making potassium (per) chlorate

[WSM]

1:1? hmm, I have read a few things about (per)chlorate cells that have held true with electroplating as well. Current density at the anode (and cathode) is a very key parameter. Current density is what actually drives/regulates the electrochemical reactions. In a chlorate cell you want a higher current density at the anode. From what I've read, too high of a current density at the cathode and the precious chlorate (in the first stage anyways) can actually be reduced at the cathode back down to chloride. Am I missing something here?

 

I've read that somewhere, too. Some electrochemists add a small percentage of dichromate to their electrolyte to help prevent this occurrence. I have avoided this practice myself so as to prevent the need to remove it later. Plus, if my tank should have a catastrophic failure, and dichromate (hexavalent chromium) were released, I'd have an environmental nightmare on my hands.

 

Let's avoid those!

 

WSM

[WSM]

the color was bothering me. I used bolts that were plated gold color they hold the connections to the top. they are the bolts that hold your toilet to the floor. there is no yellow left on them.

I think that is where the yellow is coming from.

on the salt the only thing out of the ordinary was the words that said enhanced. the yellow is light colored.

memo

 

Is it possible, some iron from the bolts is getting into your electrolyte? Iron chlorides are brown but could appear yellow if diluted.

 

WSM

Edited May 12, 2016 by WSM

[MadMat]

From what I've read dichromate is added to a cell with a platinum anode, whereas fluoride is usually used for a lead dioxide anode.

 

Memo, the yellow on the bolts is most likely zinc plating with a yellow chromate conversion coating. This is added for rust protection, and unfortunately, is very easily dissolved in your cells electrolyte. Though it is visually apparent, the actual amount of impurities added should be pretty small.

Edited May 12, 2016 by MadMat

[MadMat]

Hmm, I guess I skimmed through your last post a little too quickly Memo. If your salt was food grade and it said "enhanced" on the label, it might be iodized salt. Potassium iodide is usually added to salt and it is colorless, but in an electrolytic cell, iodine might have been liberated. One way of testing it would be to take a small sample of your electrolyte and add a bit of corn starch to it. If the yellowish color turns dark (kind of bluish) iodine is present.

[OldMarine]

I've kept up with this thread since I've been on the forum and though I realize you all are doing it for the sake of doing it, I have to ask what the product will end up costing after the initial investment?

[MadMat]

Hmm, I haven't invested much in the way of money at all, just time. Almost all of my materials I had laying around (I live on a farm and there is a LOT of old things laying around).

[OldMarine]

Exotic metal anodes/ cathodes aren't generally lying about!

[Mumbles]

Thinking about economics takes all the fun out of hobbies.

[OldMarine]

Thinking about economics takes all the fun out of hobbies.

 

Oh believe it, I know! My brother was looking through my pyro receipt box the other day and said "Damn, I know why you're still single boy!"

Cheap perc would be very good though. More money for tools and the exotic chems etc..

[WSM]

I've kept up with this thread since I've been on the forum and though I realize you all are doing it for the sake of doing it, I have to ask what the product will end up costing after the initial investment?

I believe the cost is about $0.50 to $0.60 per pound for chlorate and maybe $0.90 to $1.10 for perchlorate (plus all the work). It depends on the rate the power company charges per kilowatt-hour where your cell is run.

 

WSM

[WSM]

Thinking about economics takes all the fun out of hobbies.

 

Oh, I don't know. When you compare the real cost of your home grown oxidizers to what some pyro supply companies charge, you can start to feel really good.

 

WSM

Edited May 12, 2016 by WSM

[schroedinger]

Oh, I don't know. When you compare the real cost of your home grown oxidizers to what some pyro supply companies charge, you can start to feel really good.

WSM

I did calculte that once, about 30% for chlorate (energy is expensive here, 60% eff., bought mmo anode), or in other words (chlorate 6 €/kg) 4 € saved/kg means that after 28 kg the cell has paid itself (cost for cell was 60 €, 5 kg of Chloride + chloride and energy). After that it gets better, since all replacement cost are cheap. Anodes ~15 € cathodes 5 € + chloride and energy. That was two years ago, now chlorate got much more expensive and will vanish mid of year.

[WSM]

I did calculte that once, about 30% for chlorate (energy is expensive here, 60% eff., bought mmo anode), or in other words (chlorate 6 €/kg) 4 € saved/kg means that after 28 kg the cell has paid itself (cost for cell was 60 €, 5 kg of Chloride + chloride and energy). After that it gets better, since all replacement cost are cheap. Anodes ~15 € cathodes 5 € + chloride and energy. That was two years ago, now chlorate got much more expensive and will vanish mid of year.

 

At that point, it'll be priceless .

 

WSM

[MadMat]

This is very frustrating, a few days ago, I found a research paper online concerning the formation of beta lead dioxide on a solid lead substrate. During my initial quick look over the paper, I saw that this paper gave parameters for an alkaline electrolyte solution. Unfortunately, I didn't save the link and now I can't find the damned site!!! I think this paper could have possibly given me exactly what I am looking for

I can't remember the chemicals involved, but I do remember thinking that they were neither expensive or hard to acquire.

Edited May 12, 2016 by MadMat

[Kevin]

Did you check your browser history? I would think it should be in there.

[WSM]

This is very frustrating, a few days ago, I found a research paper online concerning the formation of beta lead dioxide on a solid lead substrate. During my initial quick look over the paper, I saw that this paper gave parameters for an alkaline electrolyte solution. Unfortunately, I didn't save the link and now I can't find the damned site!!! I think this paper could have possibly given me exactly what I am looking for

I can't remember the chemicals involved, but I do remember thinking that they were neither expensive or hard to acquire.

 

This sort of thing can drive you nuts.

 

I hope you find it. If you do, please share the link (Thanks).

 

WSM

[MadMat]

Being a published research paper it's quite possible that it simply isn't up anymore

I've tried a number of times to find it with no success

[BlueComet24]

Try looking at your browser history and maybe you'll find the site. Ctrl+H is the shortcut in most browsers to view your history.

 

Edit: Oops, I missed Kevin's post.

Edited May 12, 2016 by BlueComet24

[Mumbles]

Published research papers should be available essentially in perpetuity. If you think you find it, but just don't have access, let me know. I have journal access through my University.

[MadMat]

I've been checking through my browser history, but I found the site through a search and the history doesn't contain the sites visited just the original search. There are hundreds of searches I have to go through! I did go to a link that I thought might possibly be the one, but my comp timed out and didn't link to the site grrrrrr.

[WSM]

I finally got around to testing my brine, and sadly yes, it's contaminated with calcium and magnesium as indicated by a flocculant precipitate when 1M sodium carbonate (Na₂CO₃) plus a little 3M sodium hydroxide (NaOH) were added to it.

 

 

Now I need to decide whether to purify the brine before use or ignore the contaminants and run the cell anyway (as a friend and fellow electrochemist recommended).

 

?!?!?!!!

 

WSM

Edited May 13, 2016 by WSM

[WSM]

Now I need to decide whether to purify the brine before use or ignore the contaminants and run the cell anyway (as a friend and fellow electrochemist recommended).

WSM

 

Okay, I've slept on it and I've decided I'll treat the brine I've made up with sodium carbonate and hydroxide to remove the calcium and magnesium contamination.

 

Na₂CO₃ + CaCl₂ → CaCO₃↓ + 2NaCl

 

2NaOH + MgCl₂ → Mg(OH)₂↓ + 2NaCl

 

After the calcium and magnesium contaminants drop out of solution, a vacuum filtration step should remove them and leave a reasonably pure sodium chloride solution.

 

These steps should go a long way toward making pure sodium chlorate.

 

The next step is charging the RC with electrolyte and running the sodium cell. (Finally!)

 

WSM

Edited May 13, 2016 by WSM

[MadMat]

When adding the NaOH, don't go too high with the Ph or you will actually start to redissolve the metal hydroxide. A Maximum of 9 should be sufficient. (High Ph water treatment is a standard waste treatment for removing metals)

Edited May 13, 2016 by MadMat

[taiwanluthiers]

I don't know if it's this one, but I saved this site on my own domain (it's hard to find and the original host is slow or down)

 

http://oxidizing.typhoonguitars.com/

 

Here is the page concerning lead dioxide anodes

 

http://oxidizing.typhoonguitars.com/chlorate/leaddiox/leaddioxide.html

Edited May 13, 2016 by taiwanluthiers

[MadMat]

Nope, that's not it. I have read that one though. Thanks for trying though. The file I'm looking for is a research paper. It is a PDF. I don't know the URL, but it likely ends in a .edu. I'm still pouring over a mile of history in my comp. Persistence may pay off, but it sure is a pain in the ass.

Edited May 13, 2016 by MadMat