tube as the "nose". It should be all-steel, because steel is passivated by
conc. sulfuric. Buy a lot of plumbing parts of different sizes and threads in a hardware shop and assemble a retort from them. Bottles can be
substituted for flasks if the process does not involve heating them. Small round-bottom flasks can be made out of lighting bulbs.
[Edited on 26-9-2015 by ave369]
Smells like ammonia....
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j_sum1
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I just watched a youtube video on making sulfuric acid using magnesium sulfate and oxalic acid. It is a simple precipitation reaction. If you have
access to these, it might be an eaay route.
Search for "sulfuric acid new method".
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ave369
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j_sum1, nice find! This way, it seems, one can make dilute sulfuric acid, a substitute for the Bat, in any amounts. However, one still needs to boil
it down, and boiling down to 98% is a huge mess. I boiled the Bat many times but never got above 94% (even that required tricks and perversions). If
one needs 98%, pyrosulfate pyrolysis is the way to go.
I think, the Zintl-Karyakin method also deserves an honourable mention. This is a method for purifying boiled-down Bat or similar low-grade
concentrated sulfuric acid. You add potassium dichromate into it and distill. This requires a retort you are ready to lose, and should be done
outdoors (hexavalent chromium is a carcinogen, you don't want it to be sprayed in your home in case of glassware failure). The retort or boiling flask
should be thermally insulated with rockwool or a similar material. Discard the first, dilute grams of distillate, and you will get high-grade 99%
sulfuric acid (chromium trioxide, AFAIK, is an azeotrope breaker).
You can prepare dilute sulfuric acid by the method with oxalic acid, then boil it down as much as possible, then purify it using the Zintl-Karyakin
method. And use this acid to absorb SO3 to get oleum.
I think that a "Plumber's Nightmare" steel retort is ideal for Zintl-Karyakin, since it is immune to thermal cracking and not corroded by conc.
sulfuric. In it, you probably can do the process even at your home. One hurdle: for this retort, your boiled-down acid must be as strong as possible
(94+%). Halfway-boiled acid (80%) produces dilute sulfuric acid vapors when distilled, and these slowly attack the steel pipe instead of passivating
it.
[Edited on 26-9-2015 by ave369]
Smells like ammonia....
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ave369
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Here is a crude drawing of a DIY oleum still. Substitute pyrosulfate for sulfuric + dichromate for Zintl-Karyakin distillation.
[Edited on 26-9-2015 by ave369]
Smells like ammonia....
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j_sum1
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Out of interest, would copper pipe work for the retort? Is Cu resistent to SO3 or oleum?
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ave369
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I doubt it. Hot concentrated sulfuric acid oxidizes copper, but passivates iron. Nota bene: iron is only completely passivated by
cold sulfuric acid, but hot acid does slowly attack it. However, if the apparatus is robust enough, it won't eat through it. You'll at most get a
minor contamination of green vitriol in the resulting distillate.
[Edited on 26-9-2015 by ave369]
Smells like ammonia....
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Korialstrasz69
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Thank you all folks.i think i'l try to get a crucible and try the pyrosulfate way.
btw how does one get oxalic acid?i think it's sold in pharmacies ?
and i don't think i need that much concentration,90~95 is good enough to cook more with ammounium sulfate i think.but thank you all,great gods of
chemistry :3
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ave369
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Oxalic acid is sold in hardware stores, as cleaning powder to wipe off insoluble salts from hard water.
And more concentration is always better than less. You can skip the calcining step and put sodium bisulfate directly into the iron retort. This way
you will make (theoretically) 100% sulfuric acid, but in fact a weaker solution because part of SO3 will escape. And, at one point, dilute H2SO4 will
be condensing in the steel pipe, damaging it and fouling your distillate with green vitriol. So it's better to use half-calcined bisulfate/pyrosulfate
mixture and distill oleum.
Don't forget the respirator or gas mask! SO3 is vile shit!
[Edited on 26-9-2015 by ave369]
Smells like ammonia....
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j_sum1
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For the record, I intend to attempt the oxalic acid + epsom salt route to H2SO4 some time soon. It looks to be a bit more expensive than
electrolysing copper sulfate but a whole lot faster. About the same amount of boiling down will be required.
I intend to have the OA in slight excess. I don't want to have stray Mg in my final product. A bit of research suggests that oxalic acid decomposes
at moderate temperatures in concentrated H2SO4. Reported by Gay Lussac in 1832 no less!
I may attempt Ave's concentration methodology using pyrosulfate but it is probably overkill for me. I doubt that I really need to play with SO3.
When I actually need 98%+ in large quantities, I will simply bite the bullet and pay for dangerous goods shipping from a reputable supplier.
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Korialstrasz69
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Fuck this.clay is absence since a year because it all comes from another city and steel god knows.
i wanna ask what plastics resist SO3 ?i saw the plastic resistance sheet but it only tells about 2% and 5% sulfuric acid..does that mean none resist
more than that ?because PVC is available...
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ave369
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Plastics do not resist heat. And pyrosulfate pyrolysis occurs at 500-600 Celsius. Any plastic will burn at these temperatures. Ditto with plain
boiling down: this requires 300 Celsius, which no plastic can survive either.
Smells like ammonia....
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