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making potassium (per) chlorate


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#5261 WSM

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Posted 23 August 2020 - 08:29 AM

I've managed to build the basic framework around the borosilicate reaction vessel with its PTFE lid assembly. Rather than use reversed Belleville washers (which would provide much more force than this setup needs), I used simple steel compression springs on the top of the all-thread rods for minimal force on the lid; and to accommodate any minor thermal expansion the system should experience by running at 110oC.

I still need to add a few details to the system structure before building the cell's internal parts. I'll try to dust off my camera and add some photos for a clearer view of what I'm doing and how it's coming together.

I'm afraid it will look rather complicated by the time it's running, but the concept is fairly simple to begin with.

WSM B)

 

 

I'm adding photos so you can see where this project is at.

 

 Attached File  IMGP0002.JPG   89.55KB   1 downloads

Attached File  IMGP0003.JPG   168.85KB   1 downloads 

 

There is more to do to make the final version of just the framework, let alone even getting the cell ready for a trial run; but one step at a time...

 

WSM  B)

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Edited by WSM, 23 August 2020 - 11:51 AM.


#5262 Andead

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Posted 09 September 2020 - 07:40 AM

Quick question because I am struggling to find the answer to my question. When the titanium cathode has a layer of titanium dioxide how do  i remove it? Using dilute HCL or acetic acid or are there some other options? Thanks 



#5263 WSM

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Posted 09 September 2020 - 12:35 PM

Quick question because I am struggling to find the answer to my question. When the titanium cathode has a layer of titanium dioxide how do  i remove it? Using dilute HCL or acetic acid or are there some other options? Thanks


Experimentation might be called for. Possibly a timed soak in strong hydrochloric acid, followed by a thorough rinse in water might work.

If chemical means don't work, perhaps a mild abrasive would do the trick.

Let us know what you come up with.

WSM B)

#5264 markx

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Posted 10 September 2020 - 12:36 AM

Soak in hot phosphoric acid is a pretty agressive means to clean Ti surface from deposits. Hydrochloric and acetic shall remove the hydroxide deposits from cathodes pretty quickly, but struggle with Ti compounds. There is really no practical need to remove cathodic deposits from Ti.....apart from aesthetic purposes. The oxide is permeable to charge transfer under cathodic potential and it will restablish its precence during the next use of the equipment anyways.



#5265 WSM

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Posted 10 September 2020 - 12:54 PM

Soak in hot phosphoric acid is a pretty agressive means to clean Ti surface from deposits. Hydrochloric and acetic shall remove the hydroxide deposits from cathodes pretty quickly, but struggle with Ti compounds. There is really no practical need to remove cathodic deposits from Ti.....apart from aesthetic purposes. The oxide is permeable to charge transfer under cathodic potential and it will restablish its precence during the next use of the equipment anyways.

 

So the best solution to the problem is to ignore it? I like that.

 

If it works, great! If it doesn't work, you should know right away and use a different approach.
Try it and see... :D 

WSM B)


Edited by WSM, Yesterday, 05:28 AM.


#5266 WSM

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Posted Yesterday, 05:42 AM

I've managed to build the basic framework around the borosilicate reaction vessel with its PTFE lid assembly. Rather than use reversed Belleville washers (which would provide much more force than this setup needs), I used simple steel compression springs on the top of the all-thread rods for minimal force on the lid; and to accommodate any minor thermal expansion the system should experience by running at 110oC.

I still need to add a few details to the system structure before building the cell's internal parts. I'll try to dust off my camera and add some photos for a clearer view of what I'm doing and how it's coming together.

I'm afraid it will look rather complicated by the time it's running, but the concept is fairly simple to begin with.

WSM B)

 

 

I did a quick calculation and if I use an anode sized 4" x 6" (roughly 100 mm x 150 mm) with two cathode plates surrounding the anode, the current draw would be about 93 Amps! 

 

I need to figure out whether that's enough or too much current for a four liter volume (maximum) in my five liter reaction flask.

 

My purpose is to generate enough heat (but not too much) to run the system at 110oC, where the excess water in the electrolyte will vaporize and get out through the vent, naturally concentrating the sodium chlorate electrolyte to where it will drop solid crystals out of solution when it cools to room temperature!

 

I'm not sure if I can easily determine this mathematically, or whether an empirical approach (make the electrodes up and try it in a cell) would work better?

 

We'll see...

 

WSM B)


Edited by WSM, Yesterday, 05:45 AM.


#5267 WSM

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Posted Yesterday, 08:51 AM

After I posted about testing electrodes in a cell to measure the heat produced in the electrolyte, I realized how it could be done simply.

If I make up a temporary electrode assembly, I can immerse the electrodes in a large beaker of electrolyte to various depths and run the theoretical current while measuring the temperature of the electrolyte.

This seems to be the easiest method of determining the dimensions of the electrodes required to achieve the ideal temperature within the cell.

WSM B)

Edited by WSM, Yesterday, 08:54 AM.





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