making potassium (per) chlorate

[WSM]

In the video the cathode is in Pt anode and stainless believe.

 

I may be wrong but they look more like platinum mesh and expanded perforated titanium mesh, to me.

 

WSM

Edited March 6, 2017 by WSM

[Nitrotitanite]

there should be a video of the same but with a more accurate description I try to look for him.

[Nitrotitanite]

I think you riferissi to this video.

Here part by a potassium chloride solution.

 

 

https://www.youtube.com/watch?v=9FyGP-zSpZo&app=desktop

[WSM]

hey dude

This was one of the first Videos i've researched for informations when i started that hobby.

It's not a fake in my opinion and could be a pretty reliable concept but he did NOT made Chlorate i think since the PT Anode will be damaged a lot if you electrolyze from NaCl---->NaClO4 in one Step.

please let me know, if you know were to find those Glas vessels.

If you plan to build a Cell, buy some Anodes online and not PT since it is too expensive.

Search for a chinese MMO/PbO2 Supplyer and you will not spent hundrets of $$.

100x100PbO2, capable to handle ~25-30A will cost 45$ with shippment.

 

In my research, the only method shown to effectively run from NaCl directly to NaClO₄ uses a graphite substrate lead dioxide anode with some sodium fluoride as a buffer/catalyst. The paper was from India if I remember correctly.

 

The sodium fluoride (or any soluble fluoride, for that matter) would negatively affect titanium substrate anodes and drastically reduce their life !!!

 

WSM

Edited March 6, 2017 by WSM

[Nitrotitanite]

Here is the video that I said

 

[WSM]

I recall seeing another video in the past, with the same setup where he did make KClO₄, and it looked very different in appearance (a fine, white crystalline, wet powder on the filter paper), not the coarse crystals shown in the video above. Unless the higher temperature of his setup causes the coarse crystals we're seeing, I suspect I'm right.

WSM

 

Maybe I'm wrong.

 

I know that when I made KClO₄ from NaClO₄ (at room temperature [maybe 25^oC], not 85^oC), the look was very different (like milk till the crystals dropped to the bottom of the beaker).

 

 

WSM

Edited March 6, 2017 by WSM

[Nitrotitanite]

Probably the rapid drop in temperature causes the formed crystals are larger.

I think the difference is in the working temperature.

I think 😅😅

[WSM]

Here is the video that I said

 

Yes, this video looks more familiar to me.

 

His use of methylene blue solution looks different from mine, for some reason. Maybe it's his video camera. but my still camera shows a more pronounced difference between the blue control and the purple positive test for perchlorate:

 

 

Even my test of perchlorate in a test tube seems a different color than his. Oh well, I won't worry about it.

 

WSM

[WSM]

Probably the rapid drop in temperature causes the formed crystals are larger.

I think the difference is in the working temperature.

I think

 

Possibly. The faster the crystals form, the smaller they typically are. Usually, slow crystallization makes for larger crystals.

 

WSM

[Nitrotitanite]

The more intense color can also be caused by light, usually the cold-light neon bring out more colors.

I then believe that the larger crystals dependent on other factors, however, the important thing is that there is peclorato.

Out of curiosity, what method you used to do Perchlorate?

[WSM]

The more intense color can also be caused by light, usually the cold-light neon bring out more colors.

I then believe that the larger crystals dependent on other factors, however, the important thing is that there is peclorato.

Out of curiosity, what method you used to do Perchlorate?

 

I believe the light was from an LED lamp, but the colors shown are close to that observed in daylight, also.

 

I electrolyzed solutions of sodium chlorate using two different cells; one with an LD on titanium anode and the other with platinum plated titanium anode. I used double titanium solid plates (surrounding the anode) for the cathodes in both cells.

 

I haven't tried running directly from sodium chloride to sodium perchlorate.

 

WSM

Edited March 8, 2017 by WSM

[Nitrotitanite]

Thank

[WSM]

Thank

 

You're welcome.

 

WSM

[WSM]

I believe the light was from an LED lamp, but the colors shown are close to that observed in daylight, also.

I electrolyzed solutions of sodium chlorate using two different cells; one with an LD on titanium anode and the other with platinum plated titanium anode. I used double titanium solid plates for the cathodes in both cells.

I haven't tried running directly from sodium chloride to sodium perchlorate.

WSM

 

I should add that once the sodium perchlorate was made, I treated a sample portion of it (100 ml) with sodium metabisulfite solution to destroy the residual chlorates (with the SO₂ formed in solution) before adding KCl solution, used to convert it to potassium perchlorate. Once I had KClO₄ dropped from the solution (which formed instantly), I vacuum filtered it to separate the powdered (very fine crystalline) potassium perchlorate from the fluid parts remaining (soluble sodium salts).

 

I next rinsed the wet powder with chilled distilled water. The rinsing didn't completely remove residual sodium, but was a good first step in the process of purifying the product.

 

I suspect giving the fresh KClO₄ a soak in a large quantity of distilled water and then vacuum filtering it, followed by a chilled distilled water rinse while it remains sitting in the Buchner funnel with the vacuum running, will go a long way toward finally purifying the potassium salt of all sodium contamination. We'll see...

 

WSM

Edited March 8, 2017 by WSM

[WSM]

Happy Pi day !

 

WSM

[WSM]

I've been super busy at work (12 hour days, six days a week) and haven't been able to do much else, lately.

 

I did fill the experimental cell with water and, unfortunately, there's a slight leak amongst the bottom fittings. I'll check it more closely when I can manage to get home during the daylight hours. I'm sure it's just that I didn't tighten some of the fittings enough when I assembled the bottom plate.

 

The Viton gasket is holding fine though, so that's not the problem.

 

I think things will ease up at work soon, and I'll be able to adjust the fittings and find out if the cell will seal properly and work the way I planned it to.

 

We'll see...

 

WSM

Edited March 16, 2017 by WSM

[WSM]

I think things will ease up at work soon, and I'll be able to adjust the fittings and find out if the cell will seal properly and work the way I planned it to.

 

It's starting to look like I'll have this weekend free (Yay!), so we'll see how the cell looks after I tighten the fittings and try the water test again.

 

Once everything is tight and secure, it's time to set up a trial run and try to determine how much time it'll take to reduce the fluid level to approximately 50% of its starting point (which is when the harvesting cycle begins).

 

I'm excited to see the difference between the way things went last year and how this new cell works. If it runs as well as expected, this might be a real game changer for amateur perchlorate production .

 

WSM

[Nitrotitanite]

When everything is completed it would be nice to have a full tutorial that summarizes all 233 pages of this long post, very heavy to understand to be honest.

[Mumbles]

I don't know if it will ever truly be complete. If you want write ups you may want to check WSM's blogs. There have also been some articles written in the PGI bulletin on chlorate and perchlorate cells.

[WSM]

I don't know if it will ever truly be complete. If you want write ups you may want to check WSM's blogs. There have also been some articles written in the PGI bulletin on chlorate and perchlorate cells.

 

Hi Nitrotitanite,

 

If you do read my blog postings and have questions about anything there, feel free to ask here or by PM (your choice) and I'll do my best to answer.

 

This is true for everyone here. If we don't ask, we don't learn.

 

WSM

[Nitrotitanite]

Ok thanks for your time😃

[greenlight]

Sorry for the massive delay bit I have been busy with work.

I only just got around to wiring up the whole system today.. Another reason for the delay is I decided I wanted the whole thing mounted on a wooden table that is dodgily made from a wooden pallet and sheets of thin plywood.

There is also a dividing section that the ammeter sits in to seperate the electronics from the cell a little bit.

Here is a pic from the electronics side. It is half wired together.

Edited March 19, 2017 by greenlight

[WSM]

Sorry for the massive delay bit I have been busy with work.

I only just got around to wiring up the whole system today.. Another reason for the delay is I decided I wanted the whole thing mounted on a wooden table that is dodgily made from a wooden pallet and sheets of thin plywood.

There is also a dividing section that the ammeter sits in to seperate the electronics from the cell a little bit.

Here is a pic from the electronics side. It is half wired together.

 

It looks like it's coming together. I think it'll work fine. Let us know how it goes.

 

WSM

[WSM]

Happy Vernal Equinox (unless you're in the Southern hemisphere, in which case; Happy Autumnal Equinox) !!!

 

WSM

Edited March 20, 2017 by WSM

[Kevin]

Hi, I'm going to be adding a temperature display to my chlorate cell for its next run (May at the earliest). I bought an Inkbird ITC-100VH temperature controller/ display and a PT100 teflon insulated sensor online. I have 1/4" compression fittings, but the temperature sensor is too narrow to make a tight seal where it will enter the lid. The best solution I've come up with (Somewhat based on WSM's blog post I recall reading a while back) is to use a (roughly) 1/4" plastic plug with a hole drilled through the center for the sensor and then I'll use heat shrink tubing over them both to seal it. I have some NTE electronics brand clear, thin-walled heat shrink tubing on hand, but all it says is that it's polyolefin which, to the best of my knowledge, could be any of a number of different types of plastic. I tried contacting them to find out specifically which type it is, but, unsurprisingly, they didn't respond. Any idea if I can use this for my cell? I'm figuring I'll give it a try and if it doesn't hold up I'll purchase some better heat shrink tubing.

 

Kevin