Jump to content
APC Forum

making potassium (per) chlorate


Recommended Posts

Posted

I will contact them today about the anodes I myself was thinking 2"x6". No guarantee but I will try my best and see if it works out. That's all I can do.

 

Wonderful. Were you planning on a co-op purchase or just getting some samples to try?

 

WSM B)

Posted
Coating should be lead dioxide on titanium mesh. I'm asking for a small trial purchase of 15 to 20 in which I will need someone with an active cell to try one out. If all goes well and everything can be worked out with the supplier I will offer here first. Like I said this is to get no ones hopes up. May fall through too many variables right now.
Posted

I haven't found a new fuse for the power supply yet but the new one I ordered came today.

I refilled the cell with saturated sodium chloride solution and started it up. It has been running fine for two hours now. I plan on running it for 40 hours and adding more sodium chloride again then repeating the process a few times

Posted

I haven't found a new fuse for the power supply yet but the new one I ordered came today. I refilled the cell with saturated sodium chloride solution and started it up. It has been running fine for two hours now. I plan on running it for 40 hours and adding more sodium chloride again then repeating the process a few times

That's awesome. Keep us up to date on your progress.

 

WSM B)

Posted

Coating should be lead dioxide on titanium mesh. I'm asking for a small trial purchase of 15 to 20 in which I will need someone with an active cell to try one out. If all goes well and everything can be worked out with the supplier I will offer here first. Like I said this is to get no ones hopes up. May fall through too many variables right now.

I'd be happy to try one out. If they come through and work as well as we hope they will, hopefully the price will not be an issue.

 

Thanks for putting forth the effort.

 

WSM B)

Posted (edited)

I haven't found a new fuse for the power supply yet but the new one I ordered came today.

 

Keep an eye out for that size and rating of fuse. It must exist somewhere. If nowhere else, try eBay or some other online store.

 

Please let us know if that fixes it.

 

WSM B)

Edited by WSM
Posted

Coating should be lead dioxide on titanium mesh. I'm asking for a small trial purchase of 15 to 20 in which I will need someone with an active cell to try one out. If all goes well and everything can be worked out with the supplier I will offer here first. Like I said this is to get no ones hopes up. May fall through too many variables right now.

Try to find out if the lead dioxide is the hard crystalline (beta) form? If it is, plus well made, it should work well for us.

 

WSM B)

Posted
I sent them my requirements. Beta lead dioxide on titanium mesh 50mm x 150mm. Coating .3 to .5 mm thick. I am waiting on a reply for cost. They did ask what kind of solution they would come in contact with and I said hobby perchlorate cells. She said the lead dioxide coating was rated for long life in perchlorate cell and wast water treatment. Like I keep saying not to get anyone's hopes up cost and shipping may become an issue we'll see. I want them to be beneficial to everyone here. I have no idea what the cost will be. What would be a fair price for one of these anodes? And I'm not talking about a we can't get them inflated price! I'm just a pore country boy who has to account for every dollar I spend at the end of the month. I mean a fair price?
Posted (edited)

I sent them my requirements. Beta lead dioxide on titanium mesh 50mm x 150mm. Coating .3 to .5 mm thick. I am waiting on a reply for cost. They did ask what kind of solution they would come in contact with and I said hobby perchlorate cells. She said the lead dioxide coating was rated for long life in perchlorate cell and wast water treatment. Like I keep saying not to get anyone's hopes up cost and shipping may become an issue we'll see. I want them to be beneficial to everyone here. I have no idea what the cost will be. What would be a fair price for one of these anodes? And I'm not talking about a we can't get them inflated price! I'm just a pore country boy who has to account for every dollar I spend at the end of the month. I mean a fair price?

The last time I saw that size LD anode (the same size I used for my sodium perchlorate experiment year), they were asking $30 each or best offer. After I bought several, they've been out of stock. I suppose they had only a limited amount on hand and then either rethought the plan or might have had supplier problems. Who knows?

 

Good luck with your plan. It would be a great thing if one or two of us here could step up and supply LD anodes to the amateur community, so we could supply our own needs for oxidizers.

 

WSM B)

Edited by WSM
Posted
I'm still waiting on a reply to price, I'll keep everyone up to date as it progresses.
Posted

Pick only a moderate size! Most experimenters start small, once you have cracked a small cell it's not hard to make a bigger (current flow) cell using two or more electrodes with alternating Ti electrodes.

Posted

Okay I have run the cell for 30 hours now which should be 60% completion from what I had calculated.

I just went to recharge the cell solution after it had cooled to room temperature. I put the cell solution in a beaker on a stirrer and added about 250 grams of sodium chloride. Only about 100 grams has dissolved..

Shouldn't it be dissolving a whole lot more NaCl because I have converted 60% to sodium chlorate which is twice as soluble??

It is a brand new power supply with brand new electrodes

Posted

How did you calculate your % completion? IMO NO cell without good pH control runs at high current efficiency, and as the chloride is consumed the current efficiency will take a further hit. I'd make (only) a guess that a free running cell never exceeds 60% current efficiency, so probably you have a reasonable process for a chlorate cell with no pH control.

Posted

Pick only a moderate size! Most experimenters start small, once you have cracked a small cell it's not hard to make a bigger (current flow) cell using two or more electrodes with alternating Ti electrodes.

 

 

If you have fixed, small size anodes and want to scale up your setup; ganging them together in parallel will work. The idea of sandwiching anodes and cathodes is used in industry for larger chlor-alkali cells in a more compact setup. There is no reason we can't do this, too.

 

WSM B)

Posted (edited)

I calculated it at 54% current efficiency from this site:

http://www.oocities.org/capecanaveral/campus/5361/chlorate/runtime.html

I calculated run time as 43 hours to convert 86% of 2.25 litres saturated sosium chloride solution.

I have run it for enough time to convert 60% of it and was going to recharge with salt and run again to get the chlorate concentration up

 

We can use the runtime calculators as a rough guide, but there are myriad details to every different setup, that will affect how our cell will perform.

 

The temperature, pH, relative humidity, chemical quality, voltage level and "quality", current levels and stability, and on and on; all plays a role. Don't be discouraged, just keep at it and eventually you'll see results. I ran my first sodium chlorate cell for over six weeks before I began to harvest the chlorate crystals.

 

Potassium chlorate is so much easier, but success with sodium chlorate is possible; just keep at it. Don't worry too much about some undissolved NaCl, just keep going.

 

WSM B)

Edited by WSM
Posted
Okay thanks, I will keep running it. Is there any way to figure out an approxinate run time?
Posted

Okay thanks, I will keep running it. Is there any way to figure out an approxinate run time?

If you meter the voltage and current at the cell, tracking the current level as well as logging the runtime will clue you as to a logical end-of-run using the calculator.

 

That's how I did it and it seems to work okay so far. Good luck.

 

WSM B)

Posted (edited)

With everything else, that runtime calculator is a gem.

 

I was metering the voltage, amperage and temperature; as well as logging the runtime, but struggled with figuring out when to stop the run and start to harvest the product.

 

Between estimating the approximate efficiency and applying the runtime calculator, I finally figured it out.

 

My humblest thanks to whoever figured out how to set up that calculator.

 

WSM B)

Edited by WSM
Posted
Thankyou, so I will go out and purchase a multimeter that will read the volts and amps running through the cell? Is this all I need before continuing again?
Posted (edited)

Thankyou, so I will go out and purchase a multimeter that will read the volts and amps running through the cell? Is this all I need before continuing again?

Some have succeeded in doing that. What I did was purchase an LCD digital DC panel meter from China on eBay. I got a DC ammeter that came with a shunt, so it could meter the high current flow of my power supply to the cell.

 

There are some nice dual panel meters that display both voltage and amperage. I've found them to be accurate in performance and they usually arrive in about 10 days from China.

 

WSM B)

Edited by WSM
Posted

Okay I will put on hold til I get one of them.

Would one like this be fine?

 

http://www.ebay.com.au/itm/like/162083227396?lpid=107&ul_ref=http%253A%252F%252Frover.ebay.com%252Frover%252F1%252F705-139619-5960-0%252F2%253Fmtid%253D1797%2526kwid%253D1%2526crlp%253D40593704497_573061%2526itemid%253D162083227396%2526targetid%253D91828878337%2526rpc%253D0.00%2526rpc_upld_id%253D0%2526device%253Dm%2526mpre%253Dhttp%25253a%25252f%25252fwww.ebay.com.au%25252fitm%25252flike%25252f162083227396%25253flpid%25253d107%252526chn%25253Dps%2526adtype%253Dpla%2526googleloc%253D1000676%2526poi%253D%2526campaignid%253D184043497%2526adgroupid%253D8467825417%2526rlsatarget%253Daud-91737592657%253Apla-91828878337%2526gclid%253DCIOOx52thNACFdWWvQodHk4MvQ%2526srcrot%253D705-139619-5960-0%2526rvr_id%253D1117082699175&lpid=107&chn=ps&ul_ref=http%253A%252F%252Frover.ebay.com%252Frover%252F1%252F705-139619-5960-0%252F2%253Fmtid%253D1797%2526kwid%253D1%2526crlp%253D40593704497_573061%2526itemid%253D162083227396%2526targetid%253D91828878337%2526rpc%253D0.00%2526rpc_upld_id%253D0%2526device%253Dm%2526mpre%253Dhttp%25253a%25252f%25252fwww.ebay.com.au%25252fitm%25252flike%25252f162083227396%25253flpid%25253d107%252526chn%25253Dps%2526adtype%253Dpla%2526googleloc%253D1000676%2526poi%253D%2526campaignid%253D184043497%2526adgroupid%253D8467825417%2526rlsatarget%253Daud-91737592657%253Apla-91828878337%2526gclid%253DCIOOx52thNACFdWWvQodHk4MvQ%2526srcrot%253D705-139619-5960-0%2526rvr_id%253D1117082699175&ul_noapp=true

Posted (edited)

Okay I will put on hold til I get one of them.

Would one like this be fine?

http://www.ebay.com.au/itm/like/

Yes, it should work fine.

 

A few points to be aware of:

  • be sure to get a DC meter
  • In my experience, the LCD meters are easier to see in both daylight and night (LED displays are hard to read in daylight)
  • be careful to wire the meter correctly; reverse wiring can destroy some of these meters (personal experience)
  • some require a separate power source for the ammeter (you may need to isolate the power to the ammeter, i.e., use a different power source from the rest of it) try yours and see how it works
  • protect the panel meter from all moisture, and especially the electrolyte
  • it's useful to mount the meter in a moisture resistant enclosure (I use PVC electrical boxes; see my blogs)
  • be sure to make the electrical connections as close to the cell as possible (not on the power supply) for the most accurate reads of what power is actually getting to the electrodes
Have fun and good luck. You'll be able to monitor your cell's performance easier and understand it's progress better from what you can gather from the meters.

 

LCD temperature meters are nice, too; but the sensor needs to be protected from the electrolyte. Teflon coated sensors are available but can be costly (I've found some on eBay that cost about $10 US each [also from China]). So far, only LED panel meters (that are compatible with them) are available, but perhaps someday they'll make LCD displays for them.

 

If you have any other questions, feel free to ask.

 

WSM B)

 

Edit: These meters aren't required to successfully run a cell, but they are very useful tools to help us optimize our results and measure our progress.

Edited by WSM
Posted

Okay I will put on hold til I get one of them.

Would one like this be fine?

http://www.ebay.com.au/itm/like/

 

After a second look, I think this meter may not be the best. My concern is about the low end of the voltage range (6.5-100 Vdc, probably designed for automotive use). My preference for our cells is a range of 0-10 or more Vdc. The high end doesn't matter as long as the low end will go as low as 0-1 Vdc.

 

I'm using a dual meter which has a range of 0-200 Vdc and 0-200 A, and it works well for the 4-5 Vdc and 0-150 Amps that I'm measuring with it. The current range should be from zero to more than your power supply can output.

 

For example, check out eBay items numbered:

271808226092 (meter) and

271729386459 (shunt)

 

It runs off a 12 Vdc wall wart (plug in power supply) and does a fine job.

 

WSM B)

Posted
Alright here's an update on the lead dioxide anodes. First of all these are 50mmx150mm titanium mesh lead dioxide coated. I do not have the ability to purchase several hundred of these so I would have to purchase a small quantity at a time and the quote of manufacture and ship from china would make these about $50.00 each, more than some would have hoped for. If their is enough people wanting one I would be willing to attempt a purchase only after someone tries a sample. I can get one sample sent to me but at a hefty $95.00 price tag. If it turns out to be a good sample I would like for whomever tests it out to recomp me for what the anodes will cost $50.00 and I will eat the$45.00 loss on the sample. If it's not up to quality I just ask that you send back to me and owe nothing other than shipping back to me. If the product is good I will make a purchase and offer here in small batches. I quess I'm asking if their is enough people here willing to purchase if the sample checks out ok? What do you guys think? Pass on the deal or have a sample sent?
×
×
  • Create New...