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Korialstrasz69
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Well i was planning to do the pyrolysis in a porcelain cup and the condensing in a plastic tube or an iron tube (doesn't seem wise to me at least)but
let's see if every two bisulfate molecules released two molecule of water and every pyrosulfate released 2 SO3 it will make 100% sulfuric acid which
seems to burn PVC...
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Korialstrasz69
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Umm...fuck...
SO2 if much less corrosive than SO3 and both 20% H2O2 and elemental sulfur is available...i just discovered this method ._.
uhm... sorry ._.
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macckone
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You probably have access to lead there as well. You may need to get a car battery and
drain the sulfuric acid and then melt the lead plates but I am certain lead acid batteries
are available. You may also be able to get wheel balancing weights. Lead is easily melted
and molded. It is also pretty resistant to sulfur dioxide, sulfur vapor, sulfur trioxide and
sulfuric acid. It makes an ideal material for the collection and condensation apparatus.
Leads melting point (620C) is only slightly above(60C) copper sulfate's decomposition
temperature (560C). But it is significantly above(160C) that of sodium pyrosulfate's
decomposition temperature (460C).
Steel will not be significantly corroded by DRY sulfur dioxide or trioxide but is corroded
somewhat by sulfur both as the liquid and the vapor. And even slight traces of water
and all bets are off.
Of course lead and steel can be unwanted contaminants in your sulfuric acid.
If your reactions can't tolerate them you have to go with glass or ceramics.
[Edited on 29-9-2015 by macckone]
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ave369
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Quote: Originally posted by Korialstrasz69  | Umm...fuck...
SO2 if much less corrosive than SO3 and both 20% H2O2 and elemental sulfur is available...i just discovered this method ._.
uhm... sorry ._. |
If you want to make dilute sulfuric acid, you'd better use MgSO4 + oxalic acid method. Both reagents are cheaper and more common than H2O2.
Smells like ammonia....
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Korialstrasz69
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i can't get both probably because of my lack of knowledge,and lead batteries are available but way too expensive for me,and anyway can't i concentrate
it as far as 90% with boiling ?also i saw on wikipedia that SO2 is lever 0 oxidizer while SO3 is lever 3 oxidizer ,so i can burn sulfur in a tin can
and bubble it through H2O2 (Which is easly available,only a little expensive) and that's how i'l get my first batch and what follows will be prepared
with this neat formula : http://www.google.com/patents/US20040234441
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j_sum1
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| Quote: Originally posted by Korialstrasz69 | i can't get both probably because of my lack of knowledge,and lead batteries are available but way too expensive for me,and anyway can't i concentrate
it as far as 90% with boiling ?also i saw on wikipedia that SO2 is lever 0 oxidizer while SO3 is lever 3 oxidizer ,so i can burn sulfur in a tin can
and bubble it through H2O2 (Which is easly available,only a little expensive) and that's how i'l get my first batch and what follows will be prepared
with this neat formula : http://www.google.com/patents/US20040234441
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Yee-Ouch!
Andd you think this is going to be cheaper?
By the time you invest in enough high temp equipment to do this safely and deal with your hot gas stream, you are certainly going to be out of pocket.
It's an interesting idea, but
1. Patents have a way of not disclosing everything and so, be prepared for some surprises (including the possibility that it won't work at all.)
2. Dealing with two hazardous chemicals simultaneously at close to 300 degrees is not for the faint-hearted and is certainly not something a beginner
should attempt. (I would count myself a beginner in this case.)
3. I am going to be lazy here and not look up the thermodynamics. It would not surprise me in the slightest if it was infeasibe. Check it out before
proceeding. It seems to me that if it was a workable process then it would be one that would be done on an industrial scale long ago.
4. Even if it does work, I think you will be in for quite a bit of experimenting before you get a setup that works reliably. Just a hunch.
Seriously, I recommend electrolysis of copper sulfate. Slow but effective. CuSO4 is not too hard to obtain. You can do it in a plastic container
with a piece of lead, a strip of copper and an old phone charger. You can get good quality acid this way. What's not to like?
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macckone
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Oxidation of sulfur dioxide by hydrogen peroxide is pretty effective.
There are a number of youtube videos that use this method but you really
need 30% or higher hydrogen peroxide to get a decent yield and sulfur dioxide
is not very soluble so you need much more sulfur than the equations would indicate.
Concentrating hydrogen peroxide is also relatively easy, just tedious and you get
a good amount of loss.
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Korialstrasz69
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Copper sulfate's unavailability.i got both ammonium sulfate and sulfur by chance since both are fertilizers.but i can't get that shit i don't even
know where.
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j_sum1
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Let's see if I have this right.
* You live in Syria, which is probably not the easiest place to do amateur chemistry.
* You have access to sulfur, ammonium sulfate and hydrogen peroxide. (Unusual mix.)
* You don't have easy access to any other reagents. (I wonder if you have exhausted all possibilities though.)
* In particular you cannot get copper sulfate, copper carbonate (which can be made fairly easily btw), oxalic acid or epsom salts.
* You are relatively inexperienced as a chemist (implied, not stated.)
* You have been provided with probably the most concise list of routes to H2SO4 that I have ever seen. Twelve methods plus variations by my count.
And you are gravitating towards the methods that require SO3 or evolve high temperature ammonia.
Just exactly what do you need 98% sulfuric acid for anyway?
I am not really trying to discourage you, but I do think, walk before you run. I am all for experimentation and think that adapting a method to suit
your own particular local constraints is a great idea. I am just confused by the whole scenario where you have almost no basic reagents but need
concentrated sulfuric for... something. I am also confused as to why you want to attempt the ambitious before attempting to purchase some epsom salts
and a flower pot. (Both available from a garden supply store.)
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100PercentChemistry
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To make copper carbonate use
Materials:
50 ml Beaker
100 ml Beaker
25 ml sodium bicarbonate
12V 2A switching power supply
Water
Copper wire, 12 gauge
Evaporating dish
Electrical or Duct tape
Small Glass Jar
Stirrer
Acetic acid (vinegar)
Procedure:
1. Gather materials
2. Measure 50 ml of hot water in the 100 ml beaker
3. Measure 25 ml sodium bicarbonate into the 50 ml beaker
4. Add water to 50 ml beaker
5. Bend copper wires and attach to power supply wires with power supply still unplugged
6. Tape power supply wires down
7. Insert wires into 50 ml beaker with the bent parts over the lip
8. Observe beaker
9. Plug in power supply
10. Observe reaction, taking note every thirty seconds for five minutes
11. Take note every 5 minutes until 30 minutes
12. Record final observation at 1 hour
13. Add 80 ml of boiling water to 100 ml beaker
14. Filter out water from from electrolyzing beaker and scrape resulting solids into 100 ml beaker
15. Stir 100 ml beaker contents
16. Re-filter mixture
17. Scrape solids into evaporating dish
18. Wait until solids dry
19. Crush resulting material with mortar and pestle until a fine powder
20. Store resulting powder in jar. To test material, add acetic acid, if the material bubbles and becomes a green solution the material is copper
carbonate.
[Edited on 1-10-2015 by 100PercentChemistry]
[Edited on 1-10-2015 by 100PercentChemistry]
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100PercentChemistry
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Do you have a power supply like a computer fan, powerful battery(lantern batteries are usually 9v 1am0), or a dc power supply?
Again what do you want to synthesize?
What type of stores do you have?
[Edited on 1-10-2015 by 100PercentChemistry]
[Edited on 1-10-2015 by 100PercentChemistry]
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Korialstrasz69
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First of all,really sorry for the long post and mind fuck and insisting on getting the acid and all,but that's that.we got a few good methods for
everybody anyway so nothing went to waste.
I can get epsom salt,first of all.oxalic acid i cannot go around asking for it but still a i might find it.Hydrogen peroxide is available as a tooth
whitener and sulfur is available for tomato fertilizing,and ammonium sulfate is a regular fertilizer very well so yes not so unusual.don't wanna brag
but am not inexperienced,maybe i am actually,i have just been reading for years now and saw a whole lot of videos(NerdRage,NileRed,ChemPayer)and read
a whole fucking lot of wikipedia,so i know at least basics in working with chemicals.
this part you can skip,but i have a good cause for every single method:
1-i don't know where to get copper sulfate and don't want attention since i already said chemistry means explosive here(If it's only used by
chemists).
2-i don't have HCl and here we clean drains with NaOH.
3-A dollar costs 300 Syrian pond and i can't afford a 28k S.P battery.
4-i already left a piece of copper to rot into carbonate,need time.
5-i lack knowledge about diaphram cell i must admit.
6-since the first few methods and am looking and asking around for steel pipes or raw clay but both are not used,hardware stores sell pure iron pipes
and my city isn't getting any clay since people have been hiding weapons in clay jars(still can't get the logic here really but it's a fact).
7-and vanadium pentoxide...you guessed it.
8-ave369's method seemed great,but as i said no means available to withstand SO3 or oleum.
9-still looking for oxalic acid.
10-that's it(please kill me).
i feel like a shit.
anyway am planning to use our vacuum cleaner to make sulfuric acid from sulfur's SO2.i have already dealt with hot ammonia in my fucking kitchen,and
the experiment will be done outside anyway.and no SO3 is involved in the patent.
"Just exactly what do you need 98% sulfuric acid for anyway?"
Please stop asking this,you can't run a lab without oxidizing agents and acids and especially sulfuric acid since it's needed in equilibrium reactions
that release water.i don't have much time now but tomorrow i'l come with a bunch of reactions that i can't preform due to lack of acids.
Sorry everybody for the long post and for bothering you all with searching,especially you j_sum1,but i never realized how hard is it to be an amature
chemist in a war situation.Also sorry for turning this post from chemistry to personal problems.
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j_sum1
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| Quote: Originally posted by Korialstrasz69 |
Sorry everybody for the long post and for bothering you all with searching,especially you j_sum1,but i never realized how hard is it to be an amature
chemist in a war situation.Also sorry for turning this post from chemistry to personal problems. |
No offense taken. In any case, this has turned out to be a worthwhile thread since it summarises in one place so many different methods for obtaining
an essential reagent.
And I am sure that being an amateur chemist in a war zone is fraught with difficulty.
For the record, it has taken me a year to incrementally build up my lab and I am still making my own acids (except HCl). The truth is though that you
can do a lot of chemistry at small scale and don't need a large quantity of anything.
[edit]
Copper sulfate may be available as a fungicide or as an agent for preventing root growth in drains etc. ("Rooto" in the US.) I got mine from a
pottery supplier. You can probably order it online. It is unlikely to raise any suspicions. (You could always spray some on your tomatoes.) And if
you have copper wire and a soluble sulfate salt (which you do) then you can make it easily enough through a number of different routes.
This might be exactly what you want. An alternative is to use an unglazed terracotta flower pot inside a bucket to act as a membrane and separate
the two half cells. It might be a more reliable and robust setup than a suspended coffee filter.
Alternatively, by use of an inert electrode you could go directly from magnesium sulfate to sulfuric acid dropping a Mg(OH)2 precipitate. (Although I
have no actual experience of this method.)
[Edited on 1-10-2015 by j_sum1]
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NedsHead
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| Quote: Originally posted by j_sum1 |
Copper sulfate may be available as a fungicide or as an agent for preventing root growth in drains etc. ("Rooto" in the US.) I got mine from a
pottery supplier.
[Edited on 1-10-2015 by j_sum1] |
I get mine from the garden section at a hardware store, it says on the container that it is used for correcting copper deficiency, it can also be
called Bluestone
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Little_Ghost_again
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I found a list but it seems the site has now gone!! I dont think the Op has any chance of getting copper sulphate, it was on the embargo list I saw. I
think also its really easy to under estimate just how much of a risk he is taking buying some of these things.
I am not going to get political but I feel for the guy, its a terrible situation over there, seems like 3 sides all fighting and anybody remotely
buying something that could be turned into something is probably not going to fair well. The other thing is human rights, lets face it if he is
suspected of something it isnt likely he is going to get anywhere near a trial let alone a fair one.
Clay.....
I no nothing of your country but I do know most countries have clay somewhere below the subsoil, if it was me I would find where people hate growing
things because the soil is hard to work, I would then go and grow things there  .
Clay from my own experience normally comes up pretty clean once you get a couple feet down. A computer fan and decent wood fire with a mud surround
might just get your clay baked enough to use as a retort. I appreciate this isnt ideal but somewhere not too far from you there is surely some clay to
dig up  .
This might be utter crap but maybe a ceramic mug with a homemade clay retort top from clay you dig and fire might do the job for you.
I dont know the chemistry but seeing as you can get sodium hydroxide and copper wire maybe there is a way to copper sulphate from that? others will
need to guide on this as my knowledge is zero.
Keep us informed and carry on being careful, I watch the news alot and seeing as they are bombing the shit out of hospitals with foreign civilians in
them that are phoning up and pleading to stop and yet just because they think the bad guys are there they continue. Keep safe my friend chemistry
isnt worth dying for.
I salute you for having the balls to attempt this.
One other thought I had was maybe if you could get lead sheet like used on roofs you could line some steel with this to try and cut down on the
attacking from the weaker acid. If I could get away with it I would send you the 250g of copper sulphate I have, but my worry would be it might cause
you problems receiving it.
One thing I might be able to do for you is return a favor that someone kindly did for me on here, I got sent some MMO electrodes, I cant spare much
but I am more than happy to cut some bits off and send them. I doubt a couple of small bits would raise suspicion. Let me know if its possible to get
post from the uk.
Dont ask me, I only know enough to be dangerous
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Little_Ghost_again
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I know you want sulphuric acid but this might help as well. you can get hydrochloric acid from baking soda and table salt
NaCl + NaHCO3 ® HCl + Na2CO3
Also you have access to PVC, on here is a thread or two and one where aga pyrolized PVC and bubble the gas into water to make hydrochloric acid. I am
just trying to think of some ways to get you acids, maybe hydrochloric would be safer and easier to start with??
Dont ask me, I only know enough to be dangerous
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j_sum1
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Are you sure?
I would have thought that reaction would go in the other direction.
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Little_Ghost_again
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No i am not sure I thought it had posted the link I will try again sorry http://amedleyofpotpourri.blogspot.co.uk/2011/12/making-hydr...
Looks like I didnt paste the link last time  , I havnt got a clue if it works
but maybe the link will help answer some questions, I just skimmed through to be honest, I was hoping to help as the thought of someone with little
equipment trying to mess with some of the reactions is pretty scary.
I bitch about living in the middle of no where and not having pool shock local to me, reading this kind of thread really puts things in perspective. I
am also kinda impressed that despite everything going on over there people are trying to have a life and do a hobby that carries some serious risks
for them. It just hit a nerve with me and made me think that maybe I am not as bad off as I thought
[Edited on 4-10-2015 by Little_Ghost_again]
Dont ask me, I only know enough to be dangerous
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j_sum1
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Ok, so it is heated to drive the reaction to the right.
The products look like the standard acid + carbonate reaction: resulting in salt plus water plus CO2. What prevents this from occurring?
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Little_Ghost_again
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| Quote: Originally posted by j_sum1 | Ok, so it is heated to drive the reaction to the right.
The products look like the standard acid + carbonate reaction: resulting in salt plus water plus CO2. What prevents this from occurring?
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I only skimmed it to be honest, but I have some bicarb I found today lurking in a box, so I could give it a go after school if it helps?
Dont ask me, I only know enough to be dangerous
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Little_Ghost_again
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I read it to mean heat the salt and sodium carbonate to make the HCL, where is the acid apart from the HCL? I am just guessing but the heating drives
the gas out the tube. Sorry j_sum1 I dont know anything about this but will try with the bicarb tomorrow and see what happens.
Somehow though it might be easier for him to use PVC and heat that. Some HCL would at least give him a few other options for now
Dont ask me, I only know enough to be dangerous
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ave369
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Also, pure iron pipes will do. Maybe a bit more green vitriol impurity, but it will work.
Smells like ammonia....
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Korialstrasz69
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First of all,thank you very much Little_Ghost_again,it's really helpful to have someone feeling for you 
well now,all good grade clay for pottery comes from the city of Hama,witch stopped coming even for arts students because they've been hiding weapons
in it,but i don't think i need that anymore.
check this out:
http://imgur.com/UpDHrfh
can you guess what that color is?it's copper ions bruh!
as i mix and heat i believe i will get a nice batch of Copper sulfate ready for electrolysis,and anyone would prefer the wet chemical way on the high
temp way.and as i get my first batch i think il be using the patent and get going
thanks you very much for your offer bro,but i prefer not,i think carbon electrodes will work good enough,and i might be a little suspected already.
like we were talking about breaking bad and chemistry in college other day when that old man came asking for some money.as he walked be we looked
back and he disappeared,another man came and said something to us about him.i think i might be watched.
nonetheless,i think am in a relatively safe area.
thank you all for responses,if this one idea fails i think i'll attempt the PVC method,Thanks again all !
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Little_Ghost_again
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| Quote: Originally posted by Korialstrasz69 | First of all,thank you very much Little_Ghost_again,it's really helpful to have someone feeling for you
well now,all good grade clay for pottery comes from the city of Hama,witch stopped coming even for arts students because they've been hiding weapons
in it,but i don't think i need that anymore.
check this out:
http://imgur.com/UpDHrfh
can you guess what that color is?it's copper ions bruh!
as i mix and heat i believe i will get a nice batch of Copper sulfate ready for electrolysis,and anyone would prefer the wet chemical way on the high
temp way.and as i get my first batch i think il be using the patent and get going
thanks you very much for your offer bro,but i prefer not,i think carbon electrodes will work good enough,and i might be a little suspected already.
like we were talking about breaking bad and chemistry in college other day when that old man came asking for some money.as he walked be we looked
back and he disappeared,another man came and said something to us about him.i think i might be watched.
nonetheless,i think am in a relatively safe area.
thank you all for responses,if this one idea fails i think i'll attempt the PVC method,Thanks again all ! |
Not being funny but probably best to say nothing to nobody where you are. I lived in another part of UK that was full of clay, I now live in Scotland
and there is no clay just peat. Funny thing is when I was in Devon I wanted peat for some aquarium fish, the clay was a pain. Now I live in Scotland
the fish are happy but I could do with some clay for an oven lol.
Congrats on the copper, the PVC should give you hydrochloric and from there you are away!!
Keep things low key no such thing as a safe place, ask those that were working in the hospital  .
Dont ask me, I only know enough to be dangerous
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AJKOER
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Just found this "Acceleration of Sulfurous Acid Oxidation by Freezing of Aqueous Solution", by Kazuhiro, link: https://www.researchgate.net/publication/244692896_Accelerat... , to quote from abstract:
"Oxidation of sulfurous acid (H2SO3) to sulfuric acid (H2SO4 by dissolved oxygen (O2) in an aqueous solution was remarkably enhanced by freezing. The
concentration of sulfurous acid in a sample solution which froze in a - 10°C refrigerant for 60 min decreased by about 50%, and three freeze/thaw
cycles resulted in perfect conversion into sulfuric acid. The difference of reaction rates in -20°C and -10°C refrigerants indicated that the
rate-determining step of the reaction was the growth rate of ice formation in the sulfurous acid in an aqueous solution. The yield of sulfurous acid
oxidation in a -10°C refrigerant was higher than that in a - 20°C refrigerant."
-----------------------------------
My speculation on the pathway is the presence of a transition metal impurity, low pH, and dissolved oxygen that resulted in the formation of some
Fenton products. The hydrolysis of two such products is:
.OH + -OH = .O- + H2O
My recent research indicates at standard conditions the reaction equilibrium is actually favored to move more to the right with the formation of the
so called hydroxyl radical anion .O- (see, for example, http://pubs.acs.org/doi/abs/10.1021/j100087a022 ). But, somewhat problematic is that low pH moves the equilibrium to the left. However, the
formation of ice effectively removes water along with increased viscosity arguably could move the reaction back to the right.
Assuming the hydroxyl radical anion is created, I do recall the following reaction with it and oxygen ([Edit] Found a reference, see page 182,
equations R36, R37 and R38 in "Plasma Kinetics in Atmospheric Gases", by M. Capitelli, et al., link:
https://books.google.com/books?id=2ofqCAAAQBAJ&pg=PA182&...):
R37 .O- + O2 = O3 + e
R38 .O- + O2 = O + O2 + e
Or, possibly as:
.O- + O2 = .O3-
where I suspect the .O3- radical anion, or whatever products per above, would certainly be a stronger oxidizer than O2. The speculated reaction could
then be:
H2SO3 + .O3- = H2SO4 + .O2-
More background on .O3- radical anion, please see https://books.google.com/books?id=7B8KwVVZRPEC&pg=PA85&a... and this reference referring to it as the ozonid anion at https://books.google.com/books?id=qyN6_83vz2MC&pg=PA472&... . Note, the last reference notes O3 + e- = .O3- and the former, O3 + e- = .O- +
O2, which appears to support my cited equilibrium formation reaction of the ozonid radical anion stated above.
More associated reactions:
2 .O2- + 2 H+ = H2O2 + O2
where the oxygen could be partially recycled, and the hydrogen peroxide likely consumed in a Fenton reaction, or with Sulfurous acid:
H2SO3 + H2O2 = H2SO4 + H2O
Interestingly, some reactive oxygen species (like Singlet oxygen, for example) are best formed at low temperatures (and also, preferably at neutral to
high pH conditions).
---------------------------------
[Edit] I would be remiss not to cite a well documented path by passing air/O2 through H2SO3 in the presence of a hydroxyl radical source (like by
action of sunlight on aqueous N2O, or aqueous nitrite or nitrate salt, or a Fenton-like reaction with a transition metal oxide like Cu2O, FeO.Fe2O3,
TiO2,..).
For example, per one source: "Rate Constants for Reactions of Inorganic Radicals in Aqueous Solution" by P. Neta and Robert E. Huie, to quote:
"3.11. Sulfite Radical
The .SO3− radical is most commonly produced by the reaction of .OH with sulfite or bisulfite.
.OH + SO3(2−) → OH− + .SO3−"
And further:
"3.13. Peroxomonosulfate Radical
The SO5.− radical is produced by the reaction of .SO3− with O2.
.SO3− + O2 → SO5.−"
Also:
"The SO5.− radical is a stronger oxidant than .SO3−, with an estimated redox potential of 1.1 V at pH 7.39. It is still quite selective in its
reactions, oxidizing hydroxybenzenes at high pH rapidly but only slowly or not at all at low pH. The radical possibly also reacts by oxygen-atom
transfer with sulfite or bisulfite.
SO5.− + SO3(2−) → SO4.− + SO4(2−)
In such a case, the SO4.− would react rapidly with the SO3(2−), regenerating .SO3−, and thus making it difficult to distinguish this reaction
from an electron transfer path. "
Link: https://www.google.com/url?sa=t&source=web&rct=j&...
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Bottom line, try adding, for example, KNO3 ([Edit] better KNO3 plus sea salt or employ NaNO3/NaBr for more efficiency, see http://pubs.acs.org/doi/abs/10.1021/jp109560j?src=recsys&... ) to very cold H2SO3 and aerate in sunlight.
[Edited on 21-1-2016 by AJKOER]
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