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making potassium (per) chlorate


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Posted

Nope, i was saying the thing that i wrote.

A Chlorate cell needs to be operated at a higher then a Perchlorate cell. If you are operating a Perc cell at high temperatures, you`re doing something wrong (expet for the KClO3 --> KClO4 route). if the temperature raises in the perc cell, you will get a higher production of oxigen.

Also you don`t need a higher voltage for a perchlorate cell. (But there a some reasons why it could be interesting to do so, as you can be sure that you are pumping enought amps into the cell)

Also you`re wrong the reaction is not pure anodic, there is even a lot of bulk reaction, but this part really depends on the way you`ve build your cell (mostly Placing anodes and amperes/temperature). (In a chlorate cell)

For the bulk reaction you will need 6 electrons for the Anodic on 9.

In the Perchlorate cell you really just got anodic reaction.

 

The classic texts on (commercial) perchlorate production, generally mention a higher temperature (or was I remembering Swede's potassium chlorate to potassium perchlorate study?!).

 

It's been my understanding that chlorate is usually run at about 3.6Vdc (regardless what us amateurs do) and perchlorate between 6-7Vdc.

 

If you re-read what I wrote, I was referring to perchlorate production, not chlorate when I said it was purely anodic. I know the difference between anodic and bulk reactions in chlorate cells and how the bulk reaction is pH driven.

 

WSM B)

Posted

Yep

 

With the voltages i didn`t understand that you where writing about commercial cells, thought you were talking about amateur cell.

As maybe know of this often made fault, when people use a platin anode, and wan`t to keep chloride higher than 100g/L (High chloride means nearly no erosion, as kong as you`re over 100g/L), run there cell down to 110 at 4-5V and then change over to 6-7,5 V thinking that they are now stop making chlorate and are just making perchlorate.

 

Yes you were thinking about the straight pottasium way, with sodium you needlower temperatures.

Posted (edited)

As some people said that MnO2 anodes won`t last.

I`ve made one new Up, on Ti. Works perfect with KCl

The way i`ve done it was:

Mix Mn metal with HNO3 and H2O2

Take the solution and aply it thin onto a sheet of Ti.

Heat it on a Hotplate to 350°C

Shake dust of.

Rinse with H2O dest.

Set aside for 1 minute.

Repeat 5 times

Then heat with a gas torch.

Repeat 5 times (2x)

Leave aside for 1-2 Day`s. Now shake of all dust and use at max of 200mA cm²

 

This looks like an interesting process. If we don't have access to commercial MMO, this method may be a viable option for producing chlorates.

 

For perchlorates our options are a bit more limited.

 

WSM B)

Edited by WSM
Posted

For Perc just use LD on titanium.

 

For the Bath, i can recommend abath out of Lead nitrate, Lead carbonate and Sulfamic acid. worked perfect for me. This gave me a really sturdy cover. Couldn`t scratch any of the LD away with my nail and even with a 2mm steel dowel i could`t scratch it

Posted (edited)

For Perc just use LD on titanium.

For the Bath, i can recommend abath out of Lead nitrate, Lead carbonate and Sulfamic acid. worked perfect for me. This gave me a really sturdy cover. Couldn`t scratch any of the LD away with my nail and even with a 2mm steel dowel i could`t scratch it

 

Do you have photos and details of the process? It would be nice if your results can be reproduced.

 

WSM B)

Edited by WSM
Posted

Do you have photos and details of the process? It would be nice if your results can be reproduced.

WSM B)

 

It would be a wonderful thing if we document these projects so others can follow them. Sharing is the best way to expand our work.

 

WSM B)

Posted
LD would be great if its possible to buy them... not all of us have fancy lab equipments to produce a quality LD anode.
Posted (edited)
Atm not, but next time i`m making a new one, i will take some pictures, No worries. I think that I'm going to produce some next month (Will make a complete new cell) Edited by schroedinger
Posted (edited)

It would be a wonderful thing if we document these projects so others can follow them. Sharing is the best way to expand our work.

WSM B)

 

In my effort to gather materials for building a continuous chlorate cell, I've acquired several digital meters (primarily Voltage, Ampere and Temperature meters). One concern is that most of the external temperature sensors that come with the meters are unprotected and won't last in a cell.

 

On eBay, I found some PVDF shrink tube which can protect the sensors from the cell liquor. Even though I have a few of the teflon coated PT-100 sensors and matching digital meters, the bulk of the temperature meters I've gotten have unprotected sensors which can now be protected. When I do this I'll post photos...

 

WSM B)

Edited by WSM
Posted

Maybe the easiest think for a temperature meter, is to look for a mercury based contact thermomter.

 

The outside is made of glass, so no problem.

Posted (edited)

Maybe the easiest think for a temperature meter, is to look for a mercury based contact thermomter.

The outside is made of glass, so no problem.

 

Possibly, but I don't relish the possibility of either broken glass or liquid mercury in my cell should the device accidently get broken. This doesn't address the electrical connections either. Hardening the electrical parts from the ravages of salt spray or chlorine exposure is tough, too.

 

I like the protection offered by the PVDF materials, and how they can work to preserve my electrical components in proximity of the cell.

 

Few materials hold up to the environment of our cells. Among them are Teflon and it's analogs, PVC and CPVC, borosilicate glass (Pyrex) and a few others. One of the least expensive of the Teflon-type (fluorocarbon) is PVDF or Kynar polymers.

 

PVDF is expensive but items made of it usually run about 20% the cost of Teflon, and it's excellent in our cells.

 

WSM B)

Edited by WSM
Posted (edited)

Atm not, but next time i`m making a new one, i will take some pictures, No worries. I think that I'm going to produce some next month (Will make a complete new cell)

 

When you make the LD anode AND the cell, please include details like temperatures,

chemicals and their quality and concentration, voltage and current of electrochemical plating.

 

The material details of the cell and it's construction would be useful, too. Think, "What information would I need to duplicate this cell?" and try to include it.

 

Thanks.

 

WSM B)

Edited by WSM
Posted

No worries. Will do so, as soon as the snow is gone.

 

@WSM never heard of that stuff, over hear teflon is used for everything, and it`s not to expensive.

Posted
Consider your self very lucky if teflon parts are cheap. It is the better pick of the two. It seems to be impervious to most all harsh chemicals .
Posted

No worries. Will do so, as soon as the snow is gone.

@WSM never heard of that stuff, over hear teflon is used for everything, and it`s not to expensive.

 

Where in the world are you?

 

WSM B)

Posted
I need a help on conversion of sawdust to charcoal very urgent
Posted

@Brain Wrong Topic.

 

@WSM I'm located in lower Europe.

Posted

@Brain Wrong Topic.

@WSM I'm located in lower Europe.

 

Awesome. Now let's see, that can be anywhere from Portugal to Turkey... no, too large of a geographical area! Care to narrow it down for me?

I live on the West coast of the US, near a major metropolitan area.

 

On the other hand, if PTFE (or any other formulation of "Teflon" type materials, for that matter) are so common and inexpensive there, you are truly blessed. By all means use it if you can. Here in the US, PTFE is significantly more expensive than PVDF, which is significantly more expensive than PVC. All of them work in a cell (with varying degrees of success) and are the better materials to use (if you have the tools to work them with).

 

Most of my experimental cells involve a short section of large diameter PVC pipe, carefully solvent welded (glued) to a piece of PVC plate a bit thicker than the wall of the pipe. I've used pieces of 6" to 12" (150mm to 300mm, nominal) PVC pipe for tanks. I had limited success using plumbers cement for PVC, so I switched to an industrial PVC cement and have had better results.

 

The manufacturers of PVC pipe, etc. suggest the maximum temperature for PVC is 60oC; but Swede says that is for a pressurized system and suggests that we can likely go higher at 1 atm., without deformation, and I'm inclined to agree...

 

WSM B)

Posted

I need a help on conversion of sawdust to charcoal very urgent

 

I would try either the Pyrotechnics or the Tools sections. I think more discussions of charcoal making happen there. Good luck.

 

WSM B)

Posted (edited)

Awesome. Now let's see, that can be anywhere from Portugal to Turkey... no, too large of a geographical area! Care to narrow it down for me?

I live on the West coast of the US, near a major metropolitan area.

On the other hand, if PTFE (or any other formulation of "Teflon" type materials, for that matter) are so common and inexpensive there, you are truly blessed. By all means use it if you can. Here in the US, PTFE is significantly more expensive than PVDF, which is significantly more expensive than PVC. All of them work in a cell (with varying degrees of success) and are the better materials to use (if you have the tools to work them with).

Most of my experimental cells involve a short section of large diameter PVC pipe, carefully solvent welded (glued) to a piece of PVC plate a bit thicker than the wall of the pipe. I've used pieces of 6" to 12" (150mm to 300mm, nominal) PVC pipe for tanks. I had limited success using plumbers cement for PVC, so I switched to an industrial PVC cement and have had better results.

The manufacturers of PVC pipe, etc. suggest the maximum temperature for PVC is 60oC; but Swede says that is for a pressurized system and suggests that we can likely go higher at 1 atm., without deformation, and I'm inclined to agree...

WSM B)

 

As I was reviewing old posts, I found where Swede mentions the PVC details I referenced above. See post numbered 2030 (about page 102) for his detailed explanation. (Thank you Swede :D)

 

WSM B)

Edited by WSM
Posted (edited)

The problem with large diameter PVC pipes to be used as container is 1. Nobody is going to sell me a short section of those pipes, minimum order is probably at least 1km worth of pipes, so the only way is raid construction sites which will probably land me in jail (as they will not give them away), and 2. Where the heck do I find PVC plates? When I asked any place that sells plastics they laughed at me.

 

In any case I have used containers made from PP and it worked fine.

Edited by taiwanluthiers
Posted
Pvc is not that hard to find in large size . Many sites have waste, you just need to know how to ask for it. Most guys will toss it to you for a case of beer etc. ( make it worth their time to give it to you)
Posted

The problem with large diameter PVC pipes to be used as container is 1. Nobody is going to sell me a short section of those pipes, minimum order is probably at least 1km worth of pipes, so the only way is raid construction sites which will probably land me in jail (as they will not give them away), and 2. Where the heck do I find PVC plates? When I asked any place that sells plastics they laughed at me.

In any case I have used containers made from PP and it worked fine.

 

If you see a construction site with scrap pieces of large bore PVC pipe laying about, ask the supervisor of the job if you can have one or two. If he objects, ask why? If they're sold to scrappers, offer to pay for them. You never know unless you ask.

 

Some notes about my PVC tanks:

  • Most of the large bore PVC tanks I've made are from 1.5 to 2 times as long as the pipe diameter.
  • I've been taught the wisdom of leaving an empty space above the liquor (up to 6" or 150mm) where the bubbles can pop and minimize the amount of salty spray that can leave the cell.
  • If the wall thickness of the pipe is, for example, 9mm, use 10mm or 12mm PVC sheet for the tank bottom and lid.
  • Practice drilling holes in a scrap piece of similar material to learn how it's done, and don't destroy your work on the tank (it takes special drills to avoid breaking the PVC plastic).

 

Speaking of PP, I have some heavy-walled rectangular polypropylene (PP) tanks I bought on ebay. Though not ideal, they should work just fine (certainly better than PE, i.e. polyethylene). At 18" by 18" by 24" tall (450mm x 450mm x 600mm) one could easily be made into a 100 liter cell :o :whistle: !!!

I haven't done so but it's in the back of my mind :P.

 

WSM B)

Posted

I often thought about PVC casings, but made my best out of an acryl food storage box (the round type, with airtight closing lid). It holds up perfect and not much Work. You just need to fit the Anodes, Exhaust and Maintenance port into the lid.

 

Once if used a Steel one and the used the steel as cathode, worked perfect until i dropped the PH a little low and the Steel corroded. Wasn`t a lot of fun

Posted

CP titanium tanks would be ideal... use it as container and cathode. But it will be expensive...

 

What about Acrylic and Polycarbonate? They're easy to obtain although a little expensive, and I can weld them together with solvents. I have never managed to find PVC sheets... I'd love to get large diameter PVC pipes anyways for making ball mill jars.

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