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making potassium (per) chlorate


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Posted
A coffee maker has a hot plate, pyrex container, and a "filtration apparatus". All three can be considered labware, which they are somewhat strict about in texas.
Posted

Once i get a pool chlorinator cell, ill use its titanium rods and whatever those rods connect onto the anode mesh, to build a second electrode set for my cell. I have quite a few 150mm pvc screw cap lids laying about the place, i never noticed this until after i began to search B)

 

I just wish the pool shop would get some broken ones in soon.....

Posted

Once i get a pool chlorinator cell, ill use its titanium rods and whatever those rods connect onto the anode mesh, to build a second electrode set for my cell. I have quite a few 150mm pvc screw cap lids laying about the place, i never noticed this until after i began to search B)

I just wish the pool shop would get some broken ones in soon.....

 

Since you're coming into the Summer season, some folks may find their system didn't weather the Winter very well. Be patient, they'll come...(and good luck!)

 

WSM B)

Posted

@WSM Im interested...glare.gif . I'd love to get one going. It is a neat design for sure. I think it could be something that others may want.

 

I'll look into it. I have a friend with a plastics router that is willing to do custom work, but he says cutting thick PVC might be more challenging to cut (due to it's nature and cutting characteristics) than the acrylic he usually works with. We'll see...

 

WSM B)

Posted

I'll look into it. I have a friend with a plastics router that is willing to do custom work, but he says cutting thick PVC might be more challenging to cut (due to it's nature and cutting characteristics) than the acrylic he usually works with. We'll see...

 

WSM B)

 

There is a Racer of Vintage motorcycles that may be able to help get your PVC cut. Just sayin... ;)

 

-dag

Posted (edited)

There is a Racer of Vintage motorcycles that may be able to help get your PVC cut. Just sayin... ;)

 

-dag

 

That's true. I can always try him also. Thanks for the suggestion.

 

WSM B)

Edited by WSM
  • 2 weeks later...
Posted

I was designing the extra equipment in the heat-well portion of the CC and figured the fluid would cool before it reached the RC, resulting in crystals forming in there and jamming the line. To address that problem, I've come up with a simple plan involving a separate heated water tank and a closed loop heat exchanger to keep the liquid between the CC and the RC fluid and moving.

 

Heat Exchanger Diagram.pdf

 

The idea came to me a few days ago and I've siezed upon it to solve the potential problem of crystal fouling of the line between the two parts of the continuous system.

 

WSM B)

Posted

Looking at your plans it looks like it will work quite well. The line that runs the solution thru the heating medium will not lose heat but will instead gain heat, therefore you can use a pvc pipe to transfer the fluid between the two tanks. (One being I believe is where the eletrodes are located at and the other where you wish to crystal out the chorates. )

What the problem was for the tube in the past was the heat lose would causes the pipe to clod with crystals and I know that you know this as well. But you solve this with the heated water surrounding the transfer pipe.

Posted (edited)

Thats clever .. LOL reminds me of a distillation setup except your heating the tube v.s. cooling .

Its almost a shame that you couldnt utilize some passive heat from the cell.Somehow to do the work the closed circuit pump has to do. Steal heat from the PS or something else that radiates heat, maybe passed through/ around the transfer pipe as kind of a heat sink . ( "kills two birds with one stone" idea)

Edited by pyrojig
Posted
I haven't read through all 87 pages, but where do you purchase really cheap potassium chloride in large quantities?
Posted
In the USA KCl is available in large bags for a low sodium method of regenerating water softeners. So far in Europe I have not seen KCl other than expensive high purity lab grade product.
Posted

Looking at your plans it looks like it will work quite well. The line that runs the solution thru the heating medium will not lose heat but will instead gain heat, therefore you can use a pvc pipe to transfer the fluid between the two tanks. (One being I believe is where the eletrodes are located at and the other where you wish to crystal out the chorates. )

What the problem was for the tube in the past was the heat lose would causes the pipe to clod with crystals and I know that you know this as well. But you solve this with the heated water surrounding the transfer pipe.

 

Hi patsroom,

 

I think it'll work well, too. Thanks for the vote of confidence :D .

 

WSM B)

Posted

Thats clever .. LOL reminds me of a distillation setup except your heating the tube v.s. cooling .

Its almost a shame that you couldnt utilize some passive heat from the cell.Somehow to do the work the closed circuit pump has to do. Steal heat from the PS or something else that radiates heat, maybe passed through/ around the transfer pipe as kind of a heat sink . ( "kills two birds with one stone" idea)

 

Thanks pyrojig. I believe that's where the inspiration came from. In fact, there's no reason this arrangement wouldn't work as a condenser for a distillation setup (except most people want to see what's going on in there). I tried to think of a way to use the RC's heat but can't think of a way without dropping out crystals where I don't want them :blink: :angry:. Some brilliant idea may come up in the future to utilize otherwise wasted heat to accomplish this task, but for now I think this will do.

 

WSM B)

Posted

I haven't read through all 87 pages, but where do you purchase really cheap potassium chloride in large quantities?

 

It was fairly cheap a few years ago but everything is getting more expensive these days, unfortunately. Where available, it costs about 2 to 2.5 times what we paid about 5 years ago (very dissappointing).

 

WSM B)

Posted

In the USA KCl is available in large bags for a low sodium method of regenerating water softeners. So far in Europe I have not seen KCl other than expensive high purity lab grade product.

 

Absolutely true.

 

At the local "Big Box Home Center", large nuggets of KCl are available in plastic 40 lb bags (for low sodium water softener salt) for about $17 US before taxes. I used to pay about $7 for the same bag, not too many years ago. Oh well, cest la vie :rolleyes:.

 

I've heard it's available from farm chemical suppliers, but the purity is less than desireable. The agricultural grade KCl could always be purified by recrystallization before use in the cell. Didn't someone mention it being available in Eastern Europe?!

 

WSM B)

Posted

Thats clever .. LOL reminds me of a distillation setup except your heating the tube v.s. cooling .

Its almost a shame that you couldnt utilize some passive heat from the cell.Somehow to do the work the closed circuit pump has to do. Steal heat from the PS or something else that radiates heat, maybe passed through/ around the transfer pipe as kind of a heat sink . ( "kills two birds with one stone" idea)

 

Well, first of all, if your PS is running that hot I imagine it won't last long :( (unless this idea is used to work for both... Hmm, not bad! I'll have to store that idea for later ;) :P). Now if you use a Peltier junction to cool the crystallizer, the other side is heating and we could use that heat to do the job. Unfortunately, I'm trying to use passive and not active cooling for my crystallizer chamber (so no Peltier junction use).

 

I do like the idea af adding a small radiator to the heating circuit (for the heat source input). I had thought of using a similar setup to cool the CC actively (with a fan across the radiator) instead of passively but want to try the passive method first.

 

Thanks for the input. You never know where your inspiration will come from. One day, one of these thought nuggets will surface as the perfect fix to a troubling problem :D.

 

WSM B)

Posted

Thats clever .. LOL reminds me of a distillation setup except your heating the tube v.s. cooling .

Its almost a shame that you couldnt utilize some passive heat from the cell.Somehow to do the work the closed circuit pump has to do. Steal heat from the PS or something else that radiates heat, maybe passed through/ around the transfer pipe as kind of a heat sink . ("kills two birds with one stone" idea)

 

That brings up another thought. I wonder if I should use my KCl replenishing solution to warm the heat exchanger instead of plain water. A secondary advantage would be adding warmed solution to the RC instead of cold. I'll have to consider that...

 

Thanks, again :).

 

WSM B)

Posted

That brings up another thought. I wonder if I should use my KCl replenishing solution to warm the heat exchanger instead of plain water. A secondary advantage would be adding warmed solution to the RC instead of cold. I'll have to consider that...

 

Thanks, again :).

 

WSM B)

[/quote

 

 

 

I just like to be resourceful with the energy of a sys. It just feels better to know you can pull double duty by recycling what would have been wasted energy in the first place. I hope that your able to implement some of these nuggets into your CC . I hope your design can inspire others to create a simple yet productive CC( as well as myself!!) for a work-horse of a machine!! Now the big thing beyond that is to make it pull double duty again and make PERCH...!!!

 

 

Posted (edited)

What is the fluffy stuff in my recrystallization process? I am about to recrystallize a batch of chlorate and there seems to be tiny particles of fluffy stuff in the boiling solution. They seem to dissolve when the temps hit 90 degrees Celsius and I haven't noticed anything like that before.

 

Edit: Added a picture of the lyte. The particles (on the bottom here) appeared as soon as the temp went below 90 degrees Celsius after being boiled for 15 minutes.

 

Edit #2: I just took a look at my electrodes and there's some kind of substance on the anode that I've also not seen before.

 

Any clues?

post-10776-0-58527900-1323895792_thumb.jpg

post-10776-0-54062000-1323898312_thumb.jpg

Edited by athlon
Posted

What is the fluffy stuff in my recrystallization process? I am about to recrystallize a batch of chlorate and there seems to be tiny particles of fluffy stuff in the boiling solution. They seem to dissolve when the temps hit 90 degrees Celsius and I haven't noticed anything like that before.

Edit: Added a picture of the lyte. The particles (on the bottom here) appeared as soon as the temp went below 90 degrees Celsius after being boiled for 15 minutes.

Edit #2: I just took a look at my electrodes and there's some kind of substance on the anode that I've also not seen before.

Any clues?

 

Hi athlon,

 

Can you tell us more about your cell and setup? There isn't enough to go on yet. It looks like there may be some sort of contaminant in there, but can't tell what it is without more information.

 

WSM B)

Posted

What is the fluffy stuff in my recrystallization process? I am about to recrystallize a batch of chlorate and there seems to be tiny particles of fluffy stuff in the boiling solution. They seem to dissolve when the temps hit 90 degrees Celsius and I haven't noticed anything like that before.

 

Edit: Added a picture of the lyte. The particles (on the bottom here) appeared as soon as the temp went below 90 degrees Celsius after being boiled for 15 minutes.

 

Edit #2: I just took a look at my electrodes and there's some kind of substance on the anode that I've also not seen before.

 

Any clues?

 

 

This could be the "white smut" referred to by Swede in his blogs. No idea what it is...maybe from your water(?) I've had it on the electrodes, but after a good washing (of the crystals), never noticed any when recrystallizing.

 

When you dissolve to recrystallize, filter the solution -coffee filters will work well, and see if you have any contamination. It could also be from the KCl used.

Posted

I'm still using my 2 litre cell with consumer grade mineral salt 66% KCl and 33% NaCl as it's the only KCl salt that I can get around here.

The cell with recycled and replenished electrolyte was run for 990 Ah, (4,6V ~15A) and when I reach about 1000Ah the current starts to go down, this time it pulled 12,6A when I decided to harvest and I noticed there was a lot more on the bottom this time.

 

When I filtered the electrolyte the filter clogged almost immediately and it took ages for it to go through.

I also noticed that the precipitate at the bottom layer was rock hard and I had to break it loose from the bucket.

My electrodes usually get clean by washing in hot tap water, but not this time.

Posted

What is the fluffy stuff in my recrystallization process? I am about to recrystallize a batch of chlorate and there seems to be tiny particles of fluffy stuff in the boiling solution. They seem to dissolve when the temps hit 90 degrees Celsius and I haven't noticed anything like that before.

 

Edit: Added a picture of the lyte. The particles (on the bottom here) appeared as soon as the temp went below 90 degrees Celsius after being boiled for 15 minutes.

 

Edit #2: I just took a look at my electrodes and there's some kind of substance on the anode that I've also not seen before.

 

Any clues?

 

I get that too, but as when i add my KCl and dissolve it by heating it. I think its carbonate or bicarbonate. carbonates seem to precipitate as fluff.

It could be form overexposure to carbon dioxide, or any number of things, maybe some rare other stage of chloride/chlorate. all i know is it didnt do anything bad to my chlorate. i got my lab grade chloride sample back from the police when it was seized 7 months ago (seized in domestic dispute at a friends house) after vigorous drug testing of almost every known in the universe. my 100g dropped to 80g.

 

Anyway, the lab grade stuff made no precipitate, and after some burn testing, it is in no way inferior to the what i make from horse feed supplement.

Posted

 

Anyway, the lab grade stuff made no precipitate, and after some burn testing, it is in no way inferior to the what i make from horse feed supplement.

 

Thanks, I'll test the chlorate when it's dry. You also gave me a clue as to where I can find KCl! Have to make some calls I think :)

Posted

I'm still using my 2 litre cell with consumer grade mineral salt 66% KCl and 33% NaCl as it's the only KCl salt that I can get around here.

The cell with recycled and replenished electrolyte was run for 990 Ah, (4,6V ~15A) and when I reach about 1000Ah the current starts to go down, this time it pulled 12,6A when I decided to harvest and I noticed there was a lot more on the bottom this time.

 

When I filtered the electrolyte the filter clogged almost immediately and it took ages for it to go through.

I also noticed that the precipitate at the bottom layer was rock hard and I had to break it loose from the bucket.

My electrodes usually get clean by washing in hot tap water, but not this time.

 

 

How do you seperate the potassium chlorate from the sodium chlorate using a mixed salt as feedstock?

 

Filters clogging is expected if you have a lot of (carbonate?) contamination. You might want to try and devise a buchner funnel setup. I have one that uses a shop vac for suction.I cut the top out of a 20l pail to fit a plastic strainer, and siliconed it in. I added another hole for the shop vac to attach with a pipe extending down into the bucket. I use coffee filters for filtration.

Do you wash your chlorate after scooping out? Using a 100 or 200 mesh screen should help take away a lot of the crap. The water could then be filtered and reused if you want later.

 

As for the electroode, try cleaning with HCl.

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