making potassium (per) chlorate

[Tesla]

Still not working. I possibly don't have permission to view it.

 

Is this the same file though? It fits your description.

http://www.freepyroi...rchlorate_1.pdf

 

Yes, it is somewhat more expensive on a chemical level in a way. At least in the US both are really quite inexpensive however. Another thing that I've heard of people doing is recycling the left over solution. When you mix the sodium chlorate and potassium chloride and cool it down, you'll get primarily potassium chlorate precipitating out. The solution you filter off has mostly sodium chloride in it, with a little potassium chloride, potassium chlorate, and sodium chlorate. You can easily reuse that solution, resaturate it with sodium chloride and electrolyze it again. In the long run you essentially are only paying for potassium chloride, and a relatively small amount of sodium chloride to regenerate the liquor.

 

Yep that’s the guide. So is this method more efficient thena potassium cell?

 

[Mumbles]

I haven't heard any efficiency differences between potassium or sodium chloride, so I really don't know if one is better than the other. Sodium will allow you to make more per run, but the potassium cell will probably be cleaner. There was some mention before about the chlorate crystallizing on the electrodes, and lowering the efficiency. I don't have a lot of practical experience with cells.

 

There are a few things off with that tutorial. I don't know how well that method of electrode manufacturer would work. If you could just crush lead dioxide and coat it with PVC cement and have it work well, I don't know that many would go through the trouble of electro-depositing it. The author of that guide apparently can get 1.5x the theoretical amount of NaCl into solution. He says he filters it upon heating and cooling it, but it he uses the 600g/L figure later when describing the precipitation of potassium chlorate. You can only get about 370g/L into solution. Additionally, you cannot prepare barium chlorate by the same method. At room temperature, it has a fairly significant solubility in water of approximately 270g/L. I'd be willing to bet a real recrystallization instead of simple precipitation would do it though.

[Tesla]

I haven't heard any efficiency differences between potassium or sodium chloride, so I really don't know if one is better than the other. Sodium will allow you to make more per run, but the potassium cell will probably be cleaner. There was some mention before about the chlorate crystallizing on the electrodes, and lowering the efficiency. I don't have a lot of practical experience with cells.

 

There are a few things off with that tutorial. I don't know how well that method of electrode manufacturer would work. If you could just crush lead dioxide and coat it with PVC cement and have it work well, I don't know that many would go through the trouble of electro-depositing it. The author of that guide apparently can get 1.5x the theoretical amount of NaCl into solution. He says he filters it upon heating and cooling it, but it he uses the 600g/L figure later when describing the precipitation of potassium chlorate. You can only get about 370g/L into solution. Additionally, you cannot prepare barium chlorate by the same method. At room temperature, it has a fairly significant solubility in water of approximately 270g/L. I'd be willing to bet a real recrystallization instead of simple precipitation would do it though.

 

 

 

Ok thanks for the info, I think I'll try a potassium cellfor my first time, (it seems slightly less complicated) In the future i might switch to sodium. I bought a 4 by 10inch MMO anode and an atx computer power supply off ebay, all I need now is twoTI/stainless steel cathodes, some KCI, a five gallon bucket, some vent tubing,and I'll be set. Thank you very much for all your help Mumbles!

 

[Bonny]

Ok thanks for the info, I think I'll try a potassium cellfor my first time, (it seems slightly less complicated) In the future i might switch to sodium. I bought a 4 by 10inch MMO anode and an atx computer power supply off ebay, all I need now is twoTI/stainless steel cathodes, some KCI, a five gallon bucket, some vent tubing,and I'll be set. Thank you very much for all your help Mumbles!

 

 

If you are using a 5gal bucket and computer power supply, one cathode will be fine. My biggest anode was maybe 4 x 6 and easily handles the current from a computer supply. I would recommend getting a Ti anode rather than SS. Take a good read through this thread and Swede's blog. Great info from people who have done this many times.

[oldmanbeefjerky]

good luck.

im trying this method soon, of simply removing the potassium chlorate (literally just scooping it out every 2 days) as it forms, to get my chlorate sooner!

 

also, i realise now why my past lead dioxide (from car battery) anode cell didnt get me any chlorate!

 

i was under the impression that like potassium, sodium chlorate also becomes less soluble with the addition of oxygen, so when i performed the end boil, i discarded the liquid i now realize was full of chlorate, and kept the precipitant, which was salt!

[Tesla]

If you are using a 5gal bucket and computer power supply, one cathode will be fine. My biggest anode was maybe 4 x 6 and easily handles the current from a computer supply. I would recommend getting a Ti anode rather than SS. Take a good read through this thread and Swede's blog. Great info from people who have done this many times.

 

 

 

 

One cathode will make it easier to adjust spacing, speakingof which how do you find out how much space you should have between your anode and cathode? I'll go look through Swede's blog and see what i can find out.

 

Edited July 24, 2011 by Tesla

[oldmanbeefjerky]

Somewhat rhetorical in the extremes that question, isn't it.

well its my understanding that more spacing = more current draw , and faster electrolysis if the power supply can handle the resistance

[Bonny]

One cathode will make it easier to adjust spacing, speakingof which how do you find out how much space you should have between your anode and cathode? I'll go look through Swede's blog and see what i can find out.

 

 

I spaced my electrodes about 1" apart IIRC. That gave me about 20-25A using a computer power supply. Most (including mine) are supposedly rated for 20A, but I ran mine at 25A for weeks at a time. Run the cell until the amps drop to ~15 and then harvest - this was all done using KCl not NaCl.

 

Somewhat rhetorical in the extremes that question, isn't it.

well its my understanding that more spacing = more current draw , and faster electrolysis if the power supply can handle the resistance

 

Less spacing increases the current. And yes more current will make the process faster.

[oldmanbeefjerky]

hmm. i think a computer operated cell is in order!

 

a cell which automatically shuts down as soon as the amperage gets too low, or better yet, a current independant circuit breaker, which cuts off if the current drops to much. i havent a clue as to what it could possibly be used for, but meh, i bet they exist.

ideas just pop into my head all the time on this forum. i am going to make a great book/ blog on this.

 

pc power supplies are good like that, they are disputably one of the cheapest components of the computer, and the hardest to break by use. though i acidentally broke my ones short circuit protector when the 12v+ wire touched the case of the ATX, first my laser and now this.

might i ask how many g/L of KCl was dissolved in the cell?

[Bonny]

 

might i ask how many g/L of KCl was dissolved in the cell?

 

 

 

I used to simply use room temp water and load it with KCl. Allow it to sit sit for a day or so, stirring/shaking here and there. This also works well when "recharging" a new batch from the water of a previous run.

 

Now, I use the amount based on about 30C, which my bucket cell seems to run at. I dissolve the KCl or KClO3 in water by heating to make the process faster.

The potassium solubility chart is on the attached link under potassium chlorate... I think

 

Keep in mind this is only how I do this. Might not be the best way, but has worked well for me.

 

I'm not sure if you have looked at this site...a wealth of knowledge.

 

http://oxidizing.110mb.com/chlorate/chlorate.html

Edited July 25, 2011 by Bonny

[oldmanbeefjerky]

actually i have, there always seems to be allot of good info on that site.

so your saying its a saturated solution then.

also i should have asked before, what voltage your running your cell at, 3v or 5v? and the size of the anode your using? what your doing right now is exactly what i plan non doing once my MMO anode arrives and it seems to be working well for you.

[WSM]

might i ask how many g/L of KCl was dissolved in the cell?

 

Typically 300 to 350 grams per liter. Though it is temperature dependent, I usually just dissolve as much as will naturally go in (I only heat it if the weather is cool). Stirring will speed the process under every circumstance.

 

WSM

Edited July 25, 2011 by WSM

[oldmanbeefjerky]

i see!

so at full saturation it will pull 25A from an ATX when the electrodes are 1 inch apart.

runing at 5V because 3V generally wont allow for more than about 10 amps, so ill asume its 5V

[WSM]

i see!

so at full saturation it will pull 25A from an ATX when the electrodes are 1 inch apart.

runing at 5V because 3V generally wont allow for more than about 10 amps, so ill asume its 5V

 

Hi OMBJ,

 

That's a fair assumption. I'd run it on the 5Vdc output and the internal cell resistance should help it be closer to the textbook voltage of 3.6Vdc.

 

It never hurt my systems to be a bit higher (than 3.6 V), but too low (<1.75 V) and things start to not work right. The explanation is in a few technical journals and doctoral thesis' I've read, that I won't take the time to explain (barely understand it myself ).

 

The 5 Volt section of the computer power supply should get you going . I recommend bonding all the 5 Volt leads to a positive bus and a negative bus, then connect the buses to your electrode leads (for maximum current transfer and minimum inefficiency [heat] in the leads).

 

WSM

Edited July 25, 2011 by WSM

[WSM]

I was looking at the LD anodes from China and got an idea for chlorate electrodes using the eBay MMO mesh. I have some MMO ribbon I acquired a few years ago. It's 1/4" wide and 0.025" thick and many feet long. For better lead (pronounced leed, not Pb) contact on the mesh, I can spot weld an edge on the MMO mesh of the MMO ribbon; then spot weld a strap or tubular lead to the ribbon. I can see this giving a better electrical connection between them and lower resistance at the point they're connected.

 

What do you think? Should I bother?

 

WSM

[oldmanbeefjerky]

Hi OMBJ,

 

That's a fair assumption. I'd run it on the 5Vdc output and the internal cell resistance should help it be closer to the textbook voltage of 3.6Vdc.

 

It never hurt my systems to be a bit higher (than 3.6 V), but too low (<1.75 V) and things start to not work right. The explanation is in a few technical journals and doctoral thesis' I've read, that I won't take the time to explain (barely understand it myself ).

 

The 5 Volt section of the computer power supply should get you going . I recommend bonding all the 5 Volt leads to a positive bus and a negative bus, then connect the buses to your electrode leads (for maximum current transfer and minimum inefficiency [heat] in the leads).

 

WSM

 

already done that.

 

 

also, it sounds as if it will work, but you need to ask yourself "do i(you) think itle work?", and if yes then go ahaed and experiment, but if you want to be conservative with your electrodes then dont.

im sure other members though can come up with viable reasons why you can and cant though

[Bonny]

i see!

so at full saturation it will pull 25A from an ATX when the electrodes are 1 inch apart.

runing at 5V because 3V generally wont allow for more than about 10 amps, so ill asume its 5V

 

 

I use the 5V setting. For chlorate I was using a ~ 4 x 6 MMO anode and an equal size Ti cathode. Right now I'm using the same power supply (again at 5V) to make perc with a LD anode and Ti cathode. The run is almost done. There is a LOT of black crap in the cell, hopefully the anode is still OK.

 

I seem to have a problem with anodes making perc. I fried 2 Pt anodes and now I am wondering if my LD is surviving. I plan on shutting the cell down tomorrow or Wed (need to check my notes for start time). The amperage hasn't dropped at all though and I don't remember if it did in previous perc runs.

 

@WSM: Why not try the ribbon idea? Might be a new Are you running any (per)chlorate these days? I haven't seen any new posts on the super cell you were working on for quite awhile...

Edited July 26, 2011 by Bonny

[oldmanbeefjerky]

hmm, perhaps there is a contaminant in the cell. or your lead dioxide anodes are compressed/binded alpha. essentially dodgy.

from what ive read though, perchlorate is a tricky business, and if you dont to things exactly right, even platinum will be eroded away.

[pyrojig]

BTW thanks for the advise 2 pages ago... WOW ... ! A lot of info since then, and very useful ...

Thanks WSM, I may hit you up for advise in the near future here.

[WSM]

@WSM: Why not try the ribbon idea? Might be a new Are you running any (per)chlorate these days? I haven't seen any new posts on the super cell you were working on for quite awhile...

 

Hi Bonny,

 

I'm considering the ribbon idea for "The Monster" (the super cell). Those components are sitting and waiting (impatiently) for me to get to them . I stopped progress on it to try some experiments with the smaller system I built (the one with the concentric electrodes). I wanted to decide some fundamental concepts with that experimental system before hacking into the beautiful work done on "The Monster's" tankage.

 

Remember, "The Monster" is designed to run continuously rather than as a batch system, so a lot more control goes into it. I plan to automatically inject dilute acid to control pH, monitor voltage and current as well as RC and CC temperatures. Of special note, since the CC is a lower temperature (so crystals will drop out) I need to create a separate tank in the CC (a heat well, if you will) where I have a heater to warm the mother liquor so crystals won't form and foul float switches or jam the pump I'm using to return depleated liquor to the RC. I plan to replace the salt used up according to the amount of chlorate harvested, to try to keep everything balanced (it can be a real juggling act!).

 

The biggest problem is I need to build a shed with power (and a lock on the door) to run the thing in so nobody can mess with it. I don't have a lot of space or funds for the project (let alone time), but I need to make it safe. I don't need my little grandchildren to get into something that could harm them (or my sweet Wife would harm me)! I've had several suggestions given for different types of structures that can be put together but my Wife would rather the whole thing is out of sight (she doesn't mind me having stuff, she just doesn't want to see all my clutter ). All of this limits my options and slows my progress. I bet if I build a pool in the yard, she'd let me run a saltwater chlorinator for it! Maybe that's how I'm going to sell this to her ...

 

Again, more later...

 

WSM

[Bonny]

hmm, perhaps there is a contaminant in the cell. or your lead dioxide anodes are compressed/binded alpha. essentially dodgy.

from what ive read though, perchlorate is a tricky business, and if you dont to things exactly right, even platinum will be eroded away.

 

The only contaminants would have comoe from either the electrodes or the (bubbler) tube. WSM also questioned the LD anode. In any case I am going to shut the cell down today I think.

[WSM]

BTW thanks for the advise 2 pages ago... WOW ... ! A lot of info since then, and very useful ...

Thanks WSM, I may hit you up for advise in the near future here.

 

Hi pyrojig,

 

You're welcome. I'm glad I could help.

 

Feel free to ask questons here where everyone can try to answer. Between all the responses, you may well get inspiration to do something great we can all learn from. I've received a lot of inspiration here myself.

 

WSM

[WSM]

The only contaminants would have comoe from either the electrodes or the (bubbler) tube. WSM also questioned the LD anode. In any case I am going to shut the cell down today I think.

 

I remember patsroom saying if there are chips in the LD, to keep those parts out of the liquid. I imagine the concern is not letting the liquid cause separation between the LD and the titanium substrate (which would be witnessed by lowering current levels as the damage progressed). He said that was the only help the manufacturer of the LD would offer. We have to try the anodes and see.

 

I wonder if running sodium chlorate would work any better than potassium chlorate?

 

WSM

[oldmanbeefjerky]

What if perchlorate was forming inside the surface on the LD anode? crystals forming on it might have roots or something that did into the soft anode and as they grow they chip off lead dioxide, like tree roots in pavement. im fairly certain that in swedes blog there is an image of perchlorate forming on the anode, but i think he was using sodium in his cell.

This will most certainly be the case if it works fine with sodium chloride (shows no erosion), on your next try!

[WSM]

Hi OMBJ,

 

Swede was using potassium chlorate in his perchlorate cell. It was a proof-of-concept test; and it worked (at least in part). There were problems but at least we learned that it is possible. As far as LD on MMO is concerned, my feeling is we'll do better with sodium salts, but we need to run the tests to settle the question.

 

WSM

Edited July 26, 2011 by WSM