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anti
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mad.gif posted on 17-2-2020 at 00:45
Sodium permanganate


Hello! So, I've been trying to acquire some potassium permanganate for the last week or so. Apparently, in my country, it is HIGHLY ILLEGAL. I also don't have any access to acids, which I learned the hard way( I made my own acids a while back but now I'm out and I will restart production soon).
The thing is that I have access to sodium hydroxide.
So I tried to make some sodium permanganate, by reacting molten NaOH with NaClO3 and MnO2. But the manganate proved to be highly unstable, so it's not feasible.
I am really desperate. But I have heard that there's another way that could work: electrolysis with manganese metal electrodes. link
I've got some MnO2 from batteries(purified) lying around. But no aluminium powder nor the tools to make some, but I could make a ball mill. So then I would make thermite and somehow light it without magnesium(don't have;no access).
Then I would do the electrolysis.

Do you think it could work? I can't seem to find manganese metal for sale, and international shipping is not an option.
I would only need a few grams of Mn, that I would forge into a rod or something. Do the electrolysis, and harvest the permanganate.


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[*] posted on 17-2-2020 at 01:24


What is so important that you need permanganate......? Is there another reagent that can do the job you want it to......?
For some of the reasons you have mentioned, I have long ago given up on obtaining this oxidant and would choose a different one.


/CJ




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[*] posted on 17-2-2020 at 06:06


you can make calcium permanganate instead which is stable .
https://www.sciencemadness.org/whisper/viewthread.php?tid=15...

Ca(OCl)2+ 2Ca(OH)2+2MnO2 ----(heat)---->2CaMnO4 +CaCl2 +2H2O

3CaMnO4 + 2CO2 ---------->Ca(MnO4)2 + MnO2 +2CaCO3




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[*] posted on 17-2-2020 at 12:35


Maybe you can buy small amount like 20 g of KMnO4 in pharmacy. It is used to treat mycotic infections of feet. We used it also to treat scabies but that was very long ago, while servicing my basic military training (3 days of powdered sulphur in ointment and the fourth day a bath in very diluted KMnO4) - today there are better things with faster effect but also more expensive.



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thumbup.gif posted on 17-2-2020 at 23:00
Thanks for all the replies.



@Fery I found it in a pharmacy as pills... But it's prescription only!
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[*] posted on 18-2-2020 at 01:01


From your reaction with NaOH, NaClO3 and MnO2 you obtained sodium manganate. This compound can be converted in to permanganate by electrolysis or by adding acid in to it (vinegar is sufficient for this purpose).
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[*] posted on 18-2-2020 at 02:49


anti - what's a pity, here you could just enter the pharmacy and tell something like: I have a mycotic infection of feet, I don't want to take off shoes either socks here because of distinct terrible stink, I had the same problem some time ago and permanganate bath helped...
so synthesis seems to be your only way to go, among all methods mentioned here, there is also an electrolytical method




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[*] posted on 18-2-2020 at 03:10


Quote: Originally posted by Bedlasky  
From your reaction with NaOH, NaClO3 and MnO2 you obtained sodium manganate. This compound can be converted in to permanganate by electrolysis or by adding acid in to it (vinegar is sufficient for this purpose).

I did it. Didn't work.( The manganate just converted to manganese dioxide on contact with water)
On the info page, it's written that sodium permanganate cannot be produced that way. Also, I don't want to have to deal with any more melting, because I'm using my gas stove, and it doesn't burn very hot.
Electrolysis seems very appealing.
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[*] posted on 18-2-2020 at 03:21


Quote: Originally posted by Fery  
anti - what's a pity, here you could just enter the pharmacy and tell something like: I have a mycotic infection of feet, I don't want to take off shoes either socks here because of distinct terrible stink, I had the same problem some time ago and permanganate bath helped...
so synthesis seems to be your only way to go, among all methods mentioned here, there is also an electrolytical method

But that's what I suggested in the first place!
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[*] posted on 20-3-2020 at 06:59
UPDATE #1


OK, so apparently, you can own up to 50g legally, but it is illegal to sell in the country.

I found a source on Amazon. BUT NOW IT'S BECOME A PERSONAL MATTER!If the money does allow it, I won't give up until i come up with a working preparation that will suit ANYBODY who wants this AMAZING REAGENT.


PS0. THIS CORONAVIRUS THING IS REALLY GETTING ON MY NERVES!!!!!!!! I hope they won't close down the reagent store. It is really nice. They have: 3 types of iron oxides, green and yellow chromium oxide,titanium and zinc dioxide, nickel oxides, [ sadly no manganese oxides :( ] calcium hypochlorite(1dollar/500g bag),sodium hypochlorite, acetone, trisodic phosphate,sodium hydroxide, calcium oxide, and a few other less useful things. Also, metal pipes, and appliances, and some misc. stuff.


PS1. F*** methcathinone! The internet "cooks" chose KMnO4 as oxidiser (that is not the point), why did the govt. ban the permanganate?? You can easily substitute the permanganate (for the dehydrogenation of a certain cold medicine) with a carcinogenic chromium-based reagent that i won't name). THEY WANT PEOPLE TO FREAKING GET CANCER!!!(this is a moral issue. Catch the druggies, lock 'em up, then, when they get out, cancer comes knocking on the door and they die, OR they still live after they've paid the price for their activity.) This is OUTRAGEOUS.
Drugs are the reason home chemistry is becoming INCREASINGLY INACCESSIBLE.



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[Edited on 20-3-2020 by anti]
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[*] posted on 24-3-2020 at 09:32


What is the decomposition temperature of calcium hypochlorite? One of the permanganate preparations describes heating up a solution consisting of a hypochlorite, an alkali and suspended MnO2. Sodium hypochlorite disproportionates at those temperatures, so the yield of permanganate is VERY LOW.
My experiments with that produced no more than a sad and very very pale violet colored solution. The yeild is probably less than 0.0001%.
The question is : will Ca(OCl)2 disproportionate into chlorate upon heating in solution?
Using calcium hypochlorite to oxidise MnO2 is described in a lot of places, but nobody does it.

The method that i'm chasing after is electrolytic oxidation of manganese metal .I've been trying to acquire ferromanganese for the past month or so, but the shitty companies in my country won't sell the stuff in kilogram quantities. Also i don't have access to Al powder for thermite, and the MnO2 i get is from batteries.




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[*] posted on 24-3-2020 at 16:05


Quote:
The question is : will Ca(OCl)2 disproportionate into chlorate upon heating in solution?


Yes, it will.

What country are you in?




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[*] posted on 25-3-2020 at 02:20


Quote: Originally posted by phlogiston  
Quote:
The question is : will Ca(OCl)2 disproportionate into chlorate upon heating in solution?


Yes, it will.
so, the yeild will not be improved
What country are you in?
I live in Romania


The only methods that ought to work on a small scale would be diaphragm electrolysis with manganese anode(7 Faradays of electricity per mol, so really slow but efficient), oxidation of boiling concentrated alkali manganese dioxide suspension with chlorine gas ( I would rather NOT! Thanks.), and some ideas that I thought up, like putting some manganese dioxide into a chlorate kind of cell, maybe that would work, because of the hydroxide , chlorine, and ultimately hypochlorite production, so there would be multiple mechanisms of action that could theoretically produce the desired compound.

Another thing that I thought up and found some literature on is direct oxidation of manganese dioxide suspension via electrolysis.( I originally considered putting some dioxide in a filter paper and wrapping that on the electrode, but that won't work). I found a thread here,but the guy wasn't able to do it, so I won't consider doing it.

The roasting really did not work out for me. I tried it again , but instead of using an oxidiser, I tried to use air,and instead of mixing the powders, I dropped some MnO2 directly into some molten NaOH, and it did not work.

Not even the slightest color change.
I guess you really need to do it at a large scale to get a good yield.
Wikipedia:" It can be also prepared by reacting manganese dioxide with a solution of calcium hypochlorite and a little bit of calcium hydroxide to increase the pH level. "
That's dissapointing. But why does it not mention the low yield?
I guess Wikipedia is not being administered closely enough.




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[*] posted on 25-3-2020 at 08:38


Oh no, is this another "I'd rather fuck around in the lab for three years rather than spend an hour at the hardware store finding potassium" thread?

Seriously people, potassium is not. that. hard. Just buy potassium. For fuck's sake. Ceci n'est pas une pipe dream. The last time someone claimed that potassium wasn't available in his country I linked to a page from his government about where to get high-potassium fertilizer and he stopped replying. There is potassium available near you. I guarantee it.

Look, if you're so convinced that KGB agents will burst out of the wall and carry you off in a helicopter if you so much as glance at a canister of Lite Salt, you can probably do it with ozone, Mn (II) sulfate and sodium sulfate:

12 Na2SO4 + 6 MnSO4 + 5 O3 + 9 H2O >> 6 NaMnO4 + 18 NaHSO4

as described here:

https://www.researchgate.net/publication/41196895_Permangana...

"In neutral solution, the main product is MnO2 and only 10% MnO4- are formed even at high ozone excess. In acid solution, however, or in neutral solution when Mn2+ is complexed by polyphosphate, oxalate, sulfate, bicarbonate or phosphate, the reaction proceeds to MnO4- in an up to 100% yield."

...or, you can go to the store and buy a salt replacement formulated for people with hypertension, or you can buy high-potassium fertilizer for growing tomatoes, or you can order potassium cocoate by the pound from soapmakers, or you can just. fucking. try. for. more. than. three. seconds.

edit: fixed equation stoichiometry

[Edited on 25-3-2020 by clearly_not_atara]




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 25-3-2020 at 11:37


Quote: Originally posted by clearly_not_atara  
Oh no, is this another "I'd rather fuck around in the lab for three years rather than spend an hour at the hardware store finding potassium" thread?

Seriously people, potassium is not. that. hard. Just buy potassium. For fuck's sake. Ceci n'est pas une pipe dream. The last time someone claimed that potassium wasn't available in his country I linked to a page from his government about where to get high-potassium fertilizer and he stopped replying. There is potassium available near you. I guarantee it.

Look, if you're so convinced that KGB agents will burst out of the wall and carry you off in a helicopter if you so much as glance at a canister of Lite Salt, you can probably do it with ozone, Mn (II) sulfate and sodium sulfate:

12 Na2SO4 + 6 MnSO4 + 5 O3 + 9 H2O >> 6 NaMnO4 + 18 NaHSO4

as described here:

https://www.researchgate.net/publication/41196895_Permangana...

"In neutral solution, the main product is MnO2 and only 10% MnO4- are formed even at high ozone excess. In acid solution, however, or in neutral solution when Mn2+ is complexed by polyphosphate, oxalate, sulfate, bicarbonate or phosphate, the reaction proceeds to MnO4- in an up to 100% yield."

...or, you can go to the store and buy a salt replacement formulated for people with hypertension, or you can buy high-potassium fertilizer for growing tomatoes, or you can order potassium cocoate by the pound from soapmakers, or you can just. fucking. try. for. more. than. three. seconds.

edit: fixed equation stoichiometry

[Edited on 25-3-2020 by clearly_not_atara]

What the actual FREAK are you talking ABOUT? Have you read the thread??????? This is NOT ABOUT POTASSIUM. This is about the f****** YIELD!! Just a sec, i'll get out my 1000MV power supply and huff some of that nice ozone!
What am i even doing... It would be easier to burn down the lab and go home.
HAVE A NICE DAY




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[*] posted on 25-3-2020 at 11:50


You are trying to make permanganate. The correct way is to use potassium manganate. You are resisting this easy solution for (?????). This is absolutely about your unwillingness to do things the easy way.

Plenty of people here have worked with ozone, here are some links:

http://www.sciencemadness.org/talk/viewthread.php?tid=62229
http://www.sciencemadness.org/talk/viewthread.php?tid=1774

edit: and if you absolutely must have sodium permanganate for some ridiculous reason, you can always do salt metathesis KMnO4 + NaClO4

[Edited on 25-3-2020 by clearly_not_atara]




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 25-3-2020 at 13:19


Quote: Originally posted by clearly_not_atara  
You are trying to make permanganate. The correct way is to use potassium manganate. You are resisting this easy solution for (?????). This is absolutely about your unwillingness to do things the easy way.

Plenty of people here have worked with ozone, here are some links:

http://www.sciencemadness.org/talk/viewthread.php?tid=62229
http://www.sciencemadness.org/talk/viewthread.php?tid=1774

edit: and if you absolutely must have sodium permanganate for some ridiculous reason, you can always do salt metathesis KMnO4 + NaClO4

[Edited on 25-3-2020 by clearly_not_atara]

tens of grams of ozone??
Gosh.
So here is a summary:
-No pure MnO2 available, only battery grade
-No OTC oxidisers, but i made some KNO3 from some ammonium nitrate that i LITERALLY found in the trash
-Sale of permanganates is illegal
-Noone successfully got a good yield out of the classic manganate method(on a small scale).
-No ozone (?)
-NO OTC ACID
-NO OTC ANYTHING USEFUL
-NO OTC MANGANESE COMPOUNDS
Please enlighten me! How would one go about getting a good yield out of a messy procedure, when chemists like NurdRage, Chemplayer, etc. failed to.
This is common sense. I don't even have glassware,tho that wouldn't make any difference.
You.Just.Can't.Understand that my country really hates anything that is related to exact science.

I've come to the conclusion that it is my fault for trying to do chemistry out of a literal shithole.

Enjoy what you have, clearly_not_atara.
BE GRATEFUL! I SAY!
Let my pain be a lesson to you all!

I'll just quit while i'm ahead, thanks.




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[*] posted on 26-3-2020 at 10:41


UTFSE

https://www.sciencemadness.org/whisper/viewthread.php?tid=84...

Sodium permanganate is highly unstable. Trying to prepare and isolate the sodium salt when you failed with the potassium salt is like having trouble baking bread and switching to croissants.

If you're having trouble getting KOH from K salts, I suggest the following double metathesis:

NaOH + CaCl2 >> NaCl + Ca(OH)2 (precip)

Ca(OH)2 + K2CO3 (aq) >> CaCO3 + KOH

To prepare manganese metal, some people like thermite methods, but I think reducing an Mn(2+) salt in solution makes more sense.

[Edited on 26-3-2020 by clearly_not_atara]




[Edited on 04-20-1969 by clearly_not_atara]
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