making potassium (per) chlorate

[WSM]

I couldn't work on my system yesterday due to a planned medical exam which kept me busy all day.

 

That's over now and after work today, I hope to disassemble, clean out and reassemble my brine tank and fill it with the purified brine which I can then easily move to the cell by pump. After that's set up, I'll continue to filter the rest of the brine (now in 5 gallon buckets) and add it to the cleaned out brine tank as well.

 

If that's done I think I can start the cell run and get the precursors going. I'm still considering a solid salt chamber for the cell to help concentrate the sodium chloride solution within the tank. It seems like it should work, and may help expedite the production of sodium chlorate crystals.

 

There's much more to this, but I expect it will be more clear as I run it and add my own observations to the current body of knowledge.

 

More to come...

 

WSM

Edited May 18, 2016 by WSM

[memo]

Guillermo -William

Memo - bill

 

all the same, just different languages

 

 

memo

[Rkteer]

WSM

 

Thank-you! I actually saw and purchased one yesterday! I had sim saved as a seller but he hasn't had any on for a little while.

 

Thanks :)will let you know how I go.

 

EDIT; accidentally hit post

Edited May 18, 2016 by Rkteer

[WSM]

Guillermo -William

Memo - bill

all the same, just different languages

memo

Si!

 

WSM

Edited May 18, 2016 by WSM

[schroedinger]

Hi schoedinger,

 

I have no delusions about this being easy. I expect I'll have to take extra measures to make a success of this, but I'm learning and will share what I learn here, Yes I do have a copy (or ten) of the geocities site and refer to them and several others as I study the topic. I also have the means (and will) to apply stirring to the cell when called for.

 

I intend to solve one problem at a time as I encounter them.

 

Thanks for the encouragement.

 

WSM

No worries you will make it work, it's not that hard. I just mentioned the stirring, because that was what helped me with my cell. I used a normal lab stirred and a magnetic stir bar (just enough stirring to have a light movement in the cell). I added new sodium chloride as solids, when the chloride was below 150g/l (tested with silver nitrate). After 14 days i could harvest 200g (recrystalized once, chloride ~1%) of chlorate, which was quite equal to the ammount my pottasium cell would produce (5l cell volume, so ~3.4 kg of chlorate was estimated to be in solution, with chloride @ 92g/l). After that i harvested the liquor with KCl and got 3.3 kg of pottasium chlorate after recrystallisation. What I forgot is to check how much chlorate was in the liquor from recrystallisation of the sodium chlorate. I just mixed into the cell liquor before adding KCl.

[memo]

here are a couple of photos ,

 

[

Edited May 18, 2016 by memo

[memo]

i went ahead and finished up the first run just to see what I would get . I did it in 2 batches because limit glass ware. I did 1500 ml per batch. the first one got the majority of the brown junk. the second batch was pretty clear. I washed them both in cold water. a lot of cold water. do you think the brown stained part will be any good ?? I don't know the yield yet. its in the dry box.

 

[

[schroedinger]

Memo i can't find with what you started your cell (pottasium or sodium chloride).

The brown batch should be easy to refine.

There are basically two things to try out.

Take a sample, add some water and heat.

Now if the brown stuff stays as solid particles you can filter 'em out.

If they dissolve, you will need to recristallize to get rid of them.mDue to the low solubility of pottasium chlorate it will better suited for this.

[memo]

i started out with sodium chloride. 7 day run time then combined with potassium chloride. I think the brown color is from the bolts that hold the connectors in place. I covered them in epoxy to try and stop the staining.

 

memo

[schroedinger]

Ok, the the brown stuff will be rust. Just dissolve in hot water and filter. Epoxi doesn't hold up to a chlorate cell. Use pvc cement or pvc in THF for that.

[WSM]

That's over now and after work today, I hope to disassemble, clean out and reassemble my brine tank and fill it with the purified brine which I can then easily move to the cell by pump. After that's set up, I'll continue to filter the rest of the brine (now in 5 gallon buckets) and add it to the cleaned out brine tank as well.

If that's done I think I can start the cell run and get the precursors going.

WSM

I actually did disassemble, clean out and reassemble the brine tank. Then I used the vacuum filtration setup and purified the electrolyte (removed the solids which dropped out) and poured it back into the clean brine tank. I checked the pH and it was between 5-6, but I figured since the cell runs alkaline anyway, it should self-correct as it runs.

 

I then changed the valving and tried to pump the clean brine into the cell, but the second pump didn't work. I gravity fed some of the brine, but only got so far. Next I cleared the pump and opened it up. The impeller shaft was stuck from sitting too long. After I manually freed it and reassembled the pump, it worked like a champ and filled the cell very quickly.

 

It was about 20:00 (8:00 PM) and everything seemed ready so I fired up the power supply and the cell started to get cloudy right away (plus a chlorine smell) so it looked good.

 

I put together a single display box with a combination volt/amp meter plus the temperature meter, all fed from the same 12 Vdc power supply. This didn't work as planned. The volt meter was fine but the ammeter displayed -131 amps (but the power supply limit is 55 amps). Also the temperature meter seemed a bit wonky. I suppose unless I add a power filter to isolate the ammeter from the volt meter, it's not going to work right.

 

Till I get around to redesigning the single display, I'm using a separate ammeter display. The cell is running at 4.8 Vdc and about 31 Amps, and roughly 25^oC so far. I'll check it again in the morning.

 

I'll let this hodge-podge setup run till the chloride is mostly converted to precursors and then go from there. There's plenty to do to clean up and refine this system, but I'll make the effort later.

 

WSM

Edited May 19, 2016 by WSM

[WSM]

This morning I checked the system. The meters read:

 

4.6 Vdc

46.7 Amps

47 degrees C

 

I also checked the temperature of the tubular titanium leads going into the cell (to the electrodes) and they were 35^oC and 40^oC, respectively.

 

The electrolyte level hasn't dropped much yet, but it's still early in the run.

 

I'll take a closer look this evening and report.

 

WSM

Edited May 19, 2016 by WSM

[memo]

The brown stained came out good. the total weight for the first run was only 255g pretty poor. it is 255 grams more than I thought I would get. the second run is on day 3 it is running at 5 volts 43 amps and it is hot to the touch, so hopes are high.

 

memo

[Arthur]

WSM

if you can track the pH change with respect to amp hours then you should be able to plot how much the pH changes and program a small iwaki pump to feed acid in to keep the cell pH within range. A standard iwaki bellows pump should handle 10% HCl easily and this should be safer than having conc acid about.

[WSM]

WSM

if you can track the pH change with respect to amp hours then you should be able to plot how much the pH changes and program a small iwaki pump to feed acid in to keep the cell pH within range. A standard iwaki bellows pump should handle 10% HCl easily and this should be safer than having conc acid about.

 

Those are good suggestions, and I'm fully equipped to implement them. But my initial runs are planned to be without pH control, to establish a baseline.

 

Subsequent runs will incorporate pH control, using a gravity-fed system similar to the one Swede developed years ago (accurate timer, PTFE valve and PTFE needle valve).

 

I'll show photos of the setup later.

 

WSM

[memo]

wsm ask for photos, i got photos, how about some feed back ?

 

memo

[WSM]

wsm ask for photos, i got photos, how about some feed back ?

memo

 

It looks like it works.

 

I forgot to ask what type of anode you're using?

 

I was also curious why you start with sodium chloride if your goal is potassium chlorate? Why not electrolyze potassium chloride solution?

 

Thanks for posting the photos.

 

WSM

[memo]

pt. on ti for the anode. I choose this method to make potassium perchlorate. I will try later using just the potassium chloride.

 

memo

[taiwanluthiers]

Those pt/ti anode seems to be the only option anyways unless someone makes and sells a LD anode. Probably a lot easier to buy perchlorate than to try to find LD or make one.

[memo]

cant buy it here , or ship it in. don't ask me how I know ~

 

memo

[WSM]

pt. on ti for the anode. I choose this method to make potassium perchlorate. I will try later using just the potassium chloride.

memo

I save my platinized titanium anodes (Lead Dioxide anodes, too) for the perchlorate process.

 

MMO works wonderfully for the chlorate process. I'm also partial to CP titanium for the cathodes, though cathodic protection helps protect most materials used for cathodes (even plain iron).

 

Do you have access to MMO? There are sources on eBay that offer worldwide delivery.

 

WSM

Edited May 21, 2016 by WSM

[dagabu]

Nice write up in the bulletin WSM!

 

Did you ever finish the all in one bucket design?

[memo]

the anode is TI coated with PT and a stainless cathode

[WSM]

Nice write up in the bulletin WSM!

Did you ever finish the all in one bucket design?

Thanks, dagabu. I'm glad you like them.

 

By "all in one bucket design", do you mean bucket cell, as we call it? I built one for pyrojig which worked but needs the electrode leads to be modified. The smaller diameter leads on the first setup overheated, so I have a collection of parts assembled to build a new set of electrodes with larger diameter, copper filled titanium leads. We expect the change will allow cooler running and a hardier setup.

 

WSM

Edited May 21, 2016 by WSM

[dagabu]

Yupper!