making potassium (per) chlorate

[g&t]

ah so this is where all the action is! I've read all the threads on ukpyro forum and the e&w forum but they are stagnant. it's good to find current discussion on current development.

 

Also, G'day (hi) to everyone here. I think this is my first post!

[WarezWally]

There is a fair chunk on science madness

[BPinthemorning]

g&t, please don't flood the forum. what you said was totally unnecessary.

 

Anyway... Does anyone have a good guide to making a MnO2 anode? I've been looking everywhere and can't find anything but information on the MnO2 in batteries.

[g&t]

wow so there is! 34 pages on lead dioxide anodes.

 

I'm planning on getting some MMO mesh designed for cathodic protection in buildings etc. to make some chlorate. I'm still not sure what to use for perchlorate but I think buying a platinum coated anode would be he easiest thing for me. I'm intersted in what pkhow said on the ukpyro forum- He thinks you could use MMO anodes for perchlorate because the can withstand fairly low chloride levels. I don't have a good enough understanding of how it all works yet so I can't really question his ideas. Most people say MMO won't work but he says it will.. I guess I should try it and see!

 

 

edit: BPinthemorning, ok but I just wanted to say hi and this is the topic I'm interested in. perhaps I should have looked for a new member introduction thread. my apologies if my post is seen as flooding.

[tentacles]

bp - check on sciencemadness under technochemistry. You need some Ti, cobalt nitrate, stannic chloride, and manganese nitrate. You can reasonably do it without the stannic chloride, however. That makes it.somewhat OTC. You can find Co and Mn carbonates at a pottery supply shop. Also you need a heat gun or oven capable of 380-400C. HCl is a good idea to etch your Ti before coating - oxalic acid works too. Also you need a bit of nitric acid to make nitrates out of yonder carbonates.

 

Things you need (not a complete list)

 

Ti sheet, strip, rod, chunk, whatever

Co(NO3)2

Mn(NO3)2

SnCl4 (somewhat optional)

HCl

H2SO4

Heat gun

Tube to go on the end of the heat gun

Thermocouple that can measure >400C

Alcohol (ethanol, methanol or isopropyl)

 

If you just want to make some chlorate and don't have most of this stuff already, you are better off buying one of those MMO anodes. Unless you are looking to make a huge cell maybe.

 

g&t, welcome to the thread and the forum.

[Mumbles]

g&t, don't worry about it. BPinthemorning isn't a mod and never will be, so he really needs to stop acting like it. His post was of the same usefulness level as yours anyway, so perhaps he should follow his own advice.

 

There is an introduction thread pinned in the random discussion and chat section should you want to seek it outl

[InRainbows]

Hashashan, you know I meant heat lead with Kno3 until I get PbO, then take the PbO and heat it wait another batch of KNO3, not just obtain PbO and heat it.

[hashashan]

I doubt it can do that .. PbO2 is an extremely string oxidizer, it can oxidize chlorate to perchlorate.

I never heard that it is possible to oxidize PbO to PbO2 with KNO3.

why don't you want to use NaOCl?

[Mumbles]

H2O2 also works very well for creating PbO2 from PbO.

 

Alas back to my second point though in that the electrodes (to my knowledge) have to be grown, not pressed.

[hashashan]

Yes mumbles you are totally right, however some methods of making a PbO2 anode do require some powdery PbO2 also

[tentacles]

You can use a pressed PbO2 powder-binder substrate, but they do not work as anodes without plating a solid PbO2 layer on top. The benefit is the same thermal expansion rate as the plated on surface, I guess. It's an impractical amateur technique, as something like 6000psi was used in the molding.

 

New info on the Chlorates and Perchlorates page:

http://www.geocities.com/CapeCanaveral/Cam...ox/tiatold.html

[WarezWally]

Pretty much the same method we have seen before, coat Ti and then plate alpha and beta LD.

[BPinthemorning]

What do you guys think of this for an anode?

http://www.scitoyscatalog.com/Merchant2/me...&Category_Code=

I cant tell how thick the platinum is, but it looks like a good deal after researching the price of solid platinum wire, and platinum clad anodes...

[tentacles]

If you want a Pt plated anodes, buy Pt wire (or something) or buy a Pt plated Ti perchlorate anode. That nickel wire will corrode down the middle, leaving you with a microscopically thin Pt tube - if it doesn't just disintegrate. There ARE folks out there selling Pt plated anodes. I picked up a Pt plated Ti anode for plating gold and Pt some time ago, it will probably work fine for perch but I am hesitant to use it. I'd rather make an anode that I just just dump current into and let it run until I've got a pile of perch.

 

BTW: I paid $17, shipped, for the Pt plated anode, it's like 35cm^2. Just keep your eyes open and you can find one, no telling how long it will last though.

[BPinthemorning]

I planned on looping the wire so no nickel would come in contact with the solution...

[WarezWally]

I get white deposits on my cathode (titanium), from what I can tell they are no oxidizers. Any ideas what they could be? I clean them off with HCl (they disappear in seconds)

 

Could it be potassium hydroxide?

[tentacles]

If it's KOH, it would fizz like crazy in HCl. Is it a hard crusty deposit, filmy, slimy? Got a picture? Are you using an additive at all yet?

[WarezWally]

I only added some NaOH, it did fizz fairly crazy in HCl releasing a clear gas.

 

Looked a bit slimy, couldn't see any crystal shapes.

[Mumbles]

Hydroxides don't fizz in acid. In fact the only thing that should fizz in HCl are carbonates and free metals. Well, cyanides, azides, and a few others would fizz, but it's unlikely you have those. Let us know if it smells like almonds, or you die though

 

KOH + HCl --> H2O + KCl

[dinang]

thanks

[dankish]

Don't know if any of you have mentioned this,or have seen this but...

 

PRE-BUILT POTASSIUM CHLORATE CELL

 

PRE-BUILT POTASSIUM PERCHLORATE CELL

 

My apologies if this has been mentioned.

[tentacles]

Most of us are aware of the products available from JJF pyro.. The first problem with that setup is round anode + only 1 square cathode... But I think most folks would be more interested in a somewhat larger cell, and others are interested in anodes that can be self-produced..

[northstarpyro]

HI I make the cells listed on ebay, i'll attach some links and files that you can look at. your main problem as i see it is that you lack patients.

these cells don't go fast and your initial solution will have to mature. Once you have a solution that has been run for a bit, providing your replacing your solution regularily with new soluiton to make up for whats in the bottom of the jar. Lead dioxide is very toxic and very hard to make, graphite will just decompose and make a mess. You can get an MMO anode and Titanium mesh or tube cathode. This makes KCLO3 and it's very clean. You still have to boil off the hypo-chlorite when your done. you can then bake your kclo3 in a toster oven ( outside ) and it will p/u the extra oxygen molecule. thus you have kclo4. None of this is rocket science. But it takes time. If your in a hurry just buy it. read the attached files and good luck.

Links_to_other_materials_and_information.doc

[WarezWally]

Heating KClO3 in a toaster oven until it is molten is a very dangerous thing to do, if anything comes into contact with it be prepared for a extremely violent reaction.

 

Some of the KClO3 will decompose back into KCl and in the process will give up its oxygen. I don't know how high or pure your yields will be but it seems like a very dangerous procedure and even then you still have to destroy the chlorate for it to be of any use.

 

I dont really know if its necessary for you to boil off the hypochlorite if you just use KCl. I simply let my cell sit unpowered for a day and it turned crystal clear and had no smell of chlorine. This may be due to the fact that potassium hypochlorite easily decomposes but I cannot find any information on it.

 

I boil it anyway

[tentacles]

That's interesting, wally - that batch of KClO3 I did with graphite stayed yellow, and still smelled of hypochlorite after boiling it for hours. I still haven't recrystallized the end product, but it still smells of hypochlorite. The KCl I started with was water softener 99% grade, and I recrystallized that before using it in the cell. In my previous NaCl attempts, the hypochlorite went away after boiling briefly.

 

Did you leave the anode in the cell, unpowered? If so, perhaps the hypochlorite is preferentially catalyzed back to Cl by the anode coating. (Which becomes a catalyst when the power's off).

 

Northstarpyro: It's not necessarily possible for some of us to just go buy KClO3/4. Lead dioxide is far less toxic than some other more common lead compounds, and it's not terribly difficult to make - it does require a very toxic lead compound to do so. Certainly, making a successful lead dioxide anode is no small task.

 

Some of us just want to make our own anodes just because we can, or in some cases, because the size or form factor we desire isn't availible to purchase.