potassium permanganate synthesis

[woo-jong]

This information is from my book 'Inorganic synthesis experiments'(This book doesn't exist in USA. it's a Korean book)
this says how to synthesis potassium permanganate from manganese dioxide.

What we need : KOH 10g
KClO3 5g
MnO2 10g
a crucible , heating source, iron wire

Procedure :

1) Mix crushed 10g of KOH and 5g of KClO3 in a crucible.

2) While stirring with iron wire, heat to 400 degrees Celsius to make it melt. Stop heating when all of the mixture melts.

3) Slowly add 10g of powdered MnO2 to melted mixture. procedure 2,3 needs stirring with iron wire. If you don't stir enough, it will be difficult to perform next procedure

4) Harden the melted mixture and powder it. Dissolve this in 200ml of boiling water.

5) To neutralize excess base, we should bubble CO2 gas through the solution of procedure 4

6) Let the precipitate(MnO2) settle down into the bottom of beaker. and filter it with glass filter(not filter paper)

7) Finally , let the solution evaporate. There will be purple crystals. this is potassium permanganate. Wash it with a small amount of cold water and store it.

[megalomania]

I have recently conducted a review of the synthesis of this substance for my work on OTC benzene. While that procedure closely fits with what I have, I should add one step. To obtain a superior homogenous mixture of potassium chlorate, potassium hydroxide, and manganese dioxide dissolve these in a minimum amount of water. Upon heating to remove the water they will be well mixed. The manganese dioxide does not dissolve of course, just the potassium compounds

It is not entirely necessary to use the CO2 as you will get KMnO4. However, it will improve yields. Most assuredly there will be some potassium manganate (K2MnO4) that the CO2 will convert into permanganate. 3K2MnO4 + 2CO2 --> 2KMnO4 + MnO2 + 2K2CO3. The manganese dioxide can be recovered after this.

I want to take this to the next step. There are a few pressing issues that should be addressed in making this a worthwhile synthesis. Basically they all revolve around where to get the starting materials and how to recycle the waste products.

For the recycling it will be necessary to get back all of the potassium chloride and carbonate that is left behind. It is also desirous to purify the potassium permanganate by removing these materials. If you just let the final solution evaporate, you will get a mixture of potassium permanganate, potassium chloride, potassium carbonate, and most likely some potassium hydroxide and potassium chlorate. That seems like a mess to me. Fortunately potassium permanganate is the least soluble of these. It can be recrystallized as it were by reducing the volume of water and chilling it in an ice bath to precipitate the crystals. This may take some time to do effectively, or may take a few batches.

I would say keep all the potassium compounds because you may want them to make KOH. This leads me in to where to get KOH as well as the chlorate. I do believe there are various methods of making potassium chlorate out there? If there are I am not familiar with them at this time. I do know that getting potassium compounds are not all that simple. As far as I know the only commercial OTC source of potassium ions is driveway ice melter, and this is a mix with sodium, potassium, calcium, and magnesium chlorides.
Ahh but in the Poor Man’s James Bond there is that wonderful bit about making potassium ferrocyanide. The first step is to extract potassium carbonate from wood ashes. Bingo, plenty of potassium compounds there. Now I don’t recall if that stuff can be purified, but I do know it can be done. I once obtained a nice crop of crystals (it helps to have a fireplace that is frequently used). From here it should be a simple matter of flower pot electrolysis to obtain KOH. After doing this you can substitute the waste potassium compounds in the same electrolysis. IIRC you also make potassium chlorate by electrolysis? This should take care of both the hydroxide and chlorate.

Now then, what about manganese dioxide? I have heard you can get this from batteries. Specifically dry cell non rechargeable types, especially the big lantern kind. I have begun collecting batteries a few months ago in anticipation of cracking them open. What I do not know is what to do when I open them. I gather you want the central black core of the battery, the powdery black stuff. I could have sworn I once saw a website that had a diagrammatical representation of the battery with info on plundering the MnO2 core. I have not yet obtained a big lantern battery (I am waiting for one to die), but I imagine they would give the greatest yield on time invested. Meaning it is just as easy to cut one of those open as it is to cut open a AAA battery, but with a lantern battery you get much more.
I think the MnO2 is in a paste with a base. Chucking it into water may dissolve everything but MnO2. I am sure someone here has more experience with this than I.

Alternatively one could buy KMnO4 for their water purifier or their pond. Potassium permanganate is now listed on the DEA’s watch list and as such its availability is diminishing. I have prepared some writings on legit uses of permanganate so as to have some plausible excuses as to why to buy it from a water store (like a Culligen man, any place that sells water purifiers, softeners and such). Its use in water softeners is dwindling because only older ones use it. It can be purchased online for adding to ponds (algae control I believe, I have some excuses for that as well).
I still find it necessary to know how to make potassium permanganate from manganese dioxide because after you use potassium permanganate you end up with lots of manganese dioxide. Cheap bastard that I am I find it shameful to go through all the trouble of getting either potassium permanganate or manganese dioxide and then just throwing it away.

I have some experimenting to do it seems. I am documenting this information for my OTC benzene project, which uses potassium permanganate to oxidize toluene. It is a requirement that everything be OTC and so I have studied up on where to get potassium permanganate, and how to recycle it. Any and all criticisms and comments on my theoretical steps outlined here will be much appreciated.

[Pu239 Stuchtiger]

Potassium cations are plenty easy to come by. Potassium hydroxide lye, for example. Potassium nitrate! Potassium chloride is sold as a salt substitute.

The chlorate anion can be prepared by heating a solution of hypochlorite anions.

3[OCl-] ---> [ClO3-] + 2[Cl-]

It can also be prepared by bubbling chlorine dioxide through water - results in a stoichemitrically equal amount of chlorite and chlorate anions.

Hot solutions of chlorides can be electrolyzed, resulting in the formation of chlorates. Alternating current is desirable.

I have no trouble finding potassium permanganate. I buy it at the local hardware store; 2.27kg for $25.

<small>[ August 29, 2002, 03:07 AM: Message edited by: Pu239 Stuchtiger ]</small>

[Polverone]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">As far as I know the only commercial OTC source of potassium ions is driveway ice melter, and this is a mix with sodium, potassium, calcium, and magnesium chlorides.</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">Nope. Look for muriate of potash - potassium chloride - at agricultural supply outlets and many home and garden centers, and also for sodium-free water softening. Many premium alkali drain openers contain potassium hydroxide and potassium hypochlorite. Cream of tartar - potassium bitartrate - is available (at a high price) in the spice section of grocery stores and is easily converted to potassium carbonate by heating in air. Potassium nitrate has a number of OTC sources. KOH may be obtained in pure form as a supply for soapmaking.

You can react K2CO3 with Ca(OH)2 to obtain KOH if you don't want to use the slow, tedious electrochemical method and you have a source of calcium hydroxide.

You can obtain MnO2 from batteries, but only the old-style non-alkaline type, which are harder to find nowadays. Far better is to buy your MnO2 by the pound from a ceramics supplier.

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">Alternatively one could buy KMnO4 for their water purifier or their pond. Potassium permanganate is now listed on the DEA's watch list and as such its availability is diminishing.</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">KMnO4 has been on the DEA's watch list for quite some time, but since it is used for cocaine production in South America they don't seem to care about small (less than dozens of kilograms) domestic purchases. Acetone is "watched" too, yet you can buy it any hardware store. KMnO4 isn't too hard to find, you just have to hit the right store. It's not suspicious to purchase from a dedicated dealer, either.

KClO3 can indeed be prepared electrolytically, or by bubbling chlorine through hot KOH solution.

[frogfot]

Carbon-zink batterys are the cheapest nonrechargeables, they contain mix of carbon powder with MnO2 soaked in NH4Cl solution. Havn't heard about ammounts :(
I have extracted the NH4Cl, but don't really see how to separate MnO2 from carbon.

[Cricket]

I had never heard of glass filter paper before, so I nosed around and found a place to buy it, along with many scales (good prices).

<a href="http://lab-supplies.balances.com/lab/7" target="_blank">http://lab-supplies.balances.com/lab/7</a>

NOTE: They have a minimun of $75 order (ok if you are buying a shit load of filters and/or a scale). Maybe this was not as good a site after all.

NOTE 2: I am pretty sure I have seen a bettery with a dry powder inside, not dampened. I can't recall the name, but it was mostly black and had a lightning bolt on it and a cat too I think, maybe this will ease the process. Only name i can think of is Rayovac or something (may not be the name at all or the neme of something else).

<small>[ August 29, 2002, 08:10 AM: Message edited by: Cricket ]</small>

[vulture]

If you open a normal alkaline battery you will find a carbon grey and hard outer layer and some zinc powder with cellulose in the middle. The trouble would be getting rid of the graphite, the only way I see would be dissolving in CS2 as only the carbon dissolves into it.

Keep the zinc powder! It's very fine and extremely pure! You just have to remove the grease by dissolving it into toluene or another aromatic.

[Machiavelli]

How about heating the stuff until it glows? MnO2 is pretty inert and probably won't do anything, NH4Cl will turn to NH3 and HCl if it isn't washed out before and Carbon will turn into CO2.
And wouldn't it be easier to clean the zinc with acetone, as this is normaly my first choice to (dis)solve dirt related problems. And every forumite worth his/her salt has it standing around.

Btw, Polverone, where did you get the coke info from? I know KMnO4 is usefull for speed synths but I don't see how it could be used for coke extraction.

[Polverone]

Vulture: graphite dissolves in CS2?! I find that very surprising. I would suggest that there are better uses for it :)

Machiavelli:

From <a href="http://www.druglibrary.org/schaffer/GovPubs/cocccp.htm:" target="_blank">http://www.druglibrary.org/schaffer/GovPubs/cocccp.htm:</a>

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">Potassium permanganate is combined with water. This mixture is added to the coca paste and acid solution. Potassium permanganate is used in this step to extract other alkaloids and material that is undesired in the final product.

In particular, potassium permanganate is used to break down the alkaloid ciscinnamoylcocaine found in large concentrations in E. novogranatense varieties. If the coca paste has a high concentration of this alkaloid and potassium permanganate is not used, then crystallization of cocaine HCl will be very difficult.</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">

[kingspaz]

Machiavelli, the carbon, depending on Manganese's reactivity may reduce the MnO2.
MnO2 + C --&gt; CO2 + Mn
not sure how reactive Mn is though...

edit: just found that MnO2 is in fact reduced by carbon.
<a href="http://www.scescape.net/~woods/elements/manganese.html" target="_blank">http://www.scescape.net/~woods/elements/manganese.html</a>

<small>[ August 29, 2002, 05:25 PM: Message edited by: kingspaz ]</small>

[irish]

hi all
potassium permanganate is sold in australia under the name condys crystals,price about $17AU per KG.
it's avalable from stockfeed store's along with sulfur,KCl etc.
hope it helps
irish

[vulture]

MnO2 is a pretty strong oxidizer, don't heat it. For example, it will evolve Cl2 when in contact with HCl.

[megalomania]

I didn’t mean to imply that it was the great and powerful DEA, stealer of freedoms and rapers of children, that caused potassium permanganate to dry up. That seems to be the effect of plain ol commerce. The water softeners that use it are no longer in favor, with their being better technologies, and there are better products to put in your pond for algae control. Like most ‘pure’ chemicals out there, they are typically replaced by something better for their intended purpose. We however have alternative uses for our commercial products :D I would agree that the stuff is plenty available when you can get it. I can get a 5 Kg pail of the stuff for $20.00 at a place less than 4 blocks from me, but I still want to have answers to those annoying questions, “Why don’t you buy yourself another water softener?” or the “Can we have your name please…”

As for the potassium ions, nothing has come up in my chemical surveys of the major hardware stores and garden centers, but of course there are many wonderful things in different areas. My point being that it is far more economical to use wood ash as a source. It certainly is for me with a frequently used fireplace, those without one may find it cumbersome to acquire wood and burn it just for ash. Even most people with fireplaces rarely use them as the amount of work involved in obtaining, splitting, stacking, and hauling wood is considerable. Of course I happen to have 40 acres of forest to use. In all fairness I am not the one who cuts and splits all the damn wood, some other fool does that task.

I must check out the local ceramics stores. I have never been to one but recently I have seen several posts talking about all the goodies at one. I opened my new phonebook, which came a few days ago, to see if there were any. Well there were dozens within a 20-mile radius or so. I never knew the places were that popular. There are a few in my own town and I never heard of them.

I have obtained some diagrams of the inner working of alkaline dry cells. I am a little distressed to learn of the reaction
MnO2 + H2O + 2e- --&gt; Mn2O3 + 2OH-
At the same time I see that the MnO2 is actually coating the outside of the carbon rod and it can be scraped off with little actual carbon coming along for the ride. The mixture of zinc chloride and potassium hydroxide can be dissolved away. Any Mn2O3 would appear very much like MnO2. Could anything be done with that compound?
Otherwise it seems to me that only new batteries would have much MnO2. Ultimately this is a very ghetto way of going about getting the stuff, but it is one that is applicable to just about any country of the globe, or for that distant future when all things are banned. It is also nice to fancy yourself some sort of environmentalist by actively recycling :p

PS: There's KOH in those batteries too, sounds like one could kill two birds with one stone.

[nbk2000]

Extraction of KOH from wood ash is very uneconomical. It requires something around a ton of wood to produce enough ash for 10-12 pounds of KOH. <img border="0" title="" alt="[Eek!]" src="eek.gif" />

Whole forests were cut down and burned up to provide the makings of nitre for the black powder used in europes wars during the last few centuries.

KCl, on the other hand, is cheap. 40 pound sacks of it as "Sodium-free Water Softener Crystals" for $10. :) Converting it into something more useful than food flavoring though... <img src="http://www.roguesci.org/ubb/icons/icon17.gif" alt=" - " />

[Pu239 Stuchtiger]

I can't believe you can't find potassium chloride. It has been sold in every grocery store I have ever set foot in. Brand name: "No Salt".

[megalomania]

A ton of wood… While that may sound like a lot, I bet I go through 5-6 tons a year, perhaps even more. The fireplace is burned every day from fall through spring (i.e. when its cold out). Of course I admit this is not a typical usage for a fireplace in this day and age. Most people use their fireplaces a few times a year for company going through a dozen logs. My aunt uses those fake logs on Christmas, just one pitiful little stick burning away. We make fun of her, yes.

It appears I was a bit hasty when I said there were no potassium compounds out there. This time I actually ‘read’ my chemical survey and the results are thus:
At a pool and spa store I found potassium carbonate in solution as a pH raiser, and potassium monopersulfate as spa shock (946 mL/$7.99 and 907 g/$14.99 respectively). At a grocery store I found pure potassium chloride as ice melter (9.08 Kg/$3.99). The other ice melter mix was from Wal-Mart.

[jimwig]

recovery of MnO2 from dry batteries

US1192061

a little crusty (1916) but neat stuff on solubilities and recovering the stuff

[Alchemist]

Hello all,

just a quick note! I have also seen in several chemistry books that KNO3 can been used in place of KCLO3 for the production of KMNO4. I do NOT have the amounts in front of me, but I believe it was about the same as for the KCLO3 or just a little more!

[megalomania]

I wonder if manganese chloride could be substituted for manganese dioxide in the preparation of potassium permanganate? It is in the wrong oxidation state (II), but the same reaction that transforms the manganese (IV) dioxide into manganese (VI) in the form of potassium manganate might work the same.
3MnCl2 + 6KOH + KClO3 -&gt; 3K2MnO4 + KCl + 6HCl
(this is the usual rxn: 3MnO2 + 6KOH + KClO3 -&gt; 3K2MnO4 + KCl + 3H2O)
I bring this up because it would seem to me an easy means of separating manganese dioxide, or manganese oxide from carbon in batteries is to react the oxides with hydrochloric acid to form MnCl2. As this is soluble it can be removed from carbon. A pre-wash with water will remove any hydroxides and chlorides from the battery.

This still strikes me as a good way of getting pure dioxide through the chloride. I have some unconfirmed date here that suggests MnCl2 + Ca(OCl)2 --&gt; MnO2
Could there perhaps be other ways of getting the dioxide from the chloride? I suggested using the chloride earlier to avoid having to go through the trouble.

Some additional notes on the standard procedure may be in order now. The use of a glass fiber filter is necessary because potassium permanganate reacts with regular filter paper, it being an organic substance. One can avoid the filtering step all together by decanting the solution of permanganate. Sure you may loose a little bit, but that is better than shelling out who knows what for special filter media.

It is not necessary to use CO2 in the preparation of the permanganate. One can use just about any acid that is handy. I have a chemistry text that makes the stuff using HCl to acidify the potassium manganate solution. In one of the MAO books there is a bit that recommends bubbling in chlorine gas to avoid the formation of manganese dioxide. And wouldn’t that be convenient to use the chlorine gas generated by adding MnO2 from batteries to HCl (assuming that step works).

It is too bad I don’t have any potassium chlorate handy, I have a battery that I found, so I could test this out. If someone would be so kind as to direct me to a quick reference on chlorate synthesis so I can verify my information, I can start experimenting.

[Polverone]

MnO2 can indeed be obtained from MnCl2 by hypochlorite oxidation. But why bother with that, or with batteries at all (unless you have a lot of old ones lying around?) Get thee to a ceramics supply outlet, and buy MnO2 by the pound. Ceramic grade MnO2 can be less than $1/lb in bulk. Of course, if you *do* recycle old batteries into MnCl2 and then into MnO2, the MnO2 should be more active than what you'd get from the ceramic supplier, since it precipitates in a finely divided form upon aqueous MnCl2 oxidation.

[Boob Raider]

Wish come true Mega .... :p <a href="http://www.poortour.com/build/pyrotechnics/kclox.html" target="_blank">http://www.poortour.com/build/pyrotechnics/kclox.html</a>
This seems to be the most relavent site .... but would someone tell me how to make those damn PbO2 electrodes .... the link on this site doesnt work. I was also thinking ... if a mix of
Mn(NO3)2 and KOH would be heated or distilled (depending on if the rxn works) one should be able to get KMnO4 and H2O and N2O or something like that.

<small>[ October 01, 2002, 11:24 PM: Message edited by: Boob Raider ]</small>

[megalomania]

It has struck me as odd that there is little information on using manganese chloride in chemical operations in the older literature with it being used so much in the preparation of chlorine. In fact I have seen several references to it being a huge waste product. I knew there must be some soul who posed this question in the 19th century, so I kept digging. I found something:

Various attempts have been made to economize the vast quantities of chloride of manganese formed during the manufacture of chloride of lime. The most successful is one employed by Mr. Dunlop. It consists in precipitating the manganese as carbonate, and roasting the carbonate at a temperature of about 600 degrees. The crude acid solution of the chloride is treated with milk of lime in quantity sufficient not only to neutralize the excess of acid, but to precipitate the iron as sesquioxide. The clear liquid is then pumped up into an iron boiler and mixed with a proportion of chalk just sufficient to precipitate the whole of the manganese, an excess being carefully avoided. The mixture is heated by the injection of steam, which is maintained for about 24 hours under a pressure of from 2 to 2.5 atmospheres; under these circumstances carbonate of manganese is precipitated, and chloride of calcium formed in the liquid. The solution is run off from the precipitate, and this is well washed, pressed, and partially dried. In this condition it is introduced in shallow sheet-iron cases on wheels into large vaulted galleries of brickwork heated to about 600 degrees: through these a current of air is maintained. The carbonate is gradually made to pass from the cooler to the hotter portions of these galleries, being from time to time sprinkled with water. The carbonic anhydride is gradually expelled, and oxygen absorbed: so that at the end of 48 hours about 72% of the carbonate has been converted into black oxide. The process, however, is expensive.—
(Hofmann’s Int. Exhib. Jury Report, 1862, p. 36.)

This procedure could perhaps be simplified a bit. First, it is important to note that in the before time of the long long ago the ancients had a considerable amount of iron contamination in whatever process was used to make their manganese chloride. Apparently the manganese dioxide used in batteries is quite pure, certainly free from iron. Therefore there is no need to add calcium hydroxide solution (milk of lime) to precipitate any iron. Assuming the contents of a battery is added to water first to remove any soluble material, then to HCl to make the chloride, and finally filtered to remove carbon, the resulting manganese chloride should be quite pure.
Second, the whole adding steam at 2 atm pressure for 2 days is an industrial process. In the lab we can add calcium carbonate to the manganese chloride solution and boil it, or rather reflux. I can’t say how long it would take all this to go to completion. It may be wise to calculate the precise stoichiometric amount of chalk to add to get this done, a 1:1 mole ratio should do it.
Third, one need not use vaulted galleries of brickwork to cook the stuff. That almost sounds poetic, ahh the good old days when factories were more than just steel beams and concrete slabs. A small improvised furnace with a blow pipe to force air over or through the carbonate should do the trick. Again I can’t say how long this should be done on the small scale.

[Polverone]

Eh?!

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">This procedure could perhaps be simplified a bit.</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">You can say that again! As I said a bit earlier, hypochlorites will indeed convert MnCl2 directly to MnO2. No need to roast it. And if you do want to take a detour through the carbonate and from thence to the dioxide, don't use CaCO3! Although the industrialists of yore may have used the extremely inexpensive calcium carbonate, coupled with extended heating under pressure, on a lab scale you would be much better off using a more soluble carbonate like Na2CO3 or K2CO3. Depending on the strength of the solutions you mix, the precipitate of manganese carbonate may form a sort of gel. But this gel is easily broken up and made filterable by agitation.

But MnCl2 is so pretty that maybe you won't want to throw it away to make icky brown and black compounds. When anhydrous it is yellow, but hydrated it is a lovely rose color. If you have crystals of it that are only partially hydrated you get a beautiful hybrid rose color effect.

And of course if you prepare the hydroxide or carbonate from the chloride, you can then make any acid derivative from those. I don't know what use manganese nitrate may have, but I've prepared it nonetheless! :)

[Marvin]

I think its worth explaining a little of the chemistry behind some of the processes in the thread. What we are dealing with are redox reactions and particulaly in the case of manganese the oxidation/reduction potentials vary considerably with ph. In alkaline solution or fused melt Manganate is very stable and the processes that make it are very easy to do. Any oxide of manganese in fused KOH is very easy to oxidise to manganate. Oxygen in the air will do it, as will virtually all good oxidisers. Once you have manganate, making permanganate is not a problem as manganata is not stable in acid solution, it disproptionates into permanganate and manganese dioxide.

eg, Mn2O3 + 4KOH + 3[O] =&gt; 2K2MnO4 + 2H2O
3MnO4 2- + 4H+ =&gt; 2MnO4- + 2H2O + MnO2

With the chlorate oxidation, the KOH is the base, the chlorate ends up as chloride unable to supply potassium ions. The Manganese dioxide at the end isnt unreacted, its an inevitable result of the conversion to permanganate. The end product of the addition of carbon dioxide isnt carbonate btw, its hydrogen carbonate, which is a feeble acid, but enough to decompose the manganate. K2CO3 would work in the melt instead of KOH, but its melting point is too high. Equivalent sodium compounds do not work as well in these reactions.

Ok, using KNO3. Since the end produce of oxidation is essentially K2O and the hot melt is basic from decomposition of the nitrite 2KNO2 =&gt; K2O + 2NO + 1/2 O2 you dont need much else to make the reaction work. In fact according to Chevillot and Edwards fusing a mixture of 1 part manganese dioxide with 1.5 parts KNO3 yeilds a mixture of KMnO4 and K2MnO4 directly. The workup decomposes any manganate to permanganate and manganese dioxide as before. Since nitre is much easier/cheaper to make/get than either KClO3 or KOH I think this process is likley to be the most useful for recycling KMnO4. I'm very interested in recycling reagents, particulaly oxidisers.

As far as manganese dioxide from manganese(III) salts, manganese dioxide is synthetically equivalent to manganese (III) permanganate. Use dilute solutions and add the manganese salt to the permangonate rather than the other way round, particulaly if chloride is present. Concentrated or acid solutions with chloride liberate chlorine, which is another good reason the manganate workups shouldnt be acidified with HCl.

Getting pure salts from mixtures using fractional crystalation is a method well worth learning, essential for these permanganate methods and wipes the floor with any other method of seperating chlorate from weedkiller. Sieving is next to useless for weedkiller.

[megalomania]

Well, to commerarte my new digital camera I have idly taken some pictures just for my own amusement. Watch as I periodicially attempt to make potassium permanganate from a battery, now in color. I am not doing a formal writeup, I will just be going on the info in this thread.

Let us begin with the victum, an old 6V lantern battery. This big sucker has served its last electrons, and now I have rather easily peeled away the metal skin. Inside are for D size batteries covered in cardboard.
<img src="http://www.boomspeed.com/mega21/battery1.jpg" alt=" - " />

Next up we have a good view of what is inside the cardboard wrapping. The bottom half is what is left of a zinc metal shell. The zinc metal canister was very fragile and after a few raps with a knife the top half peeled away exposing a hard solid cylinder of manganese dioxide and carbon black (hopefully that's what it is). Between the zinc and the black is a thin paper layer.
<img src="http://www.boomspeed.com/mega21/battery2.jpg" alt=" - " />

I felt a water bath was appropriate to dissolve any soluable gunk. a lot of the zinc flaked off, it bubbled a bit, and the next day the water was grayish with a skin on the surface of the water.
<img src="http://www.boomspeed.com/mega21/battery3.jpg" alt=" - " />

At this point I used an electric grinder wheel to sand away the excess bits of zinc that I could not scrape off. What was left was more or less a black cylinder.

To kill two birds with one stone I have set up a chlorate making apparatus using the battery insides as the anode. I made a cylinder out of some old screen leaving about a 0.5 cm gap between the anode and the screen cathode. I attached some copper wire to them and connected the appropriate ends to a battery charger. This damn thing reacted right away. This picture is taken seconds after I turned it on.
<img src="http://www.boomspeed.com/mega21/battery4.jpg" alt=" - " />

Here is a top view, look at those bubbles go! I got a big whiff of something bad :( The oxygen also contains various nasties.
<img src="http://www.boomspeed.com/mega21/battery5.jpg" alt=" - " />

<small>[ October 03, 2002, 06:13 PM: Message edited by: megalomania ]</small>