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Author: Subject: Activated manganese dioxide from batteries?
Smoker Root
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[*] posted on 12-10-2019 at 00:13
Activated manganese dioxide from batteries?


Hi, I have extracted some manfanese dioxide from bateries just for the lulz. I don't have a main use for this compound alone, but I have a job for is activated form(benzyl alcohol oxidation) The problem is that to make it I need potasium permanganate whuch for me is impossible to find(I know the peoplenof USA is easy to get it, but not in my country as it is seen as a drug precursor) So I looked for another method.

I looked to two papers but could read neither of them. One that shows how to make it from activated carbon and by the azeotropic removal of water. This last one is the one that interests me the most, since it can be theoritically be done easily. Anyone has experience with this procedure? Can you give me a write up? And if not another available method?

Thank you all
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j_sum1
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[*] posted on 12-10-2019 at 00:53


To my knowledge, KMnO4 has proved very challenging for the amateur to make and even more to purify. Even chemplayer gave up on that one.


Did you remove the C from the battery paste? This accounts for about 30% of the mass.
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Smoker Root
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[*] posted on 12-10-2019 at 01:18


Quote: Originally posted by j_sum1  
To my knowledge, KMnO4 has proved very challenging for the amateur to make and even more to purify. Even chemplayer gave up on that one.


Did you remove the C from the battery paste? This accounts for about 30% of the mass.


Yeah, I have the pure manganese dioxide
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Corrosive Joeseph
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[*] posted on 12-10-2019 at 04:08


Never done it but it's on my bucket list......


Quote:


It is worthy of note that the percentage water content strongly influences both the oxidizing power and the selectivity (oxidation of multifunctional molecules) of active MnO2.

Thus it is well known that the wet material (40–60% H2O) obtained after filtration must be activated by drying (heating to 100–130 ◦C for 12–24 hours or, better at 125 C for 52 hours ).

Indeed, an excess of water decreases the oxidation power since, according tthe triphasic mechanism generally postulated it would prevent the adsorption of the substrate to the oxidatively active polar site on the surface of MnO2.
On the other hand, it is very important not to go past the point of complete activation since the presence of hydrated MnO2 species is essential to obtain an active reagent. For this reason, the drying conditions must be carefully controlled. Alternatively, the wet material can be activated by azeotropic distillation since this mild procedure preserves the active hydrated species. Thus azeotropic distillation has been used to remove the water produced during the oxidation reaction to follow the rate of MnO2 oxidations.




https://sci-hub.tw/10.1002/047084289X.rm021.pub4


/CJ




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[*] posted on 12-10-2019 at 04:51


i made pure MnO2 from USED D size batterys by heating them 250C to remove water and NH4Cl.the residue is carbon Mn2O3.then washed it and heat it to 750C to remove C and reduse Mn2O3 to MnO (carbon in side the battery will act as a reducing agent).after adding NaOH and heating to boil to dissolve ZnO to sodium zincate https://en.wikipedia.org/wiki/Sodium_zincate
and filtering out greenish brown solid.adding a strong magnet can remove some iron impurity as Fe2O3.keep the zinc filtrate to make ZnO by leaving to air to absorb CO2.
now you have two options.
add H2SO4 to make MnSO4 and filter it.
add NaOH and NaOCl to get MnO2. MnO+NaOCl -------->NaCl +MnO2
if you add NaOCl to MnSO4 chlorine will form a poison gas. MnSO4 +2NaOCl ------>Cl2+ Na2SO4 +MnO2

[Edited on 13-10-2019 by rockyit98]




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[*] posted on 12-10-2019 at 14:16


Quote: Originally posted by rockyit98  
i made pure MnO2 from USED D size batterys by heating them 250C to remove water and NH4Cl.the residue is carbon Mn2O3.then washed it and heat it to 750C to remove C and reduse Mn2O3 to MnO (carbon in side the battery will act as a reducing agent).after adding NaOH and heating to boil to dissolve ZnO to sodium zincate https://en.wikipedia.org/wiki/Sodium_zincate
and filtering out greenish brown solid.adding a strong magnet can remove some iron impurity as Fe2O3.keep the zinc filtrate to make ZnO by leaving to air to absorb CO2.
now you have two options.
add H2SO4 to make MnSO4 and filter it.
add NaOH and NaOCl to get MnO2. MnO+NaOCl -------->NaCl +MnO2
if you add NaOCl to MnSO4 chlorine will form a poison gas. MnSO4 +2NaOCl ------>Cl2+ Na2SO4


Well this is a game changer. This is a much complex purification technique. We can defenitley see how good you take in too deatil the purity of your precursors. I will maybe try this since it is nearly full OTC. Thabks a lot for this. Have you tried activating it?
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[*] posted on 12-10-2019 at 14:31


Quote: Originally posted by j_sum1  
To my knowledge, KMnO4 has proved very challenging for the amateur to make and even more to purify. Even chemplayer gave up on that one.


I recommend chlorate as the oxidant, for small amounts, but IDK what would happen if graphite was present. With whichever method of arriving at manganate, in practice it looks like more of a KMnO4 failure than it is, because of the MnO2 formed in the process and maybe lots of graphite floating around too.

Quote: Originally posted by Smoker Root  
Yeah, I have the pure manganese dioxide


How, exactly? Have you tested to see if it is already activated? Maybe all it needs is a wash, maybe a reflux with dilute nitric acid, even with graphite.




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rockyit98
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[*] posted on 12-10-2019 at 16:53


how to make calcium permanganate. haven't tried but
4MnO2 + 2Ca(OH)2+3Ca(OCl)2 -------->2Ca(MnO4)2+3CaCl2+2H2O
https://en.wikipedia.org/wiki/Calcium_permanganate




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[*] posted on 13-10-2019 at 03:10


An earlyIndustrial Methode was boiling MnO2 in 50% KOH to drynes and bubbling air throught the KOH solution. Then outwashing the K2MnO4 and later Reakt with CO2 to KMnO4 and K2CO3.
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[*] posted on 13-10-2019 at 19:45


Quote: Originally posted by rockyit98  
i made pure MnO2 from USED D size batterys


KMnO4 can probably be made just as easily (especially from alkalines) after burning off the graphite, via conversion to K manganate then CO2 to 1 mol. MnO2 and 2 mol. KMnO4. Another option besides KMnO4 reagent is conversion to a Mn salt that gives active MnO2 after heating, perhaps with a little minor further treatment.

Quote: Originally posted by Alkoholvergiftung  
An earlyIndustrial Methode was boiling MnO2 in 50% KOH to drynes and bubbling air throught the KOH solution.


This may still be going on, but is best done under pressure within a narrow (hot) temperature and KOH range. Both air and nitrate are less easy to manage at home than chlorate, since the chlorate is providing pure oxygen intimately at the right temperature; it's so much faster. Air roasts in a simple way is possible, but the yield is not good IME and you have to know Mn chemistry or learn the hard and messy way.




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[*] posted on 16-10-2019 at 13:56


Speaking of knowing your Mn chemistry, I'm not sure that NaOH isn't detrimental in this case. My (per)manganate from refined battery crud experiments years ago were probably all done using a mix of KOH and NaOH from a conc. aq. drain cleaner, rather than KOH flake. On the stovetop. It's no surprise my air roast yields were not worthwhile. Maybe manganate is easy, but my guess is still not.

PS Forms of Mn other than MnO2 are easier to convert to permanganate from air roasting, with either NaOH or KOH.

[Edited on 16-10-2019 by S.C. Wack]




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[*] posted on 16-10-2019 at 22:26


Thats why they used MnO made from the Weldon mud for Manganate Production. The MnO2 from old Batteries should mostly reduced to MnO. Treated with oxalic Acid should reduce the rest of it.
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