making potassium (per) chlorate

February 3, 2017

Hey guys
I've boiled down my stock electrolyte from 40l to 8l.
I was able to get out 806g KClO3 wchich remained in solution.
It was really pure due to lots of filtrations between the evaporation steps.
DSC_12331.JPG
DSC_12341.JPG
DSC_12351.JPG
DSC_12391.JPG
Now im boiling the last 8l down to 1-2l and i start harvesting again over the year.
This morning i came down to my workplace and take a first look into the bucket with cooled electrolyte.
Now mostly of the Chlorate is pecipitated and the Chlorides start to fall out of solution.
Since i dont work with proper calculations, ive got lots of chloride left but im not be able to tell which one ive got here.
assuming that the Kcl is much more soluble i first thought that it must be NaCl.
I washed a crystal fairly and gave it a taste and it tasted much like Kcl.
What do you think, and what can i do to find out which chloride i have left here.
DSC_12471.JPG
DSC_12501.JPG
DSC_12491.JPG

Nice work, PTFE.

I've never tried to extract all the KClO₃ from my electrolyte. Usually, we let all the potassium salt drop out that will, recharge the depleted electrolyte and run the cell again.

Granted, (here in the US) we electrolyze KCl solution, to avoid sodium contamination; but even starting with NaCl solution, not many here take the effort to extract everything possible from a cell run.

One problem (as you now see) is separating the various remaining salts, and doing it our way (not running to completion) seems a simple way to avoid such problems. I think that if you dissolve the remaining salt in the least amount of distilled water and electrolyze it, the potassium salts (being so much less soluble) will drop out first, leaving the more soluble sodium salts in solution. That's my theory, anyway. As far as I know, no one's tried it yet, but I think it'll work.

Thanks for sharing your experiences. Let us know what you decide to do.

WSM

Edited February 6, 2017 by WSM

February 8, 2017

I think that if you dissolve the remaining salt in the least amount of distilled water and electrolyze it, the potassium salts (being so much less soluble) will drop out first, leaving the more soluble sodium salts in solution. That's my theory, anyway. As far as I know, no one's tried it yet, but I think it'll work.

Do you want to test my theory and see if KClO₃ would drop out of the solution, leaving the sodium salts behind in the solution? It would be nice to know if I'm guessing right.

Let us know. Thanks.

WSM

Edited February 9, 2017 by WSM

February 10, 2017

My work schedule is extremely busy now (12 hour days, 6 days a week) and will continue till the last part of April. It seems my days are reduced to a continuous pattern of work, eat, sleep (and repeat), with little opportunity for much else. My only days off are Sundays, but those are dedicated to Family, so my active research will be on hold till this assignment is concluded in the Spring .

I will continue to study the system and designs, but I won't be able to run the experiment until late April or early May.

The upside is our financial situation will improve (not that it's horrible now), but duties requiring my personal attention will suffer.

I'm looking forward to running the high temperature sodium chlorate system and seeing if it works as well in practice as the patent indicates it will. If it does work as well as I hope it will, I'll run it till I have a lot of sodium chlorate for feedstock in the perchlorate experiments.

I'd like to see how long the platinum and lead dioxide electrodes will last in practice, as well as the total production during their lifetimes. That would give us a realistic view of the actual cost of our homegrown oxidizers.

WSM

Edited February 11, 2017 by WSM

February 12, 2017

Hi,WSM

I've never tried to extract all the KClO₃ from my electrolyte. Usually, we let all the potassium salt drop out that will, recharge the depleted electrolyte and run the cell again.

I do it just as you do, but after several runs in the past, i've ended up with 40l or more.

My parents don't like the idea of a big salty water tub breaking indoors sometime, also i don't want to pour it down the drain or anywhere else.

One problem (as you now see) is separating the various remaining salts, and doing it our way (not running to completion) seems a simple way to avoid such problems. I think that if you dissolve the remaining salt in the least amount of distilled water and electrolyze it, the potassium salts (being so much less soluble) will drop out first, leaving the more soluble sodium salts in solution. That's my theory, anyway. As far as I know, no one's tried it yet, but I think it'll work.

Thanks for sharing your experiences. Let us know what you decide to do.

My thoughts where the same, but it was a bit easier.

In the last pictures you can see the formation of remaining KCl in the remaining electrolyte.

After filtration and boiling of 3litres more of the soluion, NaCl started to come out.

It was not to much..maybe 500grams but more than the Kcl.

The Recycled, impure Kcl was dryed out and stored for the next Metathesis reaction and the impure NaCl was stored for the actual run of my small cell.

Do you want to test my theory and see if KClO₃ would drop out of the solution, leaving the sodium salts behind in the solution? It would be nice to know if I'm guessing right.

Let us know. Thanks.

WSM

Im sorry for my late response everytime.

At the moment im running my small cell in a continous run since 09.02. 10:30am.

The cell is a 2,8l Lock&Lock container and it got a little messy on my sill due to salt creep as you can see in the pictures below, but i don't care really much about it.

When you have thin cell walls you don't have to insert a temperature probe, just insulate it at the outside.

The cell is running with the old Electrode configuration at ~5.5V and ~65A / 90°C.

I've started with refreshed electrolyte and a layer of the recycled NaCl Crystals.

Today, after a runtime of ~72hrs i've removed most of the electrolyte because a layer of NaClO3 started to build up and cake around the electrodes.

When the 90°C electrolyte was transfered to the bottles, nothing has precipitated.

(Here i have to mention, that you don't have to worrie about Salt shortening your Electrodes.

Since you are using proper spacers, nothing could happen due to the nonconductivity of the solid Salts in the Cell.)

I guess a bit of KClO3 is also contained but not much.( I have taken out a bunch of the crystals and dissolved them in a tiny amount of cold water without a problem.)

The cell was then refilled with fresh brine, some tap water and after the Layer has dissolved I added the remaining NaCl.

Im planning to use this stock NaClO3 for my PbO2 Anode but I've got an tonsil-Operation next week, so it will take some time to build the cell.

Also my imersion-heater failed when i was boiling down the Stock elektrolyte.

I was doing some other stuff and was watching every 30minutes.

When the NaCl started to drop out of the solution it first crystallised between the small gaps of the PTFE tube and the Heat could not be carried away.

The good thing, no oil leaked out of the tube and no extra filtrations where needed.

For about 40$ i've buildet a new one with 2kW instead of 1kW.

Unfortunately you have to wait for a picture of the new one, but here is one of the leak in the PTFE tube.

PTFE ^_^

February 13, 2017

Hi,WSM
I do it just as you do, but after several runs in the past, i've ended up with 40l or more.
My parents don't like the idea of a big salty water tub breaking indoors sometime, also i don't want to pour it down the drain or anywhere else.
My thoughts where the same, but it was a bit easier.
In the last pictures you can see the formation of remaining KCl in the remaining electrolyte.
After filtration and boiling of 3litres more of the soluion, NaCl started to come out.
It was not to much..maybe 500grams but more than the Kcl.
The Recycled, impure Kcl was dryed out and stored for the next Metathesis reaction and the impure NaCl was stored for the actual run of my small cell.
Im sorry for my late response everytime.
At the moment im running my small cell in a continous run since 09.02. 10:30am.
The cell is a 2,8l Lock&Lock container and it got a little messy on my sill due to salt creep as you can see in the pictures below, but i don't care really much about it.
DSC_12621.JPG
DSC_12601.JPG
When you have thin cell walls you don't have to insert a temperature probe, just insulate it at the outside.
DSC_12611.JPG
The cell is running with the old Electrode configuration at ~5.5V and ~65A / 90°C.
DSC_11771.JPG
DSC_12581.JPG
I've started with refreshed electrolyte and a layer of the recycled NaCl Crystals.
Today, after a runtime of ~72hrs i've removed most of the electrolyte because a layer of NaClO3 started to build up and cake around the electrodes.
DSC_12571.JPG
When the 90°C electrolyte was transfered to the bottles, nothing has precipitated.
(Here i have to mention, that you don't have to worrie about Salt shortening your Electrodes.
Since you are using proper spacers, nothing could happen due to the nonconductivity of the solid Salts in the Cell.)
I guess a bit of KClO3 is also contained but not much.( I have taken out a bunch of the crystals and dissolved them in a tiny amount of cold water without a problem.)
The cell was then refilled with fresh brine, some tap water and after the Layer has dissolved I added the remaining NaCl.
Im planning to use this stock NaClO3 for my PbO2 Anode but I've got an tonsil-Operation next week, so it will take some time to build the cell.
Also my imersion-heater failed when i was boiling down the Stock elektrolyte.
I was doing some other stuff and was watching every 30minutes.
When the NaCl started to drop out of the solution it first crystallised between the small gaps of the PTFE tube and the Heat could not be carried away.
The good thing, no oil leaked out of the tube and no extra filtrations where needed.
For about 40$ i've buildet a new one with 2kW instead of 1kW.
Unfortunately you have to wait for a picture of the new one, but here is one of the leak in the PTFE tube.
DSC_12511.JPG
PTFE

Thanks for the updates, PTFE. It looks like you're doing good things with your setup. I would be nervous about too much electrolyte sitting around, also (better to process it and recycle the salts as much as possible).

I plan to set up my system to run as soon as things calm down at work and I have more time at home for experimenting.

Keep up the good work and posting your progress. If you get the time, see if you can give more details of the various parts of your system. Some folks wanting to develop their own system can benefit from some of the details .

WSM

Edited February 13, 2017 by WSM

February 13, 2017

I've acquired some electronic components on eBay and plan to build a couple precision timers for use with pH controllers and other projects needing accurate timing.

These timers are analogous to the expensive one's Swede used for his pH controller, and they switch a solid state relay which powers an AC outlet for running pumps, valves and other fluid handling equipment at precise intervals.

I'll show more details as the project continues and I manage to take a few photos. I'll be gone for a week in the meantime to Western Winterblast, then back to work.

More later...

WSM

February 14, 2017

Hey guys

I would be nervous about too much electrolyte sitting around, also (better to process it and recycle the salts as much as possible).

Yes, since I had some messy accidents with really small quantitys i don't like to think about a 40l mess..

How do you process your Electrolyte? Im sure i'd read something about it, pages ago. But i don't remind and i really don't want to read through the whole thread again.

I plan to set up my system to run as soon as things calm down at work and I have more time at home for experimenting.

Same here, lots to do, but not the time for the thinks i really want.

Keep up the good work and posting your progress. If you get the time, see if you can give more details of the various parts of your system. Some folks wanting to develop their own system can benefit from some of the details .

Here you are

Today I stopped the run and processed the Electrolyte.

Also i recycled the 1kw immersion heater with the leaks in the tube.

The PTFE tube was cut at some places and the heating spiral was removed to be placed in a new one.

1,5mm²Crimped to the spiral and then it was inserted into a new tube

Some Spacers where made to prevent a overheating and the tube was filled with oil.

As you fill it up, you have to fill it in from the bottom of the spiral, and only just that much, that you can blow air through the spiral, otherwise it will shoot up the pipe as it boils in the tube.

2+1kw Heating power

After all I switched my Cheap China PSU off which I got fro 30$.

It's rated for 5V60A but it gets sooo hot, that I had to modify it.

I put in bigger heat sinks to the main switching transistors and to the output rectifier.

I also bypassed the temp. controller of the fan and put a large 120mm fan on top of it. (instead of a 75mm one)

The front was cut out to get a better air flow at the rectifier schottkys.

Then the Cell was washed and brought outside to eliminate the Hypochlorite.

The Anodes looked well, but the cathodes crumble now quite easy.

I think its just grade 3 Titanium or the CD is a bit too high, but ive got lots of Ti sheets remaining.

Some Erosion products are obtained but not too much.

To destroy the remaining NaClO 20ml H2O2 were used first, then about 3g Urea. (I dont care about the ~3g/l chlorate you get when you heat for hours, and i really don't know what happens in the urea reaction...maybe someone could explain what reactions take place when you add Urea)

Do this in small portions with strong stirring. Even when it seems to be not violent, when you start stirring it, things can go fast. Be aware that an overflow could occour quite easy.

Also the smell of the Urea Reaction is quite terrifying and with no proper ventilation the air around you will get quite corrosive and harmful.

Ph was cheked (I need some better quality Ph strips, or maybe a probe) and im pleased with 8 since it goes directly into the Perc cell.

After boiling for some minutes and adding about 500ml water to reach the saturation point the electrolyte was filtered for 4 times trough the fleece showed earlier.

A sample was taken and cooled in the snow to show how many NaClO3 is present.

with the same amount of slightly warm water it was filled up and the Na salt has dissolved and i could estimate the amount of KClO3 in the Electrolyte.

A Methylene Blue test shows, that a tiny amount of Perc has started to form. Even if there is no Violet precipitant you can see a slightly greenish colour and tiny particles started to form.. this does not occour with an electrolyte runned for a shorter period or with more Chloride in solution.

After some hours, the crystalised NaClO3 was filtered out, and the remaining solution placed outside to precipitate more.

The Container composed of PP sustained quite well but at the bottom significant erosion was detected.

I would not recommend, running a PP cell over 90°C!

Also I would recommend a safty tub underneath regardless which container you use.

Im sorry for mistakes, i will check it later and give some more informations and an Edit.

Edited February 15, 2017 by PTFE

February 27, 2017

i keep looking for nw posting from WSM and none come. hope all is well...........

memo

February 27, 2017

i keep looking for nw posting from WSM and none come. hope all is well...........
memo

Everything is okay, I'm just super busy at work (lots of overtime). I've focused on pH control systems lately, and picked up some excellent gear on eBay for use with my experiments.

I'll try to post more later.

WSM

Edited February 27, 2017 by WSM

February 28, 2017

i keep looking for nw posting from WSM and none come. hope all is well...........

memo

Haha, same here. Looked frequently if something new appeared.

But I remembered, that he posted that he is on a journey for a week.

Everything is okay, I'm just super busy at work (lots of overtime). I've focused on pH control systems lately, and picked up some excellent gear on eBay for use with my experiments.

I'll try to post more later.

WSM

Nice to hear that everything is going well

i would like to know a bit about your Ph system and how you estimate the amount of hcl. Did you ever had done a test-run to determine the HCL needed per Ah of current?

For my big cell i used the formula from the page i just found out, that it seemed to be banned.

I forgott the name of it but im sure you all know it, it was the holy grail of a collection of informations and since today i can't find it anymore...(something like oxidizing.net?)

If someone has got a link to it I would be happy.

Since i had some runs of the small cell showed above, i've found out ,that not much HCL is needet.

For two runs,~6000Ah yielding approx. 2Kg NaClO3 i used not more than 100ml 10-15%HCL to held the PH in range.

But Even if the PH was under 5 i got a good yield at some of my first runs with my large cell but i never did a determination of CE of my cells.

im looking forward to hear from you WSM :lol:

edit: oxidizing.typhoonguitars.com/chlorate/chlorate.html

this was the side that i meant.

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

here its still available.. you should make your own offline version to keep that information saved

Edited February 28, 2017 by PTFE

February 28, 2017

i had to stop hosting it because i cant really afford the monthly cost anymore. I have the files however if anyone wants to continue hosting the information

February 28, 2017

Haha, same here. Looked frequently if something new appeared.
But I remembered, that he posted that he is on a journey for a week.
Nice to hear that everything is going well
i would like to know a bit about your Ph system and how you estimate the amount of hcl. Did you ever had done a test-run to determine the HCL needed per Ah of current?
For my big cell i used the formula from the page i just found out, that it seemed to be banned.
I forgott the name of it but im sure you all know it, it was the holy grail of a collection of informations and since today i can't find it anymore...(something like oxidizing.net?)
If someone has got a link to it I would be happy.
Since i had some runs of the small cell showed above, i've found out ,that not much HCL is needet.
For two runs,~6000Ah yielding approx. 2Kg NaClO3 i used not more than 100ml 10-15%HCL to held the PH in range.
But Even if the PH was under 5 i got a good yield at some of my first runs with my large cell but i never did a determination of CE of my cells.
im looking forward to hear from you WSM
edit: oxidizing.typhoonguitars.com/chlorate/chlorate.html
this was the side that i meant.
http://www.oocities.org/capecanaveral/campus/5361/chlorate/chlorate.html
here its still available.. you should make your own offline version to keep that information saved

A description of the idea, including photos of some equipment made a few years ago are included in my blog (found in the blog section above); Homegrown Oxidizers, Part Four. I got many ideas from Swede and his blogs titled, "You'll shoot your eye out..."! From time to time, I read and re-read Swede's blogs. There's a lot there.

Thanks again for sharing your adventures in electrochemistry. Maybe you could write a blog describing what you're doing and explain why you chose to do it the way you do, with enough details for others to follow in your steps. I think that would be helpful. I know I benefit from seeing what others are doing (and I like your approach to this).

WSM

Edited March 1, 2017 by WSM

March 1, 2017

Hey guys
Yes, since I had some messy accidents with really small quantitys i don't like to think about a 40l mess..
How do you process your Electrolyte? Im sure i'd read something about it, pages ago. But i don't remind and i really don't want to read through the whole thread again.
Same here, lots to do, but not the time for the thinks i really want.
Here you are
Today I stopped the run and processed the Electrolyte.
Also i recycled the 1kw immersion heater with the leaks in the tube.
The PTFE tube was cut at some places and the heating spiral was removed to be placed in a new one.
DSC_12711.JPG
DSC_12751.JPG
1,5mm²Crimped to the spiral and then it was inserted into a new tube
DSC_12771.JPG
DSC_12781.JPG
DSC_12801.JPG
Some Spacers where made to prevent a overheating and the tube was filled with oil.
As you fill it up, you have to fill it in from the bottom of the spiral, and only just that much, that you can blow air through the spiral, otherwise it will shoot up the pipe as it boils in the tube.
DSC_12791.JPG
2+1kw Heating power
After all I switched my Cheap China PSU off which I got fro 30$.
It's rated for 5V60A but it gets sooo hot, that I had to modify it.
I put in bigger heat sinks to the main switching transistors and to the output rectifier.
I also bypassed the temp. controller of the fan and put a large 120mm fan on top of it. (instead of a 75mm one)
The front was cut out to get a better air flow at the rectifier schottkys.
DSC_12681.JPG
DSC_12701.JPG
Then the Cell was washed and brought outside to eliminate the Hypochlorite.
DSC_12811.JPG
The Anodes looked well, but the cathodes crumble now quite easy.
I think its just grade 3 Titanium or the CD is a bit too high, but ive got lots of Ti sheets remaining.
DSC_13071.JPG
Some Erosion products are obtained but not too much.
To destroy the remaining NaClO 20ml H2O2 were used first, then about 3g Urea. (I dont care about the ~3g/l chlorate you get when you heat for hours, and i really don't know what happens in the urea reaction...maybe someone could explain what reactions take place when you add Urea)
Do this in small portions with strong stirring. Even when it seems to be not violent, when you start stirring it, things can go fast. Be aware that an overflow could occour quite easy.
Also the smell of the Urea Reaction is quite terrifying and with no proper ventilation the air around you will get quite corrosive and harmful.
DSC_12921.JPG
DSC_12931.JPG
Ph was cheked (I need some better quality Ph strips, or maybe a probe) and im pleased with 8 since it goes directly into the Perc cell.
After boiling for some minutes and adding about 500ml water to reach the saturation point the electrolyte was filtered for 4 times trough the fleece showed earlier.
A sample was taken and cooled in the snow to show how many NaClO3 is present.
DSC_13021.JPG
with the same amount of slightly warm water it was filled up and the Na salt has dissolved and i could estimate the amount of KClO3 in the Electrolyte.
DSC_13031.JPG
A Methylene Blue test shows, that a tiny amount of Perc has started to form. Even if there is no Violet precipitant you can see a slightly greenish colour and tiny particles started to form.. this does not occour with an electrolyte runned for a shorter period or with more Chloride in solution.
DSC_13041.JPG
After some hours, the crystalised NaClO3 was filtered out, and the remaining solution placed outside to precipitate more.
DSC_13121.JPG
DSC_13131.JPG
The Container composed of PP sustained quite well but at the bottom significant erosion was detected.
I would not recommend, running a PP cell over 90°C!
Also I would recommend a safty tub underneath regardless which container you use.
Im sorry for mistakes, i will check it later and give some more informations and an Edit.

Very nice post, PTFE.

I'll re-read it later and ask a couple questions that came to mind as I was reading it (I'm off to work right now).

WSM

March 4, 2017

After I got home from work today, I felt impressed to test the experimental tank for water tightness. I made up an adaptor for one of the outdoor water faucets, and ran tap water into and out of the tank and into a bucket. I wanted to avoid splashing any water on the outside of the tank to make leak detection easier.

I saw a small amount of water seepage at the bottom gasket, and tightened the screws slightly and the seepage seemed to stop. I used paper towels to mop up the small amount of water on the base, and will check it again tomorrow afternoon.

I think it would be a good idea to use double hex nuts on both the top and bottom plates of the cell so there won't be a tendency for them to loosen with the temperature changes, as the cell runs.

Once I determine the cell is water tight, it's time to set it up for a trial run. I still need to set up a hydrogen separator and water vapor recovery system. I'd like to recover the distilled water if I can, for making up replenishment brine. (Yes, I have thought this through for a while )

WSM

March 4, 2017

What pressures are you working with? I'm wondering if you haven't over thought the tank a bit.

March 4, 2017

What pressures are you working with? I'm wondering if you haven't over thought the tank a bit.

I'm just running the water through the tank, and collecting it in an empty bucket. Both inlet and outlet barb fittings are on the lid of the cell, leaving the cell full of water (no extra pressure, just a static load of water).

I want the tank to have structural integrity with no leaks.

WSM

March 4, 2017

I'll look at some commercial filter housings that may fit your needs. What capacity do you require and how many bottom connections are needed?

March 4, 2017

I'll look at some commercial filter housings that may fit your needs. What capacity do you require and how many bottom connections are needed?

This cell is an experiment with running at high temperature (110C) and is made of PVDF polymer for that reason.

The bottom has 4, 1/2" NPT ports and the lid has 5, 1/2" and 4, 1/4" NPT ports.

WSM

March 6, 2017

Do you know of this video here uses a laboratory reactor with three necks.

It seems very simple procedure according to the video, I wonder if the procedure is really as simple as described.

For materials, the reactor can be found at a decent price, the biggest problem for the cost is the platinum cathode.

What do you think, do you think it's a fake?

March 6, 2017

A curiosity you think you can use the filter in platinum is rhodium in catalytic converters in cars to make the electrodes?

In theory it could also work.

March 6, 2017

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.

March 6, 2017

The glass vessels are silly expensive! Good for the video but expensive for general use. I'd seriously suggest that you check out the chemistry because that looks to be a very simple process, neglecting several steps thought to be essential. What electrode material did they use?

March 6, 2017

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

Chinese / PbO2 MMO? Not what I tried to do a Google search without finding, where can I find them?

The glas reactor:

https://m.it.aliexpress.com/s/item/1878350348.html?trace=wwwdetail2mobilesitedetail&productId=1878350348&productSubject=3000ML-Multi-

nqeck-Reaction-Flask-Separately-flask-round-bottom-with-Clamp&spm=2114.46010308.4.22.s8MZol#autostay

https://it.aliexpress.com/popular/reaction-flask.html

March 6, 2017

should this be right?

Anodo di ossido di metallo misto reticolare (MMO)

March 6, 2017

Do you know of this video here uses a laboratory reactor with three necks.
It seems very simple procedure according to the video, I wonder if the procedure is really as simple as described.
For materials, the reactor can be found at a decent price, the biggest problem for the cost is the platinum cathode.
What do you think, do you think it's a fake?

I just viewed this video. It looks like he's making KClO₃, not KClO₄.

The crystals look like what I expect from potassium chlorate. When I add KCl solution to sodium perchlorate, I get an instant thick cloud of fine KClO₄ crystals.

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.

Possibly there's a mix up of the two videos? <_<

WSM

making potassium (per) chlorate

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