making potassium (per) chlorate

[tentacles]

It's not a big deal, hashashan; this was just an anode to test out my method more than anything else; I was never actually planning on using this one in a cell. Once I've played with it I'm going to crunch it up and grind the bits up to use making a better anode (again with the NC lacquer over fiber cloth).

 

Still, it's good to know not to interrupt it in the future. I've found a local place where I may be able to get litharge, hopefully the price is reasonable.

[hashashan]

Also an important note :

Its a bitch t connect the anode. You cant just use copper or iron and stuff.

you need a metal with a conductive oxide or the oxide itself. I use silver.

you can use Pt,Ag,Fe3O4...

[tentacles]

I plan on trying the silver electroplating process on the geocities chlorate site - I've made some silver nitrate and rochelle salt and have some ammonia. All I need to do my plating is some damned PH strips.

[NightHawkInLight]

So here is a question I've had.

 

If you make sodium chlorate as a precursor to KClO3 and use both a steel anode and cathode, will it still produce the chlorate? I have some going right now with steel and as expected my rod is being eaten away. What I am planning on trying is filtering the rust out of the solution before turning it all into KClO3. I have uses for the rust also so I figured why not make both at once? Anyone have an idea if I'll end up with some NaClO3 or if I'm just going to be getting my rust?

[tentacles]

Steel will not work as an anode for chlorate or perchlorate production. Magnetite makes a good chlorate anode, or graphite, or several others.

 

All you're getting is red iron oxide, which is still a useful pyro chemical.

[tentacles]

Update, was playing with the silver plating and copper plating today - it worked quite well. I made 300ml/60ml of the plating solution listed on the geocities pages (formula to follow). Plated with a copper sulfate/sulfuric acid bath - I just dumped some CuSO4 and a dash of H2SO4 in a beaker with about 300ml of water in it.

 

Pic - I cut off the part of the anode that I did not originally plate (that wasn't submerged in the plating bath). That is the end that I plated with silver then copper. The splotchy look is because it is still damp after rinsing it.

 

http://www.apcforum.net/files/DCP_2499.JPG

 

The silver plating bath I used was:

 

Part A:

300ml water (tap)

3.0g Ag(NO3)2

10 drops NH4OH (household ~7%)

 

Part B:

.2g Ag(NO3)2

.166g Rochelle salt (I actually used .2g)

100ml water (tap)

 

The part A solution is very simple - mix and then filter.

Part B is prepared by dissolving the Ag(NO3)2 in 10ml water and then adding the remaining 90ml as boiling water, then add the Rochelle salt. Boil for 20 minutes and then combine the two in the plating tank. Technically by the patent's proportions I should have used only 58.6ml of my part B solution but it doesn't seem to have hurt anything that I used more.

 

The patent says to plate at 2.5A but having not researched deeply, I just fed it some current - about 450mA until the solution turned from reddish brown to mostly clear. I got some black scum at the cathode (which is the PbO2 being plated), most likely from using sterling silver as the plating anode.

 

Despite having said I wasn't going to try this anode in a cell, I may just try it anyways for the hell of it.

 

Edit: the plated on copper can be soldered to - you would think this is obvious, but I was not sure if the lead dioxide would decompose at the temperature required.

[NightHawkInLight]

Steel will not work as an anode for chlorate or perchlorate production. Magnetite makes a good chlorate anode, or graphite, or several others.

 

All you're getting is red iron oxide, which is still a useful pyro chemical.

So even with replacement of the anode every time it rusts out, I cannot expect to have any NaClO3 in the solution after all is said and done? I was under the impression that the chlorate would still be produced with a low quality anode, it would just be very contaminated with the oxides created. Is all the energy put into corroding the anode instead of being used to form the chlorate?

I have always thought that the only reason that steel anodes cannot be used was because they would get destroyed, not because they stop production. I do not see why that would be. Please enlighten me if possible. At least like you said, I will be getting my iron oxide. I have a whole five gallon bucket full of Al turnings that may soon have a purpose...

[tentacles]

It has to do with the oxygen potential of the material - if the potential isn't high enough, the anode just produces oxygen gas. A common material that WILL produce chlorates and possibly perchlorates is lead, but it will erode from the start and you'll have some messy nasty crap in your cell.

 

Aluminum also won't work, as it will form the oxide (anodize) which is non conductive. It'll probably erode and make a mess too.

 

Not every material can make chlorate, much less perchlorate, this is why there is so much interest around the lead dioxide anodes, they can operate for a long time with little erosion even when making perchlorate from chloride. And obviously, lead dioxide is cheaper to make than platinum, which has the problem of eroding significantly when making perchlorate from chloride.

[BPinthemorning]

I am running a chlorate cell for the first time, and I am getting a large amount of carbon deposit in the mother laqure. How should I go about removing this before I get my sodium chlorate? I have been looking everywhere for the past 5 days that the cell has been running. Please help me!!!

[WarezWally]

Let it settle on the bottom and decant the liquid off the top

[hashashan]

Just filter it. whats the big deal?

[BPinthemorning]

I like warez's idea, but is the common coffee filter enugh to get carbon out of the liquid?

[Mumbles]

If some gets through, you can run it through again and the bed of trapped carbon/gunk will be able to better filter it. A coffee filter shold in general be fine.

[BPinthemorning]

Then I take the filltered liquid, ad more NaCl and put it back in the cell to run agian?

[WarezWally]

Has anyone tried pressing lead dioxide powder into a anode? I imagine with a 50t press it would be pretty hard and aslong as you don't drop it it should hold together. Connecting it to your supply may be difficult but you could always rig something up with platinum plated wire or something else that wont deteriorate (Magnetite?)

[tentacles]

warezwally: you'd need to use a binder - I used NC successfully when I pasted on the PbO2. There was a patent somewhere - it's the patent referenced on the "chlorates and perchlorates" site under the silver electroplating. The patent describes like 10 different pressed PbO2 composite anodes. The patent describes a process that is basically just injection molding them. Then they use these as a substrate to plate PbO2 over top. I think they may have described making some using just beta-PbO2 pressed but that once it erodes some, they become problematic. (because the PbO2 erodes and the plastic binder does not)

[WarezWally]

So it wouldn't hold together at all?

 

Has anyone tried mixing lead dioxide with conductive epoxy?

 

I was thinking of using that to coat a titanium sheet, still tracking down some lead dioxide powder.

[tentacles]

wally, did you read my post? the patent is at: http://v3.espacenet.com/textdoc?DB=EPODOC&IDX=US3318794&F=0

 

A whole stick of information on making pressed lead dioxide anodes.

 

"As an anode for oxidation electrolysis and having corrosion resistance, the inventors have suggested several production processes having comparatively thin layers of lead dioxide coating upon a pressure-hot-holded electrode body composed of powdered lead dioxidein a press-mold, in which one or more kinds of thermoplastic resin or thermosetting plastic resin and pretreated lead dioxide powder will be molded into an electrode under pressure at elevated temperatures."

 

I would suggest that, you COULD make one and use it without plating on PbO2, but I really doubt it would last long at all. If it were possible to make one without plating on PbO2, I would presume there would be a patent would be for that method.

[WarezWally]

I see, that leaves my epoxy method. I finally got a quote for some lead dioxide and its not cheap ($40 for 500gm) where as manganese dioxide is $6 a kilo and should also work (according to a few sites and patents)

 

There is very little information on it

[tentacles]

If you try the MnO2, let everyone know how it works (or doesn't). There is very little information on it, yet it's very easy to obtain (pottery shops) and plating it is almost exactly the same as the PbO2. (Mn(NO3)2 bath)

[BPinthemorning]

Some one needs to get a lead dioxide method down, and sell them to other enthusiests... Just an idea... But if anyone can...

[WarezWally]

I was considering a bulk buy of commercial TSLD anodes from India but i never heard back from the place. Shame as if the price was ok (under $60 for a 10x5 anode) im sure people would have purchased them.

[tentacles]

I went ahead and setup a test cell on my bench using my 4L beaker (2L H2O, ~650g NaCl). I used ~18 ft of .028" Ti wire for the cathode, bent into 4 spring shapes. Only about an inch of the anode - 3x4.5cm or so - is in the water. I covered the silver/copper/solder plated area with a thick paste of ping pong lacquer to help protect from the electrolyte. I have my thermometer in the bath, and I am hanging the anode by it's wire. I covered the top of the beaker with many pieces of glad wrap, it's far from sealed but it really helps keep the Cl2 in the jar.

 

The Ti wires REALLY electrolyze a lot of H out - it fizzes like crazy at 2.2A, and it's positively foamy at 5.5A.

 

The powdered PbO2 began eroding immediately once the cell was powered on; the plated stuff is holding up so far (~1h).

 

pic:

http://www.apcforum.net/files/DCP_2506.JPG

 

http://www.apcforum.net/files/DCP_2508.JPG

 

 

edit: I put my 12V 10A power supply on it today instead of the battery charger; it's drawing 11.5A now. My DMM shows it's actually outputting 6.5V at the 11.5A load.

 

I need to get some methylene blue to test for perchlorate, to better time my cell runs.

 

Still no obvious erosion of the plated PbO2 - despite interrupting the plating process.

 

more edit: Methylene blue is available at pet shops as a medication for fish.

[WarezWally]

Looking good

 

Wanna sell me one

[tentacles]

Looking good

 

Wanna sell me one

If this one works out, and I can get my hands on some lead oxide, I may make a couple to sell or give to sites or something. I have some Ti sheet on the way so I can make them like hashashan does. Growing the plating layer through the substrate is rather brilliant. And if you are making several, no reason you can't plate one on each side of the sheet.