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making potassium (per) chlorate


gods knight

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In the UK there is a proportionately smaller market for water softeners. BUT there is a near complete lack of KCl except at 99.9% purity and proportionate cost.
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Hi All,

My posts may be spotty for the next couple weeks. I'm travelling next week to see my Son's graduation from college and immediately taking off to the PGI convention afterward. If any of you are going to PGI, look me up (or pm me).

WSM B)

 

Well, I'm back.

 

The site in LaPorte, Indiana is excellent; and the people there are glad to have us and are looking forward to the return of the PGI. I managed to keep busy with rockets, mostly, but did a little work with smoke compositions, too.

 

I had precious little discussion with anyone at PGI about electrochemistry, but did get to share some Viton tubing with a friend from WV who runs a cell. I need to catch up with tool orders and then focus on getting my experimental system ready to run :).

 

WSM B)

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I have become increasingly interested in making a chlorate cell.. however I'm not really sure what to do on the MMO electrode front. Where/whom can I get one from? And what price range should I be expecting?

 

Thanks 2smile.gif

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I have become increasingly interested in making a chlorate cell.. however I'm not really sure what to do on the MMO electrode front. Where/whom can I get one from? And what price range should I be expecting?

Thanks 2smile.gif

 

I don't know if he's still in the business but Swede used to sell electrodes in the Agora section. Are there any shipping restrictions to South Africa?

 

WSM B)

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I don't know if he's still in the business but Swede used to sell electrodes in the Agora section. Are there any shipping restrictions to South Africa?

WSM B)

 

OMBJ (in Oz) found used MMO and titanium electrodes from a salt water pool system repair shop. Many times the electrodes are usable after cleaning them up.

 

WSM B)

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@WSM Thanks for the advice, I'll check it out :)

 

Excellent (and you're welcome)! Let us know what you find. :D

 

WSM B)

Edited by WSM
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Well I've found that I can buy MMO electrodes new from salt chlorinator retailers, in all shapes and sizes, so that's sorted. Those electrodes already have wires attached so I don't even need to solder/weld them.

 

I even managed to find a good source of KCl, very high quality for about $25 for 25 kilograms, so I'm all set biggrin2.gif

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Search Ebay SA and then .com and all the other likely ones (Australia? ) People do sell MMO electrode material and some will ship to some other countries.
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Well I've found that I can buy MMO electrodes new from salt chlorinator retailers, in all shapes and sizes, so that's sorted. Those electrodes already have wires attached so I don't even need to solder/weld them.

I even managed to find a good source of KCl, very high quality for about $25 for 25 kilograms, so I'm all set biggrin2.gif

 

Excellent! When you get it set up, take a photo and post it; plus if you have any questions, feel free to ask.

 

WSM B)

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@Arthur The pool retailer I found the MMO's at is in driving distance from my house, so that saves me on shipping and the heavy import taxes we pay here.

 

@WSM Will do, I'll probably only be able to start after I finish exams though dry2.gif

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@Arthur The pool retailer I found the MMO's at is in driving distance from my house, so that saves me on shipping and the heavy import taxes we pay here.

@WSM Will do, I'll probably only be able to start after I finish exams though dry2.gif

 

Your school work is the most important thing for now. The electrochemistry will be there when your exams are done :D. Do well...

 

WSM B)

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Your school work is the most important thing for now. The electrochemistry will be there when your exams are done :D. Do well...

 

WSM B)

 

Thanks, hopefully these exams go well, they are my finals after all biggrin2.gif

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I hope it works because I bought one about six months ago to try for perchlorate production. I consider it a $36 gamble.

 

I also have two of patsroom's Chinese LD anodes to try. I'm a little concerned about the LD because they were damaged in shipping and I'm afraid they'll separate between the titanium and the LD in an active cell. We'll see...

 

I'm thinking the two system approach to perchlorate production is the better way to go, and because of the relative solubilities of sodium and potassium salts, I'm leaning toward KCl for chlorates and NaCl for perchlorates (chloride to chlorate first and then chlorate to perchlorate, in separate operations with different systems).

 

WSM B)

 

Hi WSM,

 

This is a pretty old post, but I haven't been around for awhile. I had one of the patsroom LD anodes. It was total garbage. I did 1 run of KClO3 to KClO4 and the anode was ruined. I still have a bag of blackish KClO4 that needs cleaning.

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Hi WSM,

 

This is a pretty old post, but I haven't been around for awhile. I had one of the patsroom LD anodes. It was total garbage. I did 1 run of KClO3 to KClO4 and the anode was ruined. I still have a bag of blackish KClO4 that needs cleaning.

 

Dang, I was hoping to hear good news on the LD electrode's. Sadly it seems that the cheaper setups (electrodes)for perch dont last, even silver degrades in industrial use. They however have recovery systems that amateurs dont.

Maybe there could be something done to reduce wear, and or protect the LD ....maybe a additive to the electrolyte.

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Hi WSM,

This is a pretty old post, but I haven't been around for awhile. I had one of the patsroom LD anodes. It was total garbage. I did 1 run of KClO3 to KClO4 and the anode was ruined. I still have a bag of blackish KClO4 that needs cleaning.

 

Hi Bonny,

 

That's dissappointing :(.

 

I wonder if a sodium cell with the Chinese LD anode would work better? I have some lab grade sodium chlorate I could try the anode in, but I want to seal the damaged parts first (in hopes of preventing the LD from flaking off the MMO-on-titanium substrate). I am starting to think it would be wise to not over-do the current and voltage on these imported LD anodes, but go easy on them (at least to start), till we know their abilities and characteristics.

 

If I set up an experiment to try them, I'll post the results here.

 

WSM B)

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Dang, I was hoping to hear good news on the LD electrode's. Sadly it seems that the cheaper setups (electrodes)for perch dont last, even silver degrades in industrial use. They however have recovery systems that amateurs dont.

Maybe there could be something done to reduce wear, and or protect the LD ....maybe a additive to the electrolyte.

 

Hi pyrojig,

 

I'm sure you meant platinum and not silver in the second sentence of your post.

 

The thought of an additive or technique to protect the LD is interesting. I confess, nothing to do so comes to mind, but the thought is intriguing. If anyone has any ideas in that direction, I'd love to hear them. It would make using inexpensive LD anodes a real option for amateurs turning surplus chlorate into perchlorate :D.

 

WSM B)

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Hi pyrojig,

 

I'm sure you meant platinum and not silver in the second sentence of your post.

 

The thought of an additive or technique to protect the LD is interesting. I confess, nothing to do so comes to mind, but the thought is intriguing. If anyone has any ideas in that direction, I'd love to hear them. It would make using inexpensive LD anodes a real option for amateurs turning surplus chlorate into perchlorate :D.

 

WSM B)

 

You guessed correctly, platinum was what I was meaning to say. Not sure of a additive that would be neutral, not reactive to the chlorate. It could be something that remained in the liqueur, or had a way of filtering out without leaving contaminates in the final product.

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Hi pyrojig,

I'm sure you meant platinum and not silver in the second sentence of your post.

The thought of an additive or technique to protect the LD is interesting. I confess, nothing to do so comes to mind, but the thought is intriguing. If anyone has any ideas in that direction, I'd love to hear them. It would make using inexpensive LD anodes a real option for amateurs turning surplus chlorate into perchlorate :D.

WSM B)

 

Speaking of platinum; fortunately, solid platinum metal is not required for an electrode! Only the surface of the electrode does the work, so even a thin plating of platinum will work, so long as the metal remains.

 

As I was gathering samples of MMO, one supplier gave me a two foot sample of platinum electrode wire!!! I haven't used it yet but have a few ideas how it can be effective in a perchlorate cell (once we iron out the details of the cell and electrodes). This wire is about 1/16" OD (~1.6mm) and has a thin platinum plate on niobium with a copper core. Obviously the copper has to be sealed before the electrode is used in a cell.

 

I'll try to add more later...

 

WSM B)

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Speaking of platinum; fortunately, solid platinum metal is not required for an electrode! Only the surface of the electrode does the work, so even a thin plating of platinum will work, so long as the metal remains.

As I was gathering samples of MMO, one supplier gave me a two foot sample of platinum electrode wire!!! I haven't used it yet but have a few ideas how it can be effective in a perchlorate cell (once we iron out the details of the cell and electrodes). This wire is about 1/16" OD (~1.6mm) and has a thin platinum plate on niobium with a copper core. Obviously the copper has to be sealed before the electrode is used in a cell.

I'll try to add more later...

WSM B)

 

The supplier I got the sample from (this was a few years ago), suggested covering the bare end of the platinized wire with epoxy. I tried that with an MMO covered wire twice the diameter or 1/8" (~3mm) and after a few days noticed a green stain in the cell. The epoxy cover came off and the exposed copper was reacting, quite badly. When I washed the pale blue powder out of the end of the MMO anode wire, I could see that what was left was MMO on a niobium shell and no copper for about half an inch (~12mm).

 

For safety's sake, I threw away the chlorate crystals rather than try to use any with copper contamination. I also gave up trying to rely on epoxy resin for a seal. I think spot welding the end closed may work or keeping the exposed end out of the cell liquor somehow, would help. I have avoided using copper cored electrodes since then (about six years now), but I think they could be useful if properly prepared.

 

I suspect platinum plated MMO on titanium would work very well and any compromise to the platinum would simply cease to produce perchlorate rather than just totally fall apart.

 

WSM B)

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Drill out the copper for approx. half an inch leaveing the Pt coated Nb 'tube' behind.

You can then fill in this 'tube' with epoxy etc. You can leave the very end of the 'tube' unfilled with epoxy

and when the epoxy has set you can pinch the tube shut to hold in the epoxy and further seal the end.

An alternative is to use this anode material as a U shaped anode. ie both exposed copper ends outside

the cell.

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Drill out the copper for approx. half an inch leaveing the Pt coated Nb 'tube' behind.

You can then fill in this 'tube' with epoxy etc. You can leave the very end of the 'tube' unfilled with epoxy

and when the epoxy has set you can pinch the tube shut to hold in the epoxy and further seal the end.

An alternative is to use this anode material as a U shaped anode. ie both exposed copper ends outside

the cell.

 

Hi frank,

 

I thought of using the U shape, too. I even considered a (or several) long, very skinny U shapes spot-welded to a titanium lead for an anode. It's funny how so many different experimenters come up with similar solutions. This is great. Thanks for jogging my memory :) .

 

WSM B)

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