Lab notes - Making Potassium Permanganate
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- Опубликовано: 14 сен 2023
- My lab notes of making potassium permanganate.
First i tried reacting manganese hydroxide, potassium chlorate and potassium hydroxide by mixing them together and heating to 300 celsius. I got green stuff that i think was potassium manganate so i oxidized it further to permanganate using chlorine gas. It turned the proper purple color but when i crystallized it the result was crystals of potassium chlorate with a little permanganate mixed in.
So that was failure and i repeated the experiment again at 400 celsius thinking i just needed more heat. But it still failed and produced only small quantites of permanganate.
So i thought maybe using manganese hydroxide was wrong. I repeated the experiment but using manganese dioxide this time. I produced a much more intense color of green manganate and purple permanganate and when i crystalized it i produced the proper black crystals of potassium permanganate. To make certain it was correct, i titrated using sodium oxalate and confirmed that i had a redox active substance that assayed to 99% purity. The yield was 15.4g or about 19%.
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You don't need to heat it for several hours like i did. Other amateurs have told me they just needed to use a torch and heat it to red hot for ten minutes. Anyway, i'm still working on it, i have a proper procedure video in a few weeks.
Could you make a video on the Diels-Alder reaction?
Diels alder is pretty simple to understand its just finding practical synthesis that use it that is tricky. At least things that would be useful and accessible o the amateur.@@stick-Iink
Hey, I made a comment under the chlorate video but you didn't notice:
Personally, I would cover the main reaction beaker, the reaction is driven by high temperature, not by evaporation and in my experience,
when heating open beakers on weak (100-300 W) hotplates the temperature can be as low as 80 C, and that 20 degree difference can slow down the reaction a lot.
What is the wattage of your heating element?
Actually, chlorinated lime would be a more economical source of hypochlorite, but dirtier.
Weiridly, potassium nitrate is easier to get here than potassium chloride, how can it be used?
KNO3 is less soluble at low temps than KCl, this can be a problem.
Myself, I bought KClO3/4 just before it got regulated, I'm more interested in sodium salts, they are more useful for synthesis (iodates, ClO2, etc.).
Get rid of the kcl please.
i really enjoy that you also ahow us the failures and experimental road blocks. this tells us about the proccess even more than successes do. you walk us through your thought proccess, and i cant tell you how valuable that is to me.
These lab notes are wonderful. Failure or success, it's all the chemistry we adore this channel for ❤
Indeed, trial and error is the best teacher, ;)
Yea!
It's important ton understand that chemistry is MOSTLY failure. :')
If something is learned from 'failures' in chemistry syntheses, then those 'failures' are worthwhile failures.
Exactly.
@@ZoonCrypticon Lunche cu cu tancott sok tu
Food grade manganese dioxide is available as water filter media. Brand names Pro-OX, Filox, MangOX, Terminox, Catalox, and Pyrolox (brands are all minimum of 75% manganese dioxide).
It's relatively easy to produce reasonably pure manganese dioxide from discharged dry cells; dissolving the black paste in HCL for several days until chlorine is no longer evolving then filter the solution. Add the solution to 200g NaOH dissolved in 1l regular bleach and you get a reasonably pure MnO2 precipitate. Just be aware that the filtrate destroys filter paper, so use a frit filter funnel.
So glad to see you back making videos. You were missed!
he (or she!) has made a few vids lately. update your subscriber settings to "all" --from "personalised" :)
There's a bunch of new chem RUclipsrs, it's a renascence of home chemists. :)
@@BillAnt True, but NurdRage is in a class all his own.
@@guardduvie- I come here for the great reactions, and leave with euphoria. ;) (if you know what I mean heh)
00:51 Attempt 1 (Failed):
00:55 MnSO4 to Mn(OH)2
01:32 Add oxidant KClO3
01:50 Stabilize with KOH
02:26 React in metal container at 300 C
03:45 Re-React with Cl2 oxidant
06:14 Attempt 2 (Failed):
06:22 Repeat attempt 1 with a higher reaction temperature of 400 C
07:07 Attempt 3 (20% yield - limited success):
07:11 MnO2 + KClOc + KOH at 400 C
07:28 Re-React with Cl2 oxidant
07:56 Raw product tested
08:33 Oxalate titration - 99% +- 3% purity
I wonder if one could effectively decompose Mn(OH)2 using the furnace and a nitrogen bottle?
you wont need nitrogen to decompose Mn(OH)2 literally you want oxygen to oxidize it to +4 state and I can imagine building a fluidized bed hot air reactor to do so but thats not amateur chem and infact thats how permanganate is made industrially they use a mix of KOH and MnO2 or Mn(OH)2 and fluidize hot air through it to produce manganate.
@@CatboyChemicalSocietythank you. I am not an expert at all.
You keep my passion for chemistry alive and kicking, NurdRage! I have used your channel to make all sorts of things over the years, and I have enjoyed every single minute. Keep doing what you are doing.
That's interesting, you're the first person I've seen successfully producing usable quantities of permanganate, and the procedure isn't even difficult.
Glad to see you again Dr Lithium.
It's cool to still see you around after all this time. Been following you for so long now, it's wild to see the world change so.
I appreciate you being thorough and showing the avenues that don't end up panning out. I frequently find myself watching chemical recipes and wondering "But, what if I..." and it's great to get an answer if it's out there. "But what if I..?" ... "Then you get a big pile of poo in your filter papers "
Maybe I didn't look hard enough, but this is the first video I've seen of a fairly successful synthesis of potassium permanganate. All the previous attempts were complete failures with either zero or close to it produced, so seeing a fairly simple procedure with even a 19% yield is really exciting. Love seeing your meticulous work, between your painstaking development of a repeatable and high-yield way of obtaining sodium metal to the many paths to sulfuric acid, you've done so much towards helping out amateur chemistry!
Thanks for keeping this Channel active and posting these videos for us 🙏
Thank you so much for also including videos of your failures! It's really amazing seeing the thoughts and process, regardless of if it turned out to be a success or failure!
Potassium permanganate is such a useful chemical, whether for cleaning water for drinking, soaking fungal-infected feet to heal them, or just being a show-off and lighting fires with glycerine, I have a jar of the stuff I bought some years back and it lasts for ages cos you need so little to use it... :)
Thank you Dr N. Butyl Lithium and co for another interesting video. :)
There is one source of contamination that bugs me a little:
Aluminium cans have a plastic coating inside. After you heated the can at 300C, we could see some of the plastic was burnt.
To avoid any contamination, I would be tempted to heat the can, to burn off all the plastic and wash the can before using it in the experiment.
Keep in mind as well though, that was a steel can, not aluminium. But you are correct it would be best to either burn off or remove the plastic with dcm or another harsh solvent and then clean very well
@@In_the_shed I expect he's working with such a contaminated starting point, that a few organics will not be an issue at that stage.
@@jamesnomos8472 With that in consideration, it's remarkable that he was able to isolate 99% pure KMnO4 from such contaminated starting materials.
thats why you recrystallize with water.
@@jamesnomos8472 It is not as though the MnO2 offered by pottery suppliers is analytical grade!
I love seeing the journey from hypothesised procedure through failure and procedure redisign to hopefully success.
Nice to see you. Can't say how many of your techniques I've used over the years. Always great to watch your work.
Ohh myy.. The king has returned 🥹
he (or she!) has made a few vids lately. update your subscriber settings to "all" --from "personalised" :)
For anyone who's looking to get it and just doesn't know where, its usually sold as "Pot Perm Plus" as a regenerant for an iron filter called "manganese greensand".
You may be able to use the "manganese greensand" itself (which is pretty cheap(ish)) as a source of potassium manganate as it has a warning that exposure to chlorine will produce potassium permanganate.
I still don't know if this is used for tap water filtration or fish tanks or pools or planting soil or what.
Also known as condy's crystals, check your local pharmacy
I think the Pot Perm Plus stuff is used for filtering well water for tap use. The iron filter would reduce iron oxide for better flavor/less rust stains in sinks and tubs.
Not sure if this is useful to people as well, but potassium permanganate is also used in aquarium keeping to treat some fish illnesses and parasites.
@@lancer2204 Are you from the US? I've never seen it in any pharmacy near here. I know Canadian apothecaries/pharmacies carry a ton of things that are just plain illegal to sell in the US.
It looks like there are a lot of Darwin award candidates drinking it as part of "detox" programs. I guess I shouldn't be surprised.
Love seeing you back on youtube!
failures are tremendous learning experiences! Thanks for this video!
Your channel continues to be a blessing.
Love how you also show the fails!
banger video
Feels so good to see you back.
Cool! I’ve wanted a procedure for this for years.
Here in Florida, most grocery stores sell potassium permanganate as a pool chemical and it’s not especially expensive. The thought of making it doesn’t even cross one’s mind!
the difference between 1st and 3rd worlds i guess.
Great lab notes, NurdRage. Thank you. I'm looking forward to your followup and progress in the future!
Always impressive work. Thank you for sharing this...
it is great to see your work
FUN FACT: A lot of perchlorate and permanganate salts are isomorphic, they can form solid solutions so any recipe that mixes the two will have some very difficult to remove impurities.
Great video per usual and thank you for including some "gotcha's" you experienced!
Ohh hell yeah!!!! Finally and for first time in RUclips a synthesis of potassium permanganate that really works, only nurdrage can make it happen!!!!
Long time no see ! good to hear back from you.
Completely awesome. Even without improvement this will give a lot of hobby chemists a means to do things they were finding impossible.
Wow those acicular crystals you finally arrived at are beautiful! Reminds me of the manganese minerals that grow in the caves and abandoned mines here in Colorado 🥰
Really great video, thanks.
Outstanding!!
Excellent video thanks!
WOW!! Great stuff!! Thank you!
Great to see your return! I didn’t understand the oxidation via chlorination .
OIL RIG: Oxidation Is loss, Reduction Is Gain(of electrons). That's all.
...LOVE these videos!
TY
2 videos in 1 week?! You're spoiling us sir! ;P Would love to see another long-form video series like you did with the Advil to Tylenol, but I'm glad you're back in the lab :D
nurdrage never did anything with advil and tylenol, you must be confusing them with someone else.
Great for cleaning up CS2 .
Well done!
Potassium permanganate is used here in the UK as a pond treatment for koi and quite easy to get from koi specialist shops and Web sites.
Thank you for including your failures, a lot of chemistry channels makes it look way to simple.
Well done.
the lean crystals from the first attempt are beautiful
Nurd!! Great video!
My favourite compound. :)
My favourite video remixed. :)
Greetings, Not to take anything away from the enjoyment of making this, but I bought a 4.75 pound bottle of this at Menards a few days ago. It was with the water softeners and is used to regernerate iron-romoval media. I think it was about 35 USD. Convenient, but not as educational as DIY. Thanks for another great video.
Happy place
THE RETURN OF THE KING
Pottery supply sounds like a good way to get all sorts of oxides, any metal ion with a strong characteristic color could be there
I feel like manganese dioxide is the easiest form to get. Not only can you buy it online, but it is a thermodynamic sink. So this is a great method!
in our qualitative analysis lab I had some manganese salt in my substance and I used a small ceramic cup in which i put the Mn(IV) salt and 3-6 times as much of an equal parts mixture of Na2CO3+KNO3. this mixture was ground to a fine powder and molten to a red color until no more gas was escaping. In the end it was the most intense green with no discoloration, although it could sometimes be rather blue if it didn't oxidise all the way to MN(VI) but MN(V).
Very interesting
MMMMMMMMMM. POTASSIUM CHLORATE. Such FUN!!!!!
Over the years I've gotten used to NurRage pronouncing _"sodium hydroxide"_ in 3 syllables. I now accept it as an endearing quirk.
im.. not sure what you're talking about.
@@dimitar4y "40 grams of sum hrxd in water" 1:02
Chloride ion tends to reduce permanganate down. I'm surprised it worked at all. Very interesting.
The Rage is back in the Nerd, oh yeah! :D
Interestingly back in the 80's in Eastern Block countries, permanganate powder was sold at pharmacies as a disinfectant anyone could buy (not sure nowadays).
Still avalaible in pharamacies in Bulgaria...
still available in Belarus
@@antejl7925- Used to buy it in Romania, it was called "Hyper-Mangan". heh
This has been widely available in the late soviet union.
My dad used it to purify the 50% alcohol distillate he got from leftover wine production (yes we grew grapes too).
It reacted with impurities and settled as black flakes.
cooking gas was also not metered so he ran his distillery at no additional cost.
According to him this prevented or significantly reduced hangover.
To the leftover drink he added oak wood for a year or two to make it into cognac.
In our lab, in the past, this reaction was done a bit differently. First, it was mixed in a steel crucible the manganese dioxide, potassium chlorate and potassium hydroxide. Then, the crucible was put on a Bunsen burner till it was obtained a black liquid (approx 5-10 min) and everything was poured instantly into boiling distilled water. The mixture was filtered after cooling and carbon dioxide was bubbled till the solution became purple. Black crystals were obtained after cooling. A notable difference from the video is the temperature and the quantity of KOH. If you add more the reaction mass will melt faster. For an amateur, this reaction can be done on a stove. I do not recommend doing it because it is dangerous.
That moment in chemistry when even failures are beautiful.
Great practical demonstration, as usual.
But will you do a live with Peter & Pete ? You will only advance the craft.
Yes much to be discovered and discussed!
Hi! I have a suggestion regarding the carbon contamination from MnO2 obtained from batteries. You could try igniting a mixture of MnO2/C + KNO3/KClO3 + NH4NO3 to "burn off" most of the carbon where the quantity of ammonium nitrate used instead of KNO3/KClO3 controls the rate of reaction (burn rate). The "ash" from this reaction can be placed inside the furnace as usual with KClO3/KOH where excess ammonium nitrate will decompose into gasses and leave the iron pot.
Edit: According to Wikipedia KNO3 serves the same purpose as KClO3 of oxidizing the manganese dioxide when heated in a furnace.
You can make some fairly reactive MnO2 by dripping a solution of manganese salts into sodium hypochlorite with sodium/potassium hydroxide to limit chlorine generation, theoretically you could make manganates and permanganates that way, with an entirely wet processs.
Also, it would be very nice to see a video on making BaMnO4 from KMnO4, It's supposed to convert to manganate and oxygen on heating in a strongly basic solution but it didn't work for me, and adding a reducing agent reduces it to MnO2.
Aside from being an organic chemistry oxidant, a solid solution BaMnO4 and BaSO4 is a really pretty pigment.
A fantastic video ! Thank you very much ! A question: could you do the process in a electrochemical way ? Such as using e.g. two platinated electrodes, which on one of the sides would be surrounded by compressed MnO2 (with a textile cover sheet) as the positive electrode, and KOHaq as solvent ? Unfortunately MnO2 has a very low conductivity of about 10e-06 S/cm. On the other hand I found a patent from 1997 "ELECTROLYTIC PRODUCTION OF POTASSIUMPERMANGANATE USING A CATIONIC MEMBRANE IN AN ELECTROLYTC CELL "
Всем привет! Большое спасибо за данное видео!
There is a thin plastic layer on the inside of food cans like the one you used to cook heat it in, I'm no chemist but would a better clean metal container be offer better results?
We must be approaching end times with all these Nurd Rage videos
what the fuck
well, i remember in old chemistry book they used CO2 to oxidize it further into KMnO4
maybe take a sample from the reaction mixture once every 20 minutes and continue running for 4 hours to see if theres a certain sweetspot, then try adjusting temperature and sample it again
im very surprised this works at all, ive tried and i did get some spikes once but, it was more so proof of concept than anything, i didnt use chlorine to oxidize however, we must find alternative to chlorine. very impressed that theres an actual yield, this is one of very few if any successes we have of amateur chemists with permanganate. we just found a working recipe for nitrite as well lately
Cool!
I've use many kilos of potassium permanganate in water conditioning and it's dark purple granules, what am I missing? Also you can get it at any water shop in 2 kilo jars, it's the regenerant for green sand filters.
Is this one of those things where you can reduce the temperatures needed by running the process in an "inert" solvent?
Above 400°C, both potassium nitrate and potassium hydroxide are liquid. This liquid phase can oxidize manganese dioxide efficiently. You can try in a test tube placed above a Bunzen burner. There is plenty of manganese dioxide in cylindrical alcaline batteries.
If you're having problems buying this, check at a chemist/drugstore and ask for "condy's crystals" 👍
Great video, I always wondered can this stuff be made at home. Now I know 😄 thanks NR
I'd like to see a run using straight battery sludge as the manganese dioxide source, IIRC the carbon in the sludge is just graphite (it's for carrying current, not being an active reagent) so it shouldn't cause any reducing at the temps you need for this reaction. If it doesn't cause issues then battery sludge can be used as-is, possibly even DEAD batteries could work although you might need more chlorate, cause graphite's functionally inert and can just be filtered off with the rest of the waste slurry.
Great lab note. While KClO3 is much more difficult to get than KMnO4, this lab note shows how to refresh old KMnO4 that degraded over time partly to K2MnO4. I looked to get Teflon membranes for electrolysis, but chlorine gas is easier available.
I'm just not so sure what happens to the MnO2 that is also present in degraded KMnO4.
You can get it most places and online , by the pound , for regenerating greensand filters .
I'm still watching for how you optimize your yields , tho .
Any plans to go for for Potassium metal as a follow up to your epic sodium metal series ?
Just curious, I’ve heard that barium salts can be used to precipitate barium permanganate. You can then treat with dilute sulfuric acid to precipitate barium sulfate and a solution of permanganic acid. You can then use any alkali carbonate to neutralize the permanganic acid and end up with the alkali permanganate. I know that barium is exotic and I don’t know if it can be easily recycled once it reaches the sulfate, but that was one way I thought of to make sure you’re getting all the permanganate out of a raw reaction mix
Nice! I think there are even easier solid state methods for making alkali-manganates 😉
Missed you!! Btw, you might like the new rage ( just for the science ) of the eo mister that is a spray bottle with a titanium based anode and cathode within and electrolysizes salt water in the bottle. It was just great in concept. Elementalmaker channel on RUclips showed this. Btw, chemplayer had done this, I want to say s/he had used the dioxide or maybe it was sulfate (been a few years on the starting material, sorry) but anyways he used nitrate salts and the oxide (likely this) and roasted it in a can like you did but over a Bunsen burner. The yield I don't recall either.
:0 New video!
The easiest source (for anyone needing some) is certain brands of root killer (used for plumbing/tree roots). I found some for about 10$. My uses are for staining mahogany, not for lab use. Not sure of the purity. You need to check the label as some brands use other chemicals. It should just list ingredients as potassium permanganate.
One procedure says you should mix 500 g of KOH solution (sp. gr. = 1.475, nigh on 45%) with 105 g of KClO3 and evaporate it while adding 180 g of MnO2 and evaporating until thick. Next, the cake is cooled, crushed, and heated up to red hot. The resulting melt is dissolved in a large amount of water while bubbling CO2, the mixture is left to stand for a while, and the supernatant is evaporated until some crystals form. Maybe chlorine would be better because it somewhat increases the yield, but you definitely need a really huge temp
Is potassium permanganate some kind of banned precursor chemical nowadays? I remember I'm sure I had it in one of those home science chemistry kits as a 1970's child, and in secondary school chemistry it was one of the first to be experimented with especially because of the purple colour change redox, and also the glycerine reaction.
Woo potatium pomegranate
I always see those in the lab during my secondary school days.
I love pomegranate
Isn't this the same chemical used in the 'burning volcano' demonstration? Was hoping for some of that. Anyway, good job, pretty color.
Could an oxidation of manganese salts to +VI state be performed (in aqueous solution) with potassium peroxydisulfate? That stuff is cheaply available in bulk and unrestricted in the EU. If it forms SO3 as a side product, that's even better, provided that it's captured and recycled.
The boss
Potassium is my favourite colour
It's used medically to kill surface infections in the skin and unlike things like Detol doesn't desiccate the skin as much .I am guessing that it probably works against fungal skin problems like Ringworm too.I have a rare skin Lymphoma derived from the T Cells and have had problems with skin infections and you have to be rather careful as they are a major source of death.
new nurd rage videos ? lfg!
Just curious what would happen if you mix such a strong oxidizer into tanerite?
Out of curiosity, have you tried using potassium ferrate instead of potassium chlorate? That stuff is a lot stronger and the iron oxide residue should be easier to remove from the solution.
*Just call any company selling WATER TREATMENT supplies. They sell it by the 50 lb. bag with no questions asked. Used to CLEAN water in water treatment plants. They use TONS!*
You have to understand the world is a big place, with lots of different countries, rules, and regulations. What is easily available for you may be tightly restricted in other places. Some of my viewers have already done what you said and told me those companies refuse to sell it to individuals. So you are completely wrong when you say "any" company will sell it with "no questions asked". Your country might be great and unrestricted, but that's not the same for all countries.
But even if it were, i'm here to teach chemistry. Everything i have ever made, can be bought, but it's still interesting and educational to watch it being made. Lots and lots of educational youtube videos show how to do or make things that you can already get elsewhere, that doesn't mean those videos shouldn't be made.
@@NurdRage *Well in 'Highly Regulated Calirornia' I have noticed if you try to but chemials for "LAB" or "CHEMICAL' supply companys there is a lot of RED TAPE but if you buy from "INDUSTRIAL" suppliers they just ask 'How much do you want and where do we ship it too?'. I understand your point too...*